#! data_publication_text _publ_requested_journal Organometallics _publ_contact_author_name 'Andrew D. Phillips' _publ_contact_author_address ;School of Chemistry and Chemical Biology University College Dublin Science South Belfield Campus Belfield, Dublin Co. Dublin 4, Ireland ; _publ_contact_author_email andrew.phillips@ucd.ie _publ_contact_author_phone +353017162075 _publ_contact_author_fax +353017162088 loop_ _publ_author_name _publ_author_address 'Thommes, Katrin' ;Institut des Sciences et Ing\'enierie Chimiques Ecole Polytechnique F\'ed\'erale de Lausanne (EPFL) CH-1015 Lausanne, Switzerland. ; 'Scopelliti, Rosario' ;Institut des Sciences et Ing\'enierie Chimiques Ecole Polytechnique F\'ed\'erale de Lausanne (EPFL) CH-1015 Lausanne, Switzerland. ; 'Gandolfi, Claudio' ;Department of Chemistry University of Fribourg Chemin du Mus\'ee 9 CH-1700 Fribourg, Switzerland. ; 'Albrecht, Martin' ;Department of Chemistry University of Fribourg Chemin du Mus\'ee 9 CH-1700 Fribourg, Switzerland. ; 'Severin, Kay' ;Institut des Sciences et Ing\'enierie Chimiques Ecole Polytechnique F\'ed\'erale de Lausanne (EPFL) CH-1015 Lausanne, Switzerland. ; 'Schreiber, Dominique' ;School of Chemistry and Chemical Biology University College Dublin Science South Belfield Campus Belfield, Dublin Co. Dublin 4, Ireland ; 'Dyson, Paul' ;Institut des Sciences et Ing\'enierie Chimiques Ecole Polytechnique F\'ed\'erale de Lausanne (EPFL) CH-1015 Lausanne, Switzerland. ; data_adp265 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*RuCl((2,6-Me2C6H3NC(Me))2CH)' _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 Cl N2 Ru' _chemical_formula_sum 'C31 H40 Cl N2 Ru' _chemical_formula_weight 577.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4115(13) _cell_length_b 16.1565(7) _cell_length_c 16.810(2) _cell_angle_alpha 90.00 _cell_angle_beta 115.569(8) _cell_angle_gamma 90.00 _cell_volume 2795.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 83 _cell_measurement_theta_min 3.859 _cell_measurement_theta_max 19.568 _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.668 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details ; Bruker Nonius Area Dector Scaling and Absorption Correction SADABS 2.10 (Bruker, 2003) based on an algorithm published in R.H. Blessing, Acta Cryst. (1995), a51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonus KappaCCD with \k-goniostat' _diffrn_detector 'Bruker Apex II CCD' _diffrn_measurement_method '\f & \w scans' _diffrn_source 'Enraf Nonius FR590' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51313 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4894 _reflns_number_gt 3815 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'Collect (Hooft, R.W.W., 1998. Nonius B.V., 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg A.J.M., Nonius B.V., 1989-2000)' _computing_data_reduction 'EvalCCD (Hooft R.W.W., Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick G.M., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick G.M., 2008)' _computing_molecular_graphics 'ORTEP-3 for windows 2.02 (Farrugia, 2008)' _computing_publication_material 'WinGX 1.80.05 (Farrugia, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0095P)^2^+3.7382P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4894 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8470(3) 0.08473(17) 0.73570(18) 0.0171(7) Uani 1 1 d . . . C2 C 0.9409(3) 0.08999(18) 0.70318(19) 0.0197(7) Uani 1 1 d . . . C3 C 1.0713(3) 0.07434(18) 0.7616(2) 0.0244(7) Uani 1 1 d . . . H3 H 1.1363 0.0777 0.7407 0.029 Uiso 1 1 calc R . . C4 C 1.1064(3) 0.05411(19) 0.8488(2) 0.0279(8) Uani 1 1 d . . . H4 H 1.1950 0.0440 0.8873 0.033 Uiso 1 1 calc R . . C5 C 1.0122(3) 0.04860(18) 0.8800(2) 0.0253(8) Uani 1 1 d . . . H5 H 1.0372 0.0349 0.9401 0.030 Uiso 1 1 calc R . . C6 C 0.8816(3) 0.06281(17) 0.82466(18) 0.0186(7) Uani 1 1 d . . . C7 C 0.9073(3) 0.1106(2) 0.60802(19) 0.0255(7) Uani 1 1 d . . . H7A H 0.9121 0.0603 0.5770 0.038 Uiso 1 1 calc R . . H7B H 0.9691 0.1516 0.6057 0.038 Uiso 1 1 calc R . . H7C H 0.8191 0.1333 0.5797 0.038 Uiso 1 1 calc R . . C8 C 0.7783(3) 0.05133(19) 0.85758(19) 0.0240(7) Uani 1 1 d . . . H8A H 0.7327 -0.0011 0.8352 0.036 Uiso 1 1 calc R . . H8B H 0.7161 0.0972 0.8366 0.036 Uiso 1 1 calc R . . H8C H 0.8191 0.0505 0.9222 0.036 Uiso 1 1 calc R . . C9 C 0.6431(3) 0.02979(17) 0.63954(17) 0.0158(7) Uani 1 1 d . . . C10 C 0.7139(3) -0.05066(17) 0.64228(19) 0.0199(7) Uani 1 1 d . . . H10A H 0.7819 -0.0404 0.6226 0.030 Uiso 1 1 calc R . . H10B H 0.6521 -0.0913 0.6032 0.030 Uiso 1 1 calc R . . H10C H 0.7534 -0.0721 0.7027 0.030 Uiso 1 1 calc R . . C11 C 0.5071(3) 0.02534(17) 0.59972(17) 0.0155(7) Uani 1 1 d . . . H11 H 0.4700 -0.0225 0.5650 0.019 Uiso 1 1 calc R . . C12 C 0.4199(3) 0.08331(18) 0.60527(17) 0.0147(6) Uani 1 1 d . . . C13 C 0.2826(3) 0.05219(19) 0.58143(19) 0.0209(7) Uani 1 1 d . . . H13A H 0.2663 0.0529 0.6341 0.031 Uiso 1 1 calc R . . H13B H 0.2736 -0.0045 0.5587 0.031 Uiso 1 1 calc R . . H13C H 0.2198 0.0882 0.5362 0.031 Uiso 1 1 calc R . . C14 C 0.3520(3) 0.20939(18) 0.64291(17) 0.0156(6) Uani 1 1 d . . . C15 C 0.3408(3) 0.20747(18) 0.72356(17) 0.0162(6) Uani 1 1 d . . . C16 C 0.2452(3) 0.25586(18) 0.73143(19) 0.0211(7) Uani 1 1 d . . . H16 H 0.2369 0.2555 0.7853 0.025 Uiso 1 1 calc R . . C17 C 0.1617(3) 0.30455(19) 0.6619(2) 0.0225(7) Uani 1 1 d . . . H17 H 0.0984 0.3382 0.6688 0.027 Uiso 1 1 calc R . . C18 C 0.1713(3) 0.30382(18) 0.58236(19) 0.0208(7) Uani 1 1 d . . . H18 H 0.1133 0.3367 0.5348 0.025 Uiso 1 1 calc R . . C19 C 0.2643(3) 0.25583(18) 0.57091(18) 0.0177(7) Uani 1 1 d . . . C20 C 0.4314(3) 0.15496(19) 0.80017(18) 0.0207(7) Uani 1 1 d . . . H20A H 0.4110 0.1628 0.8506 0.031 Uiso 1 1 calc R . . H20B H 0.5215 0.1716 0.8165 0.031 Uiso 1 1 calc R . . H20C H 0.4202 0.0965 0.7828 0.031 Uiso 1 1 calc R . . C21 C 0.2664(3) 0.25148(19) 0.48129(18) 0.0211(7) Uani 1 1 d . . . H21A H 0.2224 0.2009 0.4508 0.032 Uiso 1 1 calc R . . H21B H 0.3566 0.2508 0.4891 0.032 Uiso 1 1 calc R . . H21C H 0.2217 0.2999 0.4462 0.032 Uiso 1 1 calc R . . C22 C 0.7341(3) 0.29636(17) 0.77891(17) 0.0152(6) Uani 1 1 d . . . C23 C 0.6127(3) 0.33554(17) 0.72383(18) 0.0162(6) Uani 1 1 d . . . C24 C 0.6133(3) 0.35254(17) 0.64061(17) 0.0154(7) Uani 1 1 d . . . C25 C 0.7393(3) 0.32741(17) 0.64642(18) 0.0162(6) Uani 1 1 d . . . C26 C 0.8140(3) 0.29481(17) 0.73213(17) 0.0156(6) Uani 1 1 d . . . C27 C 0.7826(3) 0.2766(2) 0.87584(17) 0.0220(7) Uani 1 1 d . . . H27A H 0.8382 0.2274 0.8902 0.033 Uiso 1 1 calc R . . H27B H 0.7084 0.2659 0.8891 0.033 Uiso 1 1 calc R . . H27C H 0.8325 0.3236 0.9110 0.033 Uiso 1 1 calc R . . C28 C 0.5154(3) 0.36744(19) 0.75379(19) 0.0212(7) Uani 1 1 d . . . H28A H 0.5348 0.4254 0.7720 0.032 Uiso 1 1 calc R . . H28B H 0.5194 0.3343 0.8038 0.032 Uiso 1 1 calc R . . H28C H 0.4281 0.3635 0.7053 0.032 Uiso 1 1 calc R . . C29 C 0.5125(3) 0.40165(19) 0.56636(19) 0.0259(8) Uani 1 1 d . . . H29A H 0.4280 0.3955 0.5678 0.039 Uiso 1 1 calc R . . H29B H 0.5066 0.3812 0.5099 0.039 Uiso 1 1 calc R . . H29C H 0.5373 0.4602 0.5731 0.039 Uiso 1 1 calc R . . C30 C 0.7864(3) 0.34138(19) 0.57637(19) 0.0229(7) Uani 1 1 d . . . H30A H 0.8390 0.3919 0.5899 0.034 Uiso 1 1 calc R . . H30B H 0.7116 0.3473 0.5188 0.034 Uiso 1 1 calc R . . H30C H 0.8391 0.2941 0.5749 0.034 Uiso 1 1 calc R . . C31 C 0.9560(3) 0.2746(2) 0.77226(19) 0.0234(7) Uani 1 1 d . . . H31A H 0.9796 0.2531 0.7266 0.035 Uiso 1 1 calc R . . H31B H 0.9750 0.2327 0.8183 0.035 Uiso 1 1 calc R . . H31C H 1.0064 0.3248 0.7981 0.035 Uiso 1 1 calc R . . N1 N 0.7101(2) 0.09802(14) 0.67893(14) 0.0136(5) Uani 1 1 d . . . N2 N 0.4535(2) 0.16134(14) 0.63442(14) 0.0133(5) Uani 1 1 d . . . Cl1 Cl 0.57586(7) 0.19262(4) 0.50295(4) 0.01631(16) Uani 1 1 d . . . Ru1 Ru 0.63006(2) 0.216733(14) 0.659534(14) 0.01165(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0202(17) 0.0101(15) 0.0167(15) -0.0004(12) 0.0040(13) 0.0020(13) C2 0.0188(17) 0.0160(16) 0.0228(16) -0.0044(13) 0.0076(14) -0.0014(13) C3 0.0203(18) 0.0180(17) 0.0343(19) -0.0034(14) 0.0112(15) 0.0015(14) C4 0.0200(18) 0.0198(18) 0.0334(19) -0.0001(14) 0.0016(15) 0.0040(14) C5 0.0299(19) 0.0165(17) 0.0185(16) 0.0023(13) 0.0003(14) 0.0036(14) C6 0.0250(18) 0.0123(15) 0.0178(16) -0.0005(12) 0.0085(13) 0.0013(13) C7 0.0255(18) 0.0282(19) 0.0269(17) -0.0041(14) 0.0152(15) -0.0027(15) C8 0.036(2) 0.0202(18) 0.0155(15) 0.0025(13) 0.0106(14) 0.0025(15) C9 0.0244(17) 0.0154(16) 0.0103(14) 0.0017(12) 0.0100(13) 0.0004(13) C10 0.0238(17) 0.0132(16) 0.0204(16) -0.0003(12) 0.0074(13) -0.0005(13) C11 0.0223(17) 0.0134(16) 0.0109(14) -0.0005(12) 0.0073(12) -0.0022(13) C12 0.0189(16) 0.0166(16) 0.0061(13) 0.0010(11) 0.0030(12) -0.0039(13) C13 0.0219(17) 0.0211(17) 0.0195(16) -0.0058(13) 0.0087(14) -0.0057(14) C14 0.0144(14) 0.0137(15) 0.0176(14) -0.0042(13) 0.0057(12) -0.0039(13) C15 0.0152(15) 0.0152(16) 0.0177(14) -0.0050(13) 0.0067(12) -0.0050(13) C16 0.0223(17) 0.0238(17) 0.0217(16) -0.0057(13) 0.0137(14) -0.0049(14) C17 0.0141(17) 0.0230(18) 0.0341(18) -0.0059(14) 0.0138(15) -0.0005(13) C18 0.0155(16) 0.0200(18) 0.0224(16) -0.0003(13) 0.0041(13) 0.0026(13) C19 0.0170(16) 0.0186(16) 0.0160(15) -0.0035(12) 0.0058(13) -0.0032(13) C20 0.0244(18) 0.0234(18) 0.0173(15) -0.0027(13) 0.0120(14) -0.0022(14) C21 0.0214(17) 0.0227(16) 0.0160(15) -0.0002(13) 0.0050(13) 0.0027(13) C22 0.0159(15) 0.0122(16) 0.0153(14) -0.0048(12) 0.0047(12) -0.0042(12) C23 0.0197(16) 0.0101(15) 0.0193(15) -0.0043(12) 0.0091(13) -0.0024(12) C24 0.0232(17) 0.0058(14) 0.0168(16) -0.0035(11) 0.0084(14) -0.0037(13) C25 0.0220(17) 0.0112(15) 0.0170(15) -0.0039(12) 0.0099(13) -0.0076(13) C26 0.0160(15) 0.0136(16) 0.0166(14) -0.0046(12) 0.0065(12) -0.0035(13) C27 0.0252(17) 0.0251(18) 0.0137(14) -0.0027(14) 0.0064(12) -0.0047(15) C28 0.0229(17) 0.0176(17) 0.0228(16) -0.0065(13) 0.0095(14) -0.0009(14) C29 0.034(2) 0.0170(17) 0.0202(16) 0.0037(13) 0.0060(15) 0.0034(15) C30 0.0320(19) 0.0209(18) 0.0216(16) -0.0029(13) 0.0169(15) -0.0108(15) C31 0.0173(16) 0.0227(18) 0.0276(17) -0.0085(14) 0.0073(13) -0.0062(14) N1 0.0151(13) 0.0144(13) 0.0118(12) 0.0003(10) 0.0061(10) -0.0003(10) N2 0.0149(13) 0.0131(13) 0.0123(12) 0.0001(10) 0.0063(10) 0.0008(10) Cl1 0.0215(4) 0.0174(4) 0.0109(3) -0.0011(3) 0.0079(3) -0.0019(3) Ru1 0.01409(12) 0.01121(12) 0.00958(10) -0.00051(10) 0.00506(8) -0.00102(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.399(4) . ? C1 C6 1.417(4) . ? C1 N1 1.453(4) . ? C2 C3 1.408(4) . ? C2 C7 1.513(4) . ? C3 C4 1.382(4) . ? C3 H3 0.9500 . ? C4 C5 1.387(5) . ? C4 H4 0.9500 . ? C5 C6 1.394(4) . ? C5 H5 0.9500 . ? C6 C8 1.515(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.342(4) . ? C9 C11 1.401(4) . ? C9 C10 1.521(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.399(4) . ? C11 H11 0.9500 . ? C12 N2 1.347(4) . ? C12 C13 1.525(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.409(4) . ? C14 C15 1.416(4) . ? C14 N2 1.452(4) . ? C15 C16 1.395(4) . ? C15 C20 1.516(4) . ? C16 C17 1.390(4) . ? C16 H16 0.9500 . ? C17 C18 1.388(4) . ? C17 H17 0.9500 . ? C18 C19 1.393(4) . ? C18 H18 0.9500 . ? C19 C21 1.519(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C26 1.438(4) . ? C22 C23 1.439(4) . ? C22 C27 1.512(4) . ? C22 Ru1 2.244(3) . ? C23 C24 1.429(4) . ? C23 C28 1.495(4) . ? C23 Ru1 2.253(3) . ? C24 C25 1.456(4) . ? C24 C29 1.507(4) . ? C24 Ru1 2.214(3) . ? C25 C26 1.421(4) . ? C25 C30 1.508(4) . ? C25 Ru1 2.244(3) . ? C26 C31 1.498(4) . ? C26 Ru1 2.297(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N1 Ru1 2.089(2) . ? N2 Ru1 2.075(2) . ? Cl1 Ru1 2.4611(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 121.0(3) . . ? C2 C1 N1 121.4(3) . . ? C6 C1 N1 117.5(3) . . ? C1 C2 C3 118.3(3) . . ? C1 C2 C7 122.7(3) . . ? C3 C2 C7 119.1(3) . . ? C4 C3 C2 121.2(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 118.4(3) . . ? C5 C6 C8 120.9(3) . . ? C1 C6 C8 120.6(3) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C11 123.8(3) . . ? N1 C9 C10 120.3(3) . . ? C11 C9 C10 115.8(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 127.3(3) . . ? C12 C11 H11 116.3 . . ? C9 C11 H11 116.3 . . ? N2 C12 C11 123.5(3) . . ? N2 C12 C13 120.2(3) . . ? C11 C12 C13 116.2(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 120.7(3) . . ? C19 C14 N2 120.1(2) . . ? C15 C14 N2 119.2(2) . . ? C16 C15 C14 118.4(3) . . ? C16 C15 C20 120.5(3) . . ? C14 C15 C20 121.0(3) . . ? C17 C16 C15 121.2(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C18 C17 C16 119.7(3) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 121.3(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C14 118.6(3) . . ? C18 C19 C21 120.1(3) . . ? C14 C19 C21 121.2(3) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C26 C22 C23 108.5(2) . . ? C26 C22 C27 124.2(3) . . ? C23 C22 C27 126.1(3) . . ? C26 C22 Ru1 73.55(15) . . ? C23 C22 Ru1 71.69(15) . . ? C27 C22 Ru1 130.4(2) . . ? C24 C23 C22 107.7(3) . . ? C24 C23 C28 125.6(3) . . ? C22 C23 C28 125.7(3) . . ? C24 C23 Ru1 69.85(15) . . ? C22 C23 Ru1 70.99(15) . . ? C28 C23 Ru1 133.4(2) . . ? C23 C24 C25 107.6(2) . . ? C23 C24 C29 126.0(3) . . ? C25 C24 C29 125.5(3) . . ? C23 C24 Ru1 72.86(16) . . ? C25 C24 Ru1 72.08(16) . . ? C29 C24 Ru1 128.9(2) . . ? C26 C25 C24 108.4(2) . . ? C26 C25 C30 125.9(3) . . ? C24 C25 C30 125.5(3) . . ? C26 C25 Ru1 73.80(16) . . ? C24 C25 Ru1 69.81(15) . . ? C30 C25 Ru1 126.61(19) . . ? C25 C26 C22 107.6(2) . . ? C25 C26 C31 126.6(3) . . ? C22 C26 C31 125.1(2) . . ? C25 C26 Ru1 69.74(15) . . ? C22 C26 Ru1 69.54(15) . . ? C31 C26 Ru1 133.0(2) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C9 N1 C1 115.2(2) . . ? C9 N1 Ru1 124.00(19) . . ? C1 N1 Ru1 120.81(17) . . ? C12 N2 C14 115.0(2) . . ? C12 N2 Ru1 125.20(19) . . ? C14 N2 Ru1 119.70(17) . . ? N2 Ru1 N1 87.52(9) . . ? N2 Ru1 C24 112.48(10) . . ? N1 Ru1 C24 159.63(10) . . ? N2 Ru1 C22 121.47(9) . . ? N1 Ru1 C22 111.09(9) . . ? C24 Ru1 C22 62.60(10) . . ? N2 Ru1 C25 148.80(10) . . ? N1 Ru1 C25 121.53(10) . . ? C24 Ru1 C25 38.11(11) . . ? C22 Ru1 C25 61.90(10) . . ? N2 Ru1 C23 100.74(10) . . ? N1 Ru1 C23 146.15(9) . . ? C24 Ru1 C23 37.29(10) . . ? C22 Ru1 C23 37.33(10) . . ? C25 Ru1 C23 62.34(10) . . ? N2 Ru1 C26 158.38(9) . . ? N1 Ru1 C26 100.57(10) . . ? C24 Ru1 C26 62.25(10) . . ? C22 Ru1 C26 36.91(10) . . ? C25 Ru1 C26 36.45(10) . . ? C23 Ru1 C26 61.76(10) . . ? N2 Ru1 Cl1 86.58(6) . . ? N1 Ru1 Cl1 84.99(6) . . ? C24 Ru1 Cl1 92.12(7) . . ? C22 Ru1 Cl1 147.02(7) . . ? C25 Ru1 Cl1 85.12(7) . . ? C23 Ru1 Cl1 127.90(7) . . ? C26 Ru1 Cl1 113.91(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.1(4) . . . . ? N1 C1 C2 C3 -178.4(3) . . . . ? C6 C1 C2 C7 178.1(3) . . . . ? N1 C1 C2 C7 0.7(4) . . . . ? C1 C2 C3 C4 0.1(4) . . . . ? C7 C2 C3 C4 -179.1(3) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C3 C4 C5 C6 0.3(5) . . . . ? C4 C5 C6 C1 -1.2(4) . . . . ? C4 C5 C6 C8 176.0(3) . . . . ? C2 C1 C6 C5 1.6(4) . . . . ? N1 C1 C6 C5 179.1(3) . . . . ? C2 C1 C6 C8 -175.6(3) . . . . ? N1 C1 C6 C8 1.8(4) . . . . ? N1 C9 C11 C12 -10.7(4) . . . . ? C10 C9 C11 C12 164.8(3) . . . . ? C9 C11 C12 N2 15.3(4) . . . . ? C9 C11 C12 C13 -161.0(3) . . . . ? C19 C14 C15 C16 -3.2(4) . . . . ? N2 C14 C15 C16 178.2(2) . . . . ? C19 C14 C15 C20 177.5(3) . . . . ? N2 C14 C15 C20 -1.1(4) . . . . ? C14 C15 C16 C17 0.5(4) . . . . ? C20 C15 C16 C17 179.8(3) . . . . ? C15 C16 C17 C18 1.5(4) . . . . ? C16 C17 C18 C19 -0.8(5) . . . . ? C17 C18 C19 C14 -1.9(4) . . . . ? C17 C18 C19 C21 175.7(3) . . . . ? C15 C14 C19 C18 3.9(4) . . . . ? N2 C14 C19 C18 -177.5(3) . . . . ? C15 C14 C19 C21 -173.7(3) . . . . ? N2 C14 C19 C21 5.0(4) . . . . ? C26 C22 C23 C24 4.3(3) . . . . ? C27 C22 C23 C24 172.3(3) . . . . ? Ru1 C22 C23 C24 -60.49(19) . . . . ? C26 C22 C23 C28 -164.8(3) . . . . ? C27 C22 C23 C28 3.2(5) . . . . ? Ru1 C22 C23 C28 130.3(3) . . . . ? C26 C22 C23 Ru1 64.83(19) . . . . ? C27 C22 C23 Ru1 -127.2(3) . . . . ? C22 C23 C24 C25 -2.9(3) . . . . ? C28 C23 C24 C25 166.2(3) . . . . ? Ru1 C23 C24 C25 -64.16(18) . . . . ? C22 C23 C24 C29 -172.7(3) . . . . ? C28 C23 C24 C29 -3.5(5) . . . . ? Ru1 C23 C24 C29 126.1(3) . . . . ? C22 C23 C24 Ru1 61.22(19) . . . . ? C28 C23 C24 Ru1 -129.6(3) . . . . ? C23 C24 C25 C26 0.5(3) . . . . ? C29 C24 C25 C26 170.3(3) . . . . ? Ru1 C24 C25 C26 -64.21(19) . . . . ? C23 C24 C25 C30 -174.1(3) . . . . ? C29 C24 C25 C30 -4.3(4) . . . . ? Ru1 C24 C25 C30 121.2(3) . . . . ? C23 C24 C25 Ru1 64.68(19) . . . . ? C29 C24 C25 Ru1 -125.5(3) . . . . ? C24 C25 C26 C22 2.2(3) . . . . ? C30 C25 C26 C22 176.7(3) . . . . ? Ru1 C25 C26 C22 -59.45(19) . . . . ? C24 C25 C26 C31 -169.1(3) . . . . ? C30 C25 C26 C31 5.4(5) . . . . ? Ru1 C25 C26 C31 129.2(3) . . . . ? C24 C25 C26 Ru1 61.64(19) . . . . ? C30 C25 C26 Ru1 -123.8(3) . . . . ? C23 C22 C26 C25 -4.0(3) . . . . ? C27 C22 C26 C25 -172.3(3) . . . . ? Ru1 C22 C26 C25 59.58(19) . . . . ? C23 C22 C26 C31 167.5(3) . . . . ? C27 C22 C26 C31 -0.8(5) . . . . ? Ru1 C22 C26 C31 -128.9(3) . . . . ? C23 C22 C26 Ru1 -63.62(19) . . . . ? C27 C22 C26 Ru1 128.1(3) . . . . ? C11 C9 N1 C1 164.4(2) . . . . ? C10 C9 N1 C1 -10.9(4) . . . . ? C11 C9 N1 Ru1 -17.4(4) . . . . ? C10 C9 N1 Ru1 167.33(19) . . . . ? C2 C1 N1 C9 90.4(3) . . . . ? C6 C1 N1 C9 -87.1(3) . . . . ? C2 C1 N1 Ru1 -87.9(3) . . . . ? C6 C1 N1 Ru1 94.7(3) . . . . ? C11 C12 N2 C14 -174.5(2) . . . . ? C13 C12 N2 C14 1.7(3) . . . . ? C11 C12 N2 Ru1 9.3(4) . . . . ? C13 C12 N2 Ru1 -174.53(18) . . . . ? C19 C14 N2 C12 -89.2(3) . . . . ? C15 C14 N2 C12 89.5(3) . . . . ? C19 C14 N2 Ru1 87.3(3) . . . . ? C15 C14 N2 Ru1 -94.1(3) . . . . ? C12 N2 Ru1 N1 -24.8(2) . . . . ? C14 N2 Ru1 N1 159.14(19) . . . . ? C12 N2 Ru1 C24 151.2(2) . . . . ? C14 N2 Ru1 C24 -24.9(2) . . . . ? C12 N2 Ru1 C22 -138.1(2) . . . . ? C14 N2 Ru1 C22 45.8(2) . . . . ? C12 N2 Ru1 C25 135.1(2) . . . . ? C14 N2 Ru1 C25 -41.0(3) . . . . ? C12 N2 Ru1 C23 -171.7(2) . . . . ? C14 N2 Ru1 C23 12.2(2) . . . . ? C12 N2 Ru1 C26 -137.7(3) . . . . ? C14 N2 Ru1 C26 46.3(3) . . . . ? C12 N2 Ru1 Cl1 60.3(2) . . . . ? C14 N2 Ru1 Cl1 -115.73(18) . . . . ? C9 N1 Ru1 N2 28.6(2) . . . . ? C1 N1 Ru1 N2 -153.3(2) . . . . ? C9 N1 Ru1 C24 -140.7(3) . . . . ? C1 N1 Ru1 C24 37.3(4) . . . . ? C9 N1 Ru1 C22 151.5(2) . . . . ? C1 N1 Ru1 C22 -30.4(2) . . . . ? C9 N1 Ru1 C25 -139.3(2) . . . . ? C1 N1 Ru1 C25 38.8(2) . . . . ? C9 N1 Ru1 C23 134.3(2) . . . . ? C1 N1 Ru1 C23 -47.6(3) . . . . ? C9 N1 Ru1 C26 -171.6(2) . . . . ? C1 N1 Ru1 C26 6.5(2) . . . . ? C9 N1 Ru1 Cl1 -58.2(2) . . . . ? C1 N1 Ru1 Cl1 119.9(2) . . . . ? C23 C24 Ru1 N2 77.86(18) . . . . ? C25 C24 Ru1 N2 -166.52(14) . . . . ? C29 C24 Ru1 N2 -44.9(3) . . . . ? C23 C24 Ru1 N1 -113.7(3) . . . . ? C25 C24 Ru1 N1 1.9(3) . . . . ? C29 C24 Ru1 N1 123.5(3) . . . . ? C23 C24 Ru1 C22 -37.09(17) . . . . ? C25 C24 Ru1 C22 78.53(17) . . . . ? C29 C24 Ru1 C22 -159.9(3) . . . . ? C23 C24 Ru1 C25 -115.6(2) . . . . ? C29 C24 Ru1 C25 121.6(3) . . . . ? C25 C24 Ru1 C23 115.6(2) . . . . ? C29 C24 Ru1 C23 -122.8(4) . . . . ? C23 C24 Ru1 C26 -78.94(18) . . . . ? C25 C24 Ru1 C26 36.69(15) . . . . ? C29 C24 Ru1 C26 158.3(3) . . . . ? C23 C24 Ru1 Cl1 165.03(16) . . . . ? C25 C24 Ru1 Cl1 -79.34(14) . . . . ? C29 C24 Ru1 Cl1 42.2(3) . . . . ? C26 C22 Ru1 N2 179.74(15) . . . . ? C23 C22 Ru1 N2 -63.75(19) . . . . ? C27 C22 Ru1 N2 58.5(3) . . . . ? C26 C22 Ru1 N1 79.28(17) . . . . ? C23 C22 Ru1 N1 -164.21(16) . . . . ? C27 C22 Ru1 N1 -42.0(3) . . . . ? C26 C22 Ru1 C24 -79.45(18) . . . . ? C23 C22 Ru1 C24 37.06(17) . . . . ? C27 C22 Ru1 C24 159.3(3) . . . . ? C26 C22 Ru1 C25 -36.16(16) . . . . ? C23 C22 Ru1 C25 80.35(18) . . . . ? C27 C22 Ru1 C25 -157.4(3) . . . . ? C26 C22 Ru1 C23 -116.5(2) . . . . ? C27 C22 Ru1 C23 122.2(3) . . . . ? C23 C22 Ru1 C26 116.5(2) . . . . ? C27 C22 Ru1 C26 -121.3(3) . . . . ? C26 C22 Ru1 Cl1 -35.7(2) . . . . ? C23 C22 Ru1 Cl1 80.8(2) . . . . ? C27 C22 Ru1 Cl1 -156.97(19) . . . . ? C26 C25 Ru1 N2 141.72(18) . . . . ? C24 C25 Ru1 N2 24.6(3) . . . . ? C30 C25 Ru1 N2 -95.2(3) . . . . ? C26 C25 Ru1 N1 -62.06(19) . . . . ? C24 C25 Ru1 N1 -179.21(14) . . . . ? C30 C25 Ru1 N1 61.0(3) . . . . ? C26 C25 Ru1 C24 117.1(2) . . . . ? C30 C25 Ru1 C24 -119.8(3) . . . . ? C26 C25 Ru1 C22 36.62(16) . . . . ? C24 C25 Ru1 C22 -80.53(17) . . . . ? C30 C25 Ru1 C22 159.7(3) . . . . ? C26 C25 Ru1 C23 79.06(17) . . . . ? C24 C25 Ru1 C23 -38.08(15) . . . . ? C30 C25 Ru1 C23 -157.9(3) . . . . ? C24 C25 Ru1 C26 -117.1(2) . . . . ? C30 C25 Ru1 C26 123.0(3) . . . . ? C26 C25 Ru1 Cl1 -143.14(16) . . . . ? C24 C25 Ru1 Cl1 99.72(15) . . . . ? C30 C25 Ru1 Cl1 -20.1(3) . . . . ? C24 C23 Ru1 N2 -113.15(17) . . . . ? C22 C23 Ru1 N2 128.86(16) . . . . ? C28 C23 Ru1 N2 7.2(3) . . . . ? C24 C23 Ru1 N1 145.10(19) . . . . ? C22 C23 Ru1 N1 27.1(3) . . . . ? C28 C23 Ru1 N1 -94.5(3) . . . . ? C22 C23 Ru1 C24 -118.0(2) . . . . ? C28 C23 Ru1 C24 120.4(4) . . . . ? C24 C23 Ru1 C22 118.0(2) . . . . ? C28 C23 Ru1 C22 -121.6(3) . . . . ? C24 C23 Ru1 C25 38.92(17) . . . . ? C22 C23 Ru1 C25 -79.06(18) . . . . ? C28 C23 Ru1 C25 159.3(3) . . . . ? C24 C23 Ru1 C26 80.39(18) . . . . ? C22 C23 Ru1 C26 -37.59(16) . . . . ? C28 C23 Ru1 C26 -159.2(3) . . . . ? C24 C23 Ru1 Cl1 -19.1(2) . . . . ? C22 C23 Ru1 Cl1 -137.08(14) . . . . ? C28 C23 Ru1 Cl1 101.3(3) . . . . ? C25 C26 Ru1 N2 -119.4(3) . . . . ? C22 C26 Ru1 N2 -0.6(3) . . . . ? C31 C26 Ru1 N2 118.8(3) . . . . ? C25 C26 Ru1 N1 130.00(17) . . . . ? C22 C26 Ru1 N1 -111.16(16) . . . . ? C31 C26 Ru1 N1 8.3(3) . . . . ? C25 C26 Ru1 C24 -38.36(16) . . . . ? C22 C26 Ru1 C24 80.48(18) . . . . ? C31 C26 Ru1 C24 -160.1(3) . . . . ? C25 C26 Ru1 C22 -118.8(2) . . . . ? C31 C26 Ru1 C22 119.4(3) . . . . ? C22 C26 Ru1 C25 118.8(2) . . . . ? C31 C26 Ru1 C25 -121.7(3) . . . . ? C25 C26 Ru1 C23 -80.81(18) . . . . ? C22 C26 Ru1 C23 38.02(16) . . . . ? C31 C26 Ru1 C23 157.5(3) . . . . ? C25 C26 Ru1 Cl1 40.83(18) . . . . ? C22 C26 Ru1 Cl1 159.66(14) . . . . ? C31 C26 Ru1 Cl1 -80.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.367 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.079 data_adp462 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*RuCl((3,5-Me2C6H3NCMe)2CH)' _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 Cl N2 Ru' _chemical_formula_sum 'C31 H40 Cl N2 Ru' _chemical_formula_weight 577.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0996(17) _cell_length_b 8.1612(8) _cell_length_c 24.661(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.246(9) _cell_angle_gamma 90.00 _cell_volume 2748.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 4504 _cell_measurement_theta_min 2.8449 _cell_measurement_theta_max 28.8815 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.343 _exptl_crystal_size_mid 0.283 _exptl_crystal_size_min 0.189 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_T_min 0.96479 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_detector_area_resol_mean 8.2812 _diffrn_measurement_method '\w and \p scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17514 _diffrn_reflns_av_R_equivalents 0.0998 _diffrn_reflns_av_sigmaI/netI 0.1281 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4834 _reflns_number_gt 2632 _reflns_threshold_expression I>2/s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick G.M., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick G.M., 2008)' _computing_molecular_graphics 'ORTEP-3 for windows 2.02 (Farrugia, 2008)' _computing_publication_material 'WinGX 1.80.05 (Farrugia, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4834 _refine_ls_number_parameters 327 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 0.842 _refine_ls_restrained_S_all 0.842 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.24591(3) 0.75485(6) 0.887073(17) 0.01286(10) Uani 1 1 d . . . Cl1 Cl 0.26017(9) 1.03545(14) 0.92535(6) 0.0207(3) Uani 1 1 d . . . N1 N 0.3259(3) 0.6803(4) 0.97387(18) 0.0136(10) Uani 1 1 d . . . N2 N 0.3759(3) 0.7982(4) 0.88197(18) 0.0159(10) Uani 1 1 d . . . C1 C 0.2700(3) 0.6163(6) 1.0046(2) 0.0164(11) Uani 1 1 d . . . C2 C 0.2179(3) 0.7272(6) 1.02216(19) 0.0190(12) Uani 1 1 d . . . H2 H 0.2221 0.8410 1.0154 0.023 Uiso 1 1 calc R . . C3 C 0.1593(4) 0.6737(6) 1.0496(2) 0.0203(12) Uani 1 1 d . . . C4 C 0.1550(4) 0.5071(6) 1.0586(2) 0.0212(13) Uani 1 1 d . . . H4 H 0.1148 0.4688 1.0769 0.025 Uiso 1 1 calc R . . C5 C 0.2071(4) 0.3945(6) 1.0419(2) 0.0187(12) Uani 1 1 d . . . C6 C 0.2655(3) 0.4501(6) 1.0146(2) 0.0184(12) Uani 1 1 d . . . H6 H 0.3021 0.3745 1.0030 0.022 Uiso 1 1 calc R . . C7 C 0.1024(4) 0.7949(6) 1.0688(2) 0.0311(15) Uani 1 1 d . . . H7A H 0.1472 0.8510 1.1054 0.047 Uiso 1 1 calc R . . H7B H 0.0522 0.7367 1.0765 0.047 Uiso 1 1 calc R . . H7C H 0.0710 0.8757 1.0368 0.047 Uiso 1 1 calc R . . C8 C 0.1951(4) 0.2130(6) 1.0486(2) 0.0268(15) Uani 1 1 d . . . H8A H 0.2574 0.1671 1.0775 0.040 Uiso 1 1 calc R . . H8B H 0.1757 0.1590 1.0097 0.040 Uiso 1 1 calc R . . H8C H 0.1446 0.1953 1.0630 0.040 Uiso 1 1 calc R . . C9 C 0.4214(4) 0.7009(5) 1.0074(2) 0.0149(12) Uani 1 1 d . . . C10 C 0.4678(4) 0.6455(6) 1.0721(2) 0.0234(13) Uani 1 1 d . . . H10A H 0.4273 0.6812 1.0921 0.035 Uiso 1 1 calc R . . H10B H 0.5333 0.6936 1.0924 0.035 Uiso 1 1 calc R . . H10C H 0.4730 0.5257 1.0736 0.035 Uiso 1 1 calc R . . C11 C 0.4835(3) 0.7716(6) 0.98612(19) 0.0169(11) Uani 1 1 d . . . H11 H 0.5482 0.7930 1.0152 0.020 Uiso 1 1 calc R . . C12 C 0.4632(4) 0.8152(5) 0.9279(2) 0.0174(12) Uani 1 1 d . . . C13 C 0.5478(4) 0.8812(6) 0.9164(2) 0.0243(13) Uani 1 1 d . . . H13A H 0.5682 0.7983 0.8953 0.037 Uiso 1 1 calc R . . H13B H 0.6029 0.9075 0.9547 0.037 Uiso 1 1 calc R . . H13C H 0.5269 0.9804 0.8918 0.037 Uiso 1 1 calc R . . C14 C 0.3700(4) 0.8372(6) 0.8234(2) 0.0164(12) Uani 1 1 d . . . C15 C 0.3943(3) 0.7196(6) 0.7912(2) 0.0194(13) Uani 1 1 d . . . H15 H 0.4160 0.6142 0.8080 0.023 Uiso 1 1 calc R . . C16 C 0.3866(3) 0.7570(8) 0.73433(19) 0.0207(10) Uani 1 1 d . . . C17 C 0.3579(4) 0.9105(6) 0.7113(2) 0.0239(13) Uani 1 1 d . . . H17 H 0.3539 0.9355 0.6727 0.029 Uiso 1 1 calc R . . C18 C 0.3346(4) 1.0307(6) 0.7429(2) 0.0215(12) Uani 1 1 d . . . C19 C 0.3408(3) 0.9916(6) 0.7993(2) 0.0199(12) Uani 1 1 d . . . H19 H 0.3247 1.0719 0.8215 0.024 Uiso 1 1 calc R . . C20 C 0.4081(4) 0.6255(6) 0.6974(2) 0.0348(15) Uani 1 1 d . . . H20A H 0.3513 0.6133 0.6586 0.052 Uiso 1 1 calc R . . H20B H 0.4213 0.5210 0.7190 0.052 Uiso 1 1 calc R . . H20C H 0.4654 0.6578 0.6910 0.052 Uiso 1 1 calc R . . C21 C 0.3031(4) 1.1990(6) 0.7169(3) 0.0384(17) Uani 1 1 d . . . H21A H 0.2318 1.2082 0.7011 0.058 Uiso 1 1 calc R . . H21B H 0.3231 1.2171 0.6845 0.058 Uiso 1 1 calc R . . H21C H 0.3340 1.2814 0.7483 0.058 Uiso 1 1 calc R . . C22 C 0.1566(3) 0.5685(6) 0.8236(2) 0.0179(12) Uani 1 1 d . . . C23 C 0.1476(3) 0.7107(5) 0.7888(2) 0.0143(12) Uani 1 1 d . . . C24 C 0.1089(4) 0.8365(6) 0.8108(2) 0.0204(13) Uani 1 1 d . . . C25 C 0.0858(3) 0.7664(7) 0.85719(19) 0.0189(11) Uani 1 1 d . . . C26 C 0.1125(4) 0.5996(6) 0.8628(2) 0.0172(12) Uani 1 1 d U . . C27 C 0.1955(4) 0.4064(6) 0.8146(2) 0.0339(15) Uani 1 1 d . . . H27A H 0.2132 0.3390 0.8507 0.051 Uiso 1 1 calc R . . H27B H 0.2535 0.4243 0.8072 0.051 Uiso 1 1 calc R . . H27C H 0.1451 0.3500 0.7802 0.051 Uiso 1 1 calc R . . C28 C 0.1601(4) 0.7150(6) 0.7316(2) 0.0266(14) Uani 1 1 d . . . H28A H 0.0971 0.6920 0.6977 0.040 Uiso 1 1 calc R . . H28B H 0.2080 0.6320 0.7332 0.040 Uiso 1 1 calc R . . H28C H 0.1832 0.8236 0.7266 0.040 Uiso 1 1 calc R . . C29 C 0.0843(4) 1.0067(6) 0.7861(2) 0.0300(14) Uani 1 1 d . . . H29A H 0.1293 1.0400 0.7690 0.045 Uiso 1 1 calc R . . H29B H 0.0904 1.0823 0.8184 0.045 Uiso 1 1 calc R . . H29C H 0.0169 1.0092 0.7548 0.045 Uiso 1 1 calc R . . C30 C 0.0299(4) 0.8537(7) 0.8865(2) 0.0316(15) Uani 1 1 d . . . H30A H -0.0391 0.8632 0.8579 0.047 Uiso 1 1 calc R . . H30B H 0.0575 0.9634 0.8991 0.047 Uiso 1 1 calc R . . H30C H 0.0347 0.7914 0.9216 0.047 Uiso 1 1 calc R . . C31 C 0.0809(4) 0.4715(6) 0.8949(2) 0.0319(15) Uani 1 1 d . . . H31A H 0.0730 0.5222 0.9286 0.048 Uiso 1 1 calc R . . H31B H 0.1308 0.3853 0.9100 0.048 Uiso 1 1 calc R . . H31C H 0.0185 0.4236 0.8671 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01228(18) 0.01563(18) 0.01136(17) -0.0004(3) 0.00569(14) -0.0013(3) Cl1 0.0234(8) 0.0169(6) 0.0203(7) -0.0017(6) 0.0080(6) -0.0007(6) N1 0.019(3) 0.009(2) 0.016(2) 0.0012(18) 0.011(2) -0.0027(18) N2 0.017(2) 0.015(2) 0.017(2) 0.0008(17) 0.008(2) 0.0010(18) C1 0.015(3) 0.024(3) 0.011(3) 0.003(2) 0.006(2) 0.002(2) C2 0.024(3) 0.017(3) 0.016(2) 0.002(3) 0.009(2) 0.000(3) C3 0.023(3) 0.024(3) 0.018(3) -0.004(2) 0.013(3) -0.004(2) C4 0.021(3) 0.025(3) 0.024(3) 0.002(3) 0.015(3) -0.004(3) C5 0.019(3) 0.018(3) 0.016(3) 0.005(2) 0.005(3) -0.004(2) C6 0.019(3) 0.021(3) 0.017(3) 0.003(2) 0.010(2) 0.005(2) C7 0.037(4) 0.031(4) 0.038(3) 0.003(3) 0.028(3) 0.000(3) C8 0.026(3) 0.031(4) 0.030(3) 0.001(3) 0.018(3) -0.005(3) C9 0.023(3) 0.018(3) 0.007(2) 0.0014(19) 0.009(2) 0.001(2) C10 0.024(3) 0.035(3) 0.013(3) 0.002(2) 0.009(3) -0.006(3) C11 0.016(2) 0.022(3) 0.011(2) 0.000(3) 0.004(2) 0.000(3) C12 0.012(3) 0.017(3) 0.024(3) -0.002(2) 0.008(3) -0.001(2) C13 0.020(3) 0.034(3) 0.023(3) 0.000(3) 0.013(3) -0.007(3) C14 0.012(3) 0.023(3) 0.017(3) -0.003(2) 0.009(2) -0.005(2) C15 0.016(3) 0.018(3) 0.019(3) 0.002(2) 0.003(2) 0.001(2) C16 0.019(3) 0.025(3) 0.021(2) -0.002(4) 0.011(2) -0.001(4) C17 0.023(3) 0.032(3) 0.019(3) 0.001(3) 0.011(3) -0.009(3) C18 0.022(3) 0.021(3) 0.021(3) 0.002(2) 0.008(3) -0.002(3) C19 0.023(3) 0.023(3) 0.015(3) -0.002(2) 0.010(3) -0.003(2) C20 0.041(4) 0.041(4) 0.029(3) 0.002(3) 0.021(3) 0.011(3) C21 0.056(4) 0.032(4) 0.028(3) 0.009(3) 0.018(3) 0.003(3) C22 0.011(3) 0.015(3) 0.023(3) -0.005(2) 0.003(2) -0.004(2) C23 0.009(3) 0.019(3) 0.015(3) -0.003(2) 0.004(2) -0.005(2) C24 0.012(3) 0.018(3) 0.023(3) 0.004(2) -0.001(3) 0.000(2) C25 0.018(3) 0.029(3) 0.010(2) -0.002(3) 0.006(2) 0.002(3) C26 0.022(3) 0.027(3) 0.003(2) -0.002(2) 0.005(2) -0.008(2) C27 0.039(4) 0.024(3) 0.036(4) -0.006(3) 0.013(3) -0.003(3) C28 0.027(3) 0.034(4) 0.018(3) -0.002(3) 0.008(2) -0.007(3) C29 0.024(3) 0.027(3) 0.026(3) 0.002(3) -0.003(3) 0.008(3) C30 0.016(3) 0.055(4) 0.024(3) -0.005(3) 0.008(3) 0.002(3) C31 0.029(4) 0.044(3) 0.023(3) -0.004(3) 0.011(3) -0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N1 2.050(4) . ? Ru1 N2 2.051(4) . ? Ru1 C22 2.187(5) . ? Ru1 C25 2.208(4) . ? Ru1 C24 2.224(5) . ? Ru1 C26 2.235(5) . ? Ru1 C23 2.266(5) . ? Ru1 Cl1 2.4512(13) . ? N1 C9 1.332(6) . ? N1 C1 1.450(6) . ? N2 C12 1.329(6) . ? N2 C14 1.444(6) . ? C1 C2 1.385(6) . ? C1 C6 1.385(6) . ? C2 C3 1.393(6) . ? C2 H2 0.9500 . ? C3 C4 1.384(6) . ? C3 C7 1.512(6) . ? C4 C5 1.382(6) . ? C4 H4 0.9500 . ? C5 C6 1.394(6) . ? C5 C8 1.510(6) . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.381(6) . ? C9 C10 1.512(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.382(6) . ? C11 H11 0.9500 . ? C12 C13 1.520(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.383(6) . ? C14 C15 1.390(6) . ? C15 C16 1.392(6) . ? C15 H15 0.9500 . ? C16 C17 1.367(7) . ? C16 C20 1.528(7) . ? C17 C18 1.388(7) . ? C17 H17 0.9500 . ? C18 C19 1.391(6) . ? C18 C21 1.504(6) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C26 1.411(6) . ? C22 C23 1.415(6) . ? C22 C27 1.502(6) . ? C23 C24 1.399(6) . ? C23 C28 1.501(6) . ? C24 C25 1.449(6) . ? C24 C29 1.498(6) . ? C25 C26 1.410(7) . ? C25 C30 1.505(6) . ? C26 C31 1.507(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N2 87.85(16) . . ? N1 Ru1 C22 116.72(17) . . ? N2 Ru1 C22 112.96(17) . . ? N1 Ru1 C25 115.75(16) . . ? N2 Ru1 C25 155.85(16) . . ? C22 Ru1 C25 62.48(19) . . ? N1 Ru1 C24 153.30(18) . . ? N2 Ru1 C24 117.76(18) . . ? C22 Ru1 C24 62.33(19) . . ? C25 Ru1 C24 38.16(17) . . ? N1 Ru1 C26 100.00(16) . . ? N2 Ru1 C26 149.15(16) . . ? C22 Ru1 C26 37.21(16) . . ? C25 Ru1 C26 37.00(18) . . ? C24 Ru1 C26 62.36(18) . . ? N1 Ru1 C23 153.43(15) . . ? N2 Ru1 C23 99.75(17) . . ? C22 Ru1 C23 37.00(16) . . ? C25 Ru1 C23 61.67(17) . . ? C24 Ru1 C23 36.30(16) . . ? C26 Ru1 C23 61.24(16) . . ? N1 Ru1 Cl1 87.66(10) . . ? N2 Ru1 Cl1 86.19(10) . . ? C22 Ru1 Cl1 148.39(13) . . ? C25 Ru1 Cl1 89.56(15) . . ? C24 Ru1 Cl1 86.74(13) . . ? C26 Ru1 Cl1 123.64(14) . . ? C23 Ru1 Cl1 118.05(12) . . ? C9 N1 C1 116.0(4) . . ? C9 N1 Ru1 127.6(3) . . ? C1 N1 Ru1 116.0(3) . . ? C12 N2 C14 116.4(4) . . ? C12 N2 Ru1 126.4(3) . . ? C14 N2 Ru1 116.5(3) . . ? C2 C1 C6 120.4(4) . . ? C2 C1 N1 117.6(4) . . ? C6 C1 N1 122.0(4) . . ? C1 C2 C3 120.7(5) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 117.9(5) . . ? C4 C3 C7 121.4(4) . . ? C2 C3 C7 120.7(4) . . ? C5 C4 C3 122.3(5) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 119.0(4) . . ? C4 C5 C8 120.6(4) . . ? C6 C5 C8 120.2(5) . . ? C1 C6 C5 119.6(5) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C11 123.2(4) . . ? N1 C9 C10 120.6(4) . . ? C11 C9 C10 116.2(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C12 128.1(5) . . ? C9 C11 H11 115.9 . . ? C12 C11 H11 115.9 . . ? N2 C12 C11 123.9(4) . . ? N2 C12 C13 119.1(4) . . ? C11 C12 C13 117.0(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 119.8(4) . . ? C19 C14 N2 120.3(4) . . ? C15 C14 N2 120.0(4) . . ? C14 C15 C16 119.7(5) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 119.6(5) . . ? C17 C16 C20 120.4(4) . . ? C15 C16 C20 119.9(5) . . ? C16 C17 C18 121.8(5) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 118.3(5) . . ? C17 C18 C21 121.1(5) . . ? C19 C18 C21 120.6(5) . . ? C14 C19 C18 120.8(5) . . ? C14 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C26 C22 C23 108.4(4) . . ? C26 C22 C27 126.0(5) . . ? C23 C22 C27 125.2(5) . . ? C26 C22 Ru1 73.2(3) . . ? C23 C22 Ru1 74.6(3) . . ? C27 C22 Ru1 123.9(3) . . ? C24 C23 C22 108.4(4) . . ? C24 C23 C28 125.9(4) . . ? C22 C23 C28 124.8(4) . . ? C24 C23 Ru1 70.2(3) . . ? C22 C23 Ru1 68.4(3) . . ? C28 C23 Ru1 135.5(3) . . ? C23 C24 C25 107.3(4) . . ? C23 C24 C29 126.6(5) . . ? C25 C24 C29 125.8(5) . . ? C23 C24 Ru1 73.5(3) . . ? C25 C24 Ru1 70.3(3) . . ? C29 C24 Ru1 127.0(4) . . ? C26 C25 C24 107.7(4) . . ? C26 C25 C30 127.2(5) . . ? C24 C25 C30 124.5(5) . . ? C26 C25 Ru1 72.5(3) . . ? C24 C25 Ru1 71.5(3) . . ? C30 C25 Ru1 128.2(3) . . ? C25 C26 C22 107.8(4) . . ? C25 C26 C31 125.5(5) . . ? C22 C26 C31 125.7(5) . . ? C25 C26 Ru1 70.5(3) . . ? C22 C26 Ru1 69.5(3) . . ? C31 C26 Ru1 134.7(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru1 N1 C9 12.8(4) . . . . ? C22 Ru1 N1 C9 127.6(4) . . . . ? C25 Ru1 N1 C9 -161.8(4) . . . . ? C24 Ru1 N1 C9 -151.4(4) . . . . ? C26 Ru1 N1 C9 162.8(4) . . . . ? C23 Ru1 N1 C9 120.5(4) . . . . ? Cl1 Ru1 N1 C9 -73.4(4) . . . . ? N2 Ru1 N1 C1 -175.5(3) . . . . ? C22 Ru1 N1 C1 -60.8(4) . . . . ? C25 Ru1 N1 C1 9.8(4) . . . . ? C24 Ru1 N1 C1 20.2(5) . . . . ? C26 Ru1 N1 C1 -25.6(3) . . . . ? C23 Ru1 N1 C1 -67.8(5) . . . . ? Cl1 Ru1 N1 C1 98.2(3) . . . . ? N1 Ru1 N2 C12 -18.1(4) . . . . ? C22 Ru1 N2 C12 -136.3(4) . . . . ? C25 Ru1 N2 C12 150.1(4) . . . . ? C24 Ru1 N2 C12 154.0(4) . . . . ? C26 Ru1 N2 C12 -124.1(4) . . . . ? C23 Ru1 N2 C12 -172.5(4) . . . . ? Cl1 Ru1 N2 C12 69.7(4) . . . . ? N1 Ru1 N2 C14 171.4(3) . . . . ? C22 Ru1 N2 C14 53.2(3) . . . . ? C25 Ru1 N2 C14 -20.4(6) . . . . ? C24 Ru1 N2 C14 -16.5(4) . . . . ? C26 Ru1 N2 C14 65.4(4) . . . . ? C23 Ru1 N2 C14 17.1(3) . . . . ? Cl1 Ru1 N2 C14 -100.8(3) . . . . ? C9 N1 C1 C2 99.4(5) . . . . ? Ru1 N1 C1 C2 -73.2(5) . . . . ? C9 N1 C1 C6 -82.7(6) . . . . ? Ru1 N1 C1 C6 104.6(5) . . . . ? C6 C1 C2 C3 -0.6(7) . . . . ? N1 C1 C2 C3 177.2(4) . . . . ? C1 C2 C3 C4 -0.1(7) . . . . ? C1 C2 C3 C7 180.0(5) . . . . ? C2 C3 C4 C5 0.6(8) . . . . ? C7 C3 C4 C5 -179.4(5) . . . . ? C3 C4 C5 C6 -0.5(8) . . . . ? C3 C4 C5 C8 -175.9(5) . . . . ? C2 C1 C6 C5 0.8(7) . . . . ? N1 C1 C6 C5 -177.0(4) . . . . ? C4 C5 C6 C1 -0.2(7) . . . . ? C8 C5 C6 C1 175.2(5) . . . . ? C1 N1 C9 C11 -175.1(4) . . . . ? Ru1 N1 C9 C11 -3.5(7) . . . . ? C1 N1 C9 C10 5.2(6) . . . . ? Ru1 N1 C9 C10 176.8(3) . . . . ? N1 C9 C11 C12 -7.8(8) . . . . ? C10 C9 C11 C12 171.8(5) . . . . ? C14 N2 C12 C11 -175.0(4) . . . . ? Ru1 N2 C12 C11 14.6(7) . . . . ? C14 N2 C12 C13 3.0(6) . . . . ? Ru1 N2 C12 C13 -167.5(3) . . . . ? C9 C11 C12 N2 1.9(8) . . . . ? C9 C11 C12 C13 -176.1(5) . . . . ? C12 N2 C14 C19 -94.9(5) . . . . ? Ru1 N2 C14 C19 76.6(5) . . . . ? C12 N2 C14 C15 84.7(5) . . . . ? Ru1 N2 C14 C15 -103.8(4) . . . . ? C19 C14 C15 C16 -1.6(7) . . . . ? N2 C14 C15 C16 178.8(4) . . . . ? C14 C15 C16 C17 1.8(7) . . . . ? C14 C15 C16 C20 -176.8(4) . . . . ? C15 C16 C17 C18 -0.9(8) . . . . ? C20 C16 C17 C18 177.7(5) . . . . ? C16 C17 C18 C19 -0.2(8) . . . . ? C16 C17 C18 C21 -180.0(5) . . . . ? C15 C14 C19 C18 0.5(7) . . . . ? N2 C14 C19 C18 -179.9(4) . . . . ? C17 C18 C19 C14 0.4(7) . . . . ? C21 C18 C19 C14 -179.8(5) . . . . ? N1 Ru1 C22 C26 70.0(3) . . . . ? N2 Ru1 C22 C26 169.7(3) . . . . ? C25 Ru1 C22 C26 -36.6(3) . . . . ? C24 Ru1 C22 C26 -79.9(3) . . . . ? C23 Ru1 C22 C26 -115.2(4) . . . . ? Cl1 Ru1 C22 C26 -66.9(4) . . . . ? N1 Ru1 C22 C23 -174.8(3) . . . . ? N2 Ru1 C22 C23 -75.1(3) . . . . ? C25 Ru1 C22 C23 78.6(3) . . . . ? C24 Ru1 C22 C23 35.3(3) . . . . ? C26 Ru1 C22 C23 115.2(4) . . . . ? Cl1 Ru1 C22 C23 48.3(4) . . . . ? N1 Ru1 C22 C27 -52.5(5) . . . . ? N2 Ru1 C22 C27 47.2(5) . . . . ? C25 Ru1 C22 C27 -159.1(5) . . . . ? C24 Ru1 C22 C27 157.6(5) . . . . ? C26 Ru1 C22 C27 -122.5(6) . . . . ? C23 Ru1 C22 C27 122.3(5) . . . . ? Cl1 Ru1 C22 C27 170.6(3) . . . . ? C26 C22 C23 C24 7.0(6) . . . . ? C27 C22 C23 C24 -179.9(5) . . . . ? Ru1 C22 C23 C24 -59.0(4) . . . . ? C26 C22 C23 C28 -162.7(4) . . . . ? C27 C22 C23 C28 10.4(8) . . . . ? Ru1 C22 C23 C28 131.3(4) . . . . ? C26 C22 C23 Ru1 66.0(3) . . . . ? C27 C22 C23 Ru1 -120.9(5) . . . . ? N1 Ru1 C23 C24 130.7(4) . . . . ? N2 Ru1 C23 C24 -124.4(3) . . . . ? C22 Ru1 C23 C24 120.2(4) . . . . ? C25 Ru1 C23 C24 39.2(3) . . . . ? C26 Ru1 C23 C24 81.6(3) . . . . ? Cl1 Ru1 C23 C24 -33.5(3) . . . . ? N1 Ru1 C23 C22 10.5(5) . . . . ? N2 Ru1 C23 C22 115.4(3) . . . . ? C25 Ru1 C23 C22 -81.0(3) . . . . ? C24 Ru1 C23 C22 -120.2(4) . . . . ? C26 Ru1 C23 C22 -38.6(3) . . . . ? Cl1 Ru1 C23 C22 -153.7(2) . . . . ? N1 Ru1 C23 C28 -107.8(5) . . . . ? N2 Ru1 C23 C28 -2.8(5) . . . . ? C22 Ru1 C23 C28 -118.3(6) . . . . ? C25 Ru1 C23 C28 160.8(5) . . . . ? C24 Ru1 C23 C28 121.6(6) . . . . ? C26 Ru1 C23 C28 -156.9(5) . . . . ? Cl1 Ru1 C23 C28 88.1(4) . . . . ? C22 C23 C24 C25 -4.7(5) . . . . ? C28 C23 C24 C25 164.8(4) . . . . ? Ru1 C23 C24 C25 -62.6(3) . . . . ? C22 C23 C24 C29 -177.9(5) . . . . ? C28 C23 C24 C29 -8.4(8) . . . . ? Ru1 C23 C24 C29 124.2(5) . . . . ? C22 C23 C24 Ru1 57.9(3) . . . . ? C28 C23 C24 Ru1 -132.5(5) . . . . ? N1 Ru1 C24 C23 -131.0(3) . . . . ? N2 Ru1 C24 C23 66.8(3) . . . . ? C22 Ru1 C24 C23 -36.0(3) . . . . ? C25 Ru1 C24 C23 -115.8(4) . . . . ? C26 Ru1 C24 C23 -78.2(3) . . . . ? Cl1 Ru1 C24 C23 150.8(3) . . . . ? N1 Ru1 C24 C25 -15.2(5) . . . . ? N2 Ru1 C24 C25 -177.4(3) . . . . ? C22 Ru1 C24 C25 79.8(3) . . . . ? C26 Ru1 C24 C25 37.6(3) . . . . ? C23 Ru1 C24 C25 115.8(4) . . . . ? Cl1 Ru1 C24 C25 -93.4(3) . . . . ? N1 Ru1 C24 C29 105.3(5) . . . . ? N2 Ru1 C24 C29 -56.9(5) . . . . ? C22 Ru1 C24 C29 -159.7(5) . . . . ? C25 Ru1 C24 C29 120.5(6) . . . . ? C26 Ru1 C24 C29 158.1(5) . . . . ? C23 Ru1 C24 C29 -123.7(6) . . . . ? Cl1 Ru1 C24 C29 27.1(4) . . . . ? C23 C24 C25 C26 0.8(5) . . . . ? C29 C24 C25 C26 174.0(5) . . . . ? Ru1 C24 C25 C26 -64.0(3) . . . . ? C23 C24 C25 C30 -171.1(5) . . . . ? C29 C24 C25 C30 2.2(8) . . . . ? Ru1 C24 C25 C30 124.2(5) . . . . ? C23 C24 C25 Ru1 64.7(3) . . . . ? C29 C24 C25 Ru1 -122.0(5) . . . . ? N1 Ru1 C25 C26 -71.4(3) . . . . ? N2 Ru1 C25 C26 121.8(4) . . . . ? C22 Ru1 C25 C26 36.8(3) . . . . ? C24 Ru1 C25 C26 116.2(4) . . . . ? C23 Ru1 C25 C26 78.9(3) . . . . ? Cl1 Ru1 C25 C26 -158.5(2) . . . . ? N1 Ru1 C25 C24 172.5(3) . . . . ? N2 Ru1 C25 C24 5.6(6) . . . . ? C22 Ru1 C25 C24 -79.4(3) . . . . ? C26 Ru1 C25 C24 -116.2(4) . . . . ? C23 Ru1 C25 C24 -37.3(3) . . . . ? Cl1 Ru1 C25 C24 85.3(3) . . . . ? N1 Ru1 C25 C30 52.7(5) . . . . ? N2 Ru1 C25 C30 -114.2(5) . . . . ? C22 Ru1 C25 C30 160.8(5) . . . . ? C24 Ru1 C25 C30 -119.8(6) . . . . ? C26 Ru1 C25 C30 124.0(6) . . . . ? C23 Ru1 C25 C30 -157.1(5) . . . . ? Cl1 Ru1 C25 C30 -34.5(5) . . . . ? C24 C25 C26 C22 3.5(5) . . . . ? C30 C25 C26 C22 175.0(5) . . . . ? Ru1 C25 C26 C22 -59.8(3) . . . . ? C24 C25 C26 C31 -165.1(5) . . . . ? C30 C25 C26 C31 6.4(8) . . . . ? Ru1 C25 C26 C31 131.6(5) . . . . ? C24 C25 C26 Ru1 63.3(3) . . . . ? C30 C25 C26 Ru1 -125.2(5) . . . . ? C23 C22 C26 C25 -6.4(5) . . . . ? C27 C22 C26 C25 -179.5(5) . . . . ? Ru1 C22 C26 C25 60.4(3) . . . . ? C23 C22 C26 C31 162.1(5) . . . . ? C27 C22 C26 C31 -10.9(8) . . . . ? Ru1 C22 C26 C31 -131.0(5) . . . . ? C23 C22 C26 Ru1 -66.8(3) . . . . ? C27 C22 C26 Ru1 120.1(5) . . . . ? N1 Ru1 C26 C25 119.9(3) . . . . ? N2 Ru1 C26 C25 -137.3(3) . . . . ? C22 Ru1 C26 C25 -118.6(4) . . . . ? C24 Ru1 C26 C25 -38.8(3) . . . . ? C23 Ru1 C26 C25 -80.1(3) . . . . ? Cl1 Ru1 C26 C25 26.1(3) . . . . ? N1 Ru1 C26 C22 -121.5(3) . . . . ? N2 Ru1 C26 C22 -18.7(5) . . . . ? C25 Ru1 C26 C22 118.6(4) . . . . ? C24 Ru1 C26 C22 79.8(3) . . . . ? C23 Ru1 C26 C22 38.4(3) . . . . ? Cl1 Ru1 C26 C22 144.6(2) . . . . ? N1 Ru1 C26 C31 -1.1(5) . . . . ? N2 Ru1 C26 C31 101.7(5) . . . . ? C22 Ru1 C26 C31 120.4(6) . . . . ? C25 Ru1 C26 C31 -121.0(6) . . . . ? C24 Ru1 C26 C31 -159.8(6) . . . . ? C23 Ru1 C26 C31 158.8(6) . . . . ? Cl1 Ru1 C26 C31 -95.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.954 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.097 data_adp471 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*RuCl((3,5-(CF3)2C6H3NCMe)2CH)' _chemical_melting_point ? _chemical_formula_moiety 'C31 H28 Cl F12 N2 Ru' _chemical_formula_sum 'C31 H28 Cl F12 N2 Ru' _chemical_formula_weight 793.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 30.7359(4) _cell_length_b 27.2804(3) _cell_length_c 15.0300(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12602.5(3) _cell_formula_units_Z 16 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 57279 _cell_measurement_theta_min 2.6101 _cell_measurement_theta_max 28.7587 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6352 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_T_min 0.81391 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_measurement_method '\w and \p scans' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_detector_area_resol_mean 8.2812 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102336 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 21963 _reflns_number_gt 20014 _reflns_threshold_expression I>2/s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick G.M., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick G.M., 2008)' _computing_molecular_graphics 'ORTEP-3 for windows 2.02 (Farrugia, 2008)' _computing_publication_material 'WinGX 1.80.05 (Farrugia, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Structure features four crystallographically independent molecules. A number of CF3 substituents are positioned disordered over multiple sites. A split refinement method used employed where the occupancy was allowed to refine. Some of the fluorine atoms are prolate due diffuse electron density. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+30.6950P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 21963 _refine_ls_number_parameters 1780 _refine_ls_number_restraints 83 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.199 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.07212(16) 0.60472(17) 0.1887(4) 0.0177(11) Uani 1 1 d . . . C2 C 0.04783(17) 0.63932(19) 0.1432(4) 0.0209(12) Uani 1 1 d . . . H2 H 0.0293 0.6295 0.0960 0.025 Uiso 1 1 calc R . . C3 C 0.05064(17) 0.68765(19) 0.1665(4) 0.0236(12) Uani 1 1 d . . . C4 C 0.07802(15) 0.70363(18) 0.2347(4) 0.0234(12) Uani 1 1 d . . . H4 H 0.0801 0.7374 0.2496 0.028 Uiso 1 1 calc R . . C5 C 0.10223(17) 0.66845(18) 0.2802(4) 0.0214(12) Uani 1 1 d . . . C6 C 0.09926(16) 0.61945(18) 0.2583(4) 0.0208(11) Uani 1 1 d . . . H6 H 0.1156 0.5958 0.2905 0.025 Uiso 1 1 calc R . . C7 C 0.0225(2) 0.7237(2) 0.1192(5) 0.0363(15) Uani 1 1 d . . . C8 C 0.1325(2) 0.6834(2) 0.3539(5) 0.0377(16) Uani 1 1 d . . . C9 C 0.09341(16) 0.54214(19) 0.0900(4) 0.0149(12) Uani 1 1 d . . . C10 C 0.11820(17) 0.58145(18) 0.0401(4) 0.0216(12) Uani 1 1 d . . . H10A H 0.0976 0.6048 0.0140 0.032 Uiso 1 1 calc R . . H10B H 0.1355 0.5663 -0.0073 0.032 Uiso 1 1 calc R . . H10C H 0.1376 0.5987 0.0813 0.032 Uiso 1 1 calc R . . C11 C 0.09726(19) 0.4946(2) 0.0598(5) 0.0199(13) Uani 1 1 d . . . H11 H 0.1137 0.4910 0.0068 0.024 Uiso 1 1 calc R . . C12 C 0.08115(17) 0.45176(19) 0.0941(5) 0.0182(12) Uani 1 1 d . . . C13 C 0.04430(16) 0.40177(17) 0.1958(4) 0.0170(11) Uani 1 1 d . . . C14 C 0.09455(19) 0.40515(19) 0.0480(5) 0.0236(13) Uani 1 1 d . . . H14A H 0.1098 0.3839 0.0903 0.035 Uiso 1 1 calc R . . H14B H 0.1139 0.4130 -0.0017 0.035 Uiso 1 1 calc R . . H14C H 0.0686 0.3883 0.0256 0.035 Uiso 1 1 calc R . . C15 C 0.01177(18) 0.37559(19) 0.1526(4) 0.0239(12) Uani 1 1 d . . . H15 H -0.0034 0.3899 0.1040 0.029 Uiso 1 1 calc R . . C16 C 0.00159(18) 0.3285(2) 0.1808(4) 0.0272(13) Uani 1 1 d . A . C17 C 0.02214(17) 0.30710(19) 0.2526(5) 0.0292(12) Uani 1 1 d . . . H17 H 0.0145 0.2751 0.2718 0.035 Uiso 1 1 calc R . . C18 C 0.05455(18) 0.33388(19) 0.2964(4) 0.0234(12) Uani 1 1 d . . . C19 C 0.06507(16) 0.38103(18) 0.2692(4) 0.0207(12) Uani 1 1 d . . . H19 H 0.0865 0.3992 0.3007 0.025 Uiso 1 1 calc R . . C20 C -0.0344(2) 0.3020(2) 0.1322(5) 0.0396(16) Uani 1 1 d DU . . C21 C 0.0771(2) 0.3120(2) 0.3748(5) 0.0370(16) Uani 1 1 d . . . C22 C 0.00568(17) 0.5184(2) 0.3828(4) 0.0205(12) Uani 1 1 d . . . C23 C -0.01125(18) 0.47576(19) 0.3425(4) 0.0207(12) Uani 1 1 d . . . C24 C -0.03252(17) 0.4895(2) 0.2638(5) 0.0212(13) Uani 1 1 d . . . C25 C -0.02767(15) 0.54143(17) 0.2526(5) 0.0176(10) Uani 1 1 d . . . C26 C -0.00501(17) 0.55971(18) 0.3278(4) 0.0185(11) Uani 1 1 d . . . C27 C 0.02690(19) 0.5216(2) 0.4717(5) 0.0312(13) Uani 1 1 d . . . H27A H 0.0054 0.5148 0.5182 0.047 Uiso 1 1 calc R . . H27B H 0.0388 0.5546 0.4802 0.047 Uiso 1 1 calc R . . H27C H 0.0505 0.4974 0.4753 0.047 Uiso 1 1 calc R . . C28 C -0.0131(2) 0.4268(2) 0.3889(5) 0.0395(16) Uani 1 1 d . . . H28A H -0.0325 0.4290 0.4405 0.059 Uiso 1 1 calc R . . H28B H 0.0162 0.4176 0.4087 0.059 Uiso 1 1 calc R . . H28C H -0.0242 0.4019 0.3476 0.059 Uiso 1 1 calc R . . C29 C -0.06050(18) 0.4581(2) 0.2063(5) 0.0286(14) Uani 1 1 d . . . H29A H -0.0538 0.4235 0.2174 0.043 Uiso 1 1 calc R . . H29B H -0.0550 0.4658 0.1436 0.043 Uiso 1 1 calc R . . H29C H -0.0912 0.4643 0.2201 0.043 Uiso 1 1 calc R . . C30 C -0.04961(18) 0.5720(2) 0.1830(5) 0.0308(14) Uani 1 1 d . . . H30A H -0.0431 0.5586 0.1239 0.046 Uiso 1 1 calc R . . H30B H -0.0390 0.6058 0.1867 0.046 Uiso 1 1 calc R . . H30C H -0.0811 0.5715 0.1927 0.046 Uiso 1 1 calc R . . C31 C 0.0001(2) 0.6127(2) 0.3528(5) 0.0398(16) Uani 1 1 d . . . H31A H -0.0245 0.6229 0.3899 0.060 Uiso 1 1 calc R . . H31B H 0.0009 0.6328 0.2988 0.060 Uiso 1 1 calc R . . H31C H 0.0272 0.6171 0.3861 0.060 Uiso 1 1 calc R . . C32 C 0.30480(17) 0.58659(18) 0.1975(4) 0.0196(12) Uani 1 1 d . . . C33 C 0.27468(17) 0.61586(17) 0.1554(4) 0.0218(12) Uani 1 1 d . . . H33 H 0.2574 0.6030 0.1084 0.026 Uiso 1 1 calc R . . C34 C 0.2696(2) 0.66519(19) 0.1826(4) 0.0347(15) Uani 1 1 d . B . C35 C 0.2962(2) 0.68411(19) 0.2473(5) 0.0423(16) Uani 1 1 d . . . H35 H 0.2937 0.7176 0.2641 0.051 Uiso 1 1 calc R . . C36 C 0.3264(2) 0.6547(2) 0.2877(4) 0.0310(14) Uani 1 1 d . . . C37 C 0.33053(18) 0.60551(18) 0.2637(4) 0.0252(13) Uani 1 1 d . . . H37 H 0.3511 0.5852 0.2931 0.030 Uiso 1 1 calc R . . C38 C 0.2355(3) 0.6961(2) 0.1380(6) 0.057(2) Uani 1 1 d . . . C39 C 0.3540(2) 0.6761(2) 0.3590(5) 0.0427(17) Uani 1 1 d . . . C40 C 0.33578(17) 0.53254(18) 0.0939(5) 0.0170(12) Uani 1 1 d . . . C41 C 0.35328(19) 0.5779(2) 0.0476(5) 0.0263(14) Uani 1 1 d . . . H41A H 0.3289 0.5983 0.0276 0.039 Uiso 1 1 calc R . . H41B H 0.3708 0.5680 -0.0038 0.039 Uiso 1 1 calc R . . H41C H 0.3714 0.5966 0.0892 0.039 Uiso 1 1 calc R . . C42 C 0.34698(18) 0.4883(2) 0.0581(5) 0.0182(13) Uani 1 1 d . . . H42 H 0.3630 0.4901 0.0041 0.022 Uiso 1 1 calc R . . C43 C 0.33866(17) 0.44129(19) 0.0883(4) 0.0174(12) Uani 1 1 d . . . C44 C 0.35822(18) 0.40009(19) 0.0361(4) 0.0244(13) Uani 1 1 d . . . H44A H 0.3776 0.3810 0.0746 0.037 Uiso 1 1 calc R . . H44B H 0.3749 0.4134 -0.0140 0.037 Uiso 1 1 calc R . . H44C H 0.3350 0.3788 0.0135 0.037 Uiso 1 1 calc R . . C45 C 0.31077(17) 0.38237(18) 0.1861(4) 0.0200(12) Uani 1 1 d . . . C46 C 0.28190(17) 0.35122(19) 0.1411(4) 0.0247(13) Uani 1 1 d . . . H46 H 0.2643 0.3639 0.0944 0.030 Uiso 1 1 calc R . . C47 C 0.2788(2) 0.3027(2) 0.1639(5) 0.0396(16) Uani 1 1 d . C . C48 C 0.3046(2) 0.2833(2) 0.2295(5) 0.0482(19) Uani 1 1 d . . . H48 H 0.3030 0.2494 0.2433 0.058 Uiso 1 1 calc R . . C49 C 0.33311(18) 0.3139(2) 0.2761(4) 0.0317(14) Uani 1 1 d . . . C50 C 0.33563(16) 0.36309(17) 0.2542(5) 0.0237(11) Uani 1 1 d . . . H50 H 0.3547 0.3839 0.2865 0.028 Uiso 1 1 calc R . . C51 C 0.2443(4) 0.2731(3) 0.1175(8) 0.077(4) Uani 1 1 d . . . C52 C 0.3608(3) 0.2954(3) 0.3511(7) 0.060(2) Uani 1 1 d . . . C53 C 0.25660(18) 0.4784(2) 0.3851(4) 0.0295(14) Uani 1 1 d . . . C54 C 0.24205(17) 0.4375(2) 0.3353(4) 0.0240(12) Uani 1 1 d . . . C55 C 0.21932(16) 0.45673(19) 0.2589(4) 0.0199(11) Uani 1 1 d . . . C56 C 0.22012(18) 0.5087(2) 0.2666(4) 0.0220(13) Uani 1 1 d . . . C57 C 0.24344(19) 0.5218(2) 0.3433(5) 0.0263(14) Uani 1 1 d . . . C58 C 0.2781(2) 0.4739(3) 0.4755(5) 0.0426(16) Uani 1 1 d U . . H58A H 0.2561 0.4769 0.5222 0.064 Uiso 1 1 calc R . . H58B H 0.2998 0.5000 0.4824 0.064 Uiso 1 1 calc R . . H58C H 0.2925 0.4420 0.4802 0.064 Uiso 1 1 calc R . . C59 C 0.2433(2) 0.3840(2) 0.3621(5) 0.0471(19) Uani 1 1 d . . . H59A H 0.2704 0.3773 0.3943 0.071 Uiso 1 1 calc R . . H59B H 0.2420 0.3634 0.3088 0.071 Uiso 1 1 calc R . . H59C H 0.2185 0.3767 0.4007 0.071 Uiso 1 1 calc R . . C60 C 0.19290(18) 0.4270(2) 0.1960(4) 0.0265(13) Uani 1 1 d . . . H60A H 0.1629 0.4251 0.2176 0.040 Uiso 1 1 calc R . . H60B H 0.2051 0.3939 0.1919 0.040 Uiso 1 1 calc R . . H60C H 0.1933 0.4424 0.1371 0.040 Uiso 1 1 calc R . . C61 C 0.19475(18) 0.5415(2) 0.2047(4) 0.0253(13) Uani 1 1 d . . . H61A H 0.2032 0.5347 0.1430 0.038 Uiso 1 1 calc R . . H61B H 0.2010 0.5759 0.2187 0.038 Uiso 1 1 calc R . . H61C H 0.1636 0.5353 0.2120 0.038 Uiso 1 1 calc R . . C62 C 0.2470(2) 0.5715(3) 0.3850(5) 0.0460(18) Uani 1 1 d . . . H62A H 0.2283 0.5730 0.4376 0.069 Uiso 1 1 calc R . . H62B H 0.2379 0.5965 0.3420 0.069 Uiso 1 1 calc R . . H62C H 0.2773 0.5775 0.4025 0.069 Uiso 1 1 calc R . . C63 C 0.17497(17) 0.10996(19) 0.5289(4) 0.0239(12) Uani 1 1 d . . . C64 C 0.14396(18) 0.1380(2) 0.5724(4) 0.0291(13) Uani 1 1 d . . . H64 H 0.1277 0.1244 0.6200 0.035 Uiso 1 1 calc R . . C65 C 0.1368(2) 0.1862(2) 0.5458(5) 0.0417(17) Uani 1 1 d . . . C66 C 0.1605(2) 0.2067(2) 0.4757(5) 0.0520(19) Uani 1 1 d . . . H66 H 0.1556 0.2396 0.4575 0.062 Uiso 1 1 calc R . . C67 C 0.1910(2) 0.1781(2) 0.4334(5) 0.0456(18) Uani 1 1 d . . . C68 C 0.19841(19) 0.1299(2) 0.4595(5) 0.0336(15) Uani 1 1 d . . . H68 H 0.2196 0.1107 0.4295 0.040 Uiso 1 1 calc R . . C69 C 0.1017(3) 0.2146(3) 0.5925(5) 0.053(2) Uani 1 1 d . . . C70 C 0.2161(3) 0.1980(3) 0.3555(6) 0.072(3) Uani 1 1 d . . . C71 C 0.20808(18) 0.05732(19) 0.6313(5) 0.0194(13) Uani 1 1 d . . . C72 C 0.2236(2) 0.1028(2) 0.6807(5) 0.0293(14) Uani 1 1 d . . . H72A H 0.2379 0.1251 0.6389 0.044 Uiso 1 1 calc R . . H72B H 0.2442 0.0932 0.7273 0.044 Uiso 1 1 calc R . . H72C H 0.1985 0.1194 0.7078 0.044 Uiso 1 1 calc R . . C73 C 0.2219(2) 0.01252(19) 0.6667(5) 0.0173(13) Uani 1 1 d . . . H73 H 0.2379 0.0140 0.7208 0.021 Uiso 1 1 calc R . . C74 C 0.21477(17) -0.0344(2) 0.6314(5) 0.0185(13) Uani 1 1 d . . . C75 C 0.23668(17) -0.07584(18) 0.6807(4) 0.0197(12) Uani 1 1 d . . . H75A H 0.2149 -0.1004 0.6973 0.030 Uiso 1 1 calc R . . H75B H 0.2506 -0.0630 0.7345 0.030 Uiso 1 1 calc R . . H75C H 0.2587 -0.0909 0.6423 0.030 Uiso 1 1 calc R . . C76 C 0.19097(16) -0.09371(18) 0.5314(4) 0.0183(11) Uani 1 1 d . . . C77 C 0.16450(19) -0.1278(2) 0.5736(4) 0.0328(14) Uani 1 1 d . . . H77 H 0.1454 -0.1173 0.6195 0.039 Uiso 1 1 calc R . . C78 C 0.1654(2) -0.1762(2) 0.5504(4) 0.0458(18) Uani 1 1 d . D . C79 C 0.1929(2) -0.1932(2) 0.4868(5) 0.0448(17) Uani 1 1 d . . . H79 H 0.1943 -0.2271 0.4728 0.054 Uiso 1 1 calc R . . C80 C 0.21918(19) -0.1588(2) 0.4425(4) 0.0257(13) Uani 1 1 d . . . C81 C 0.21780(16) -0.11018(17) 0.4634(4) 0.0186(11) Uani 1 1 d . . . H81 H 0.2353 -0.0875 0.4314 0.022 Uiso 1 1 calc R . . C82 C 0.1350(3) -0.2111(3) 0.5984(6) 0.086(4) Uani 1 1 d D . . C83 C 0.24822(19) -0.17611(19) 0.3694(4) 0.0263(12) Uani 1 1 d U . . C84 C 0.1301(2) -0.0004(3) 0.3386(5) 0.0484(19) Uani 1 1 d . . . C85 C 0.11469(18) 0.0418(3) 0.3801(4) 0.0380(16) Uani 1 1 d . . . C86 C 0.09341(18) 0.0262(3) 0.4593(4) 0.0325(15) Uani 1 1 d . . . C87 C 0.09596(17) -0.0253(2) 0.4662(5) 0.0285(13) Uani 1 1 d . . . C88 C 0.11974(18) -0.0418(3) 0.3868(5) 0.0374(15) Uani 1 1 d . . . C89 C 0.1519(2) -0.0010(3) 0.2478(5) 0.063(2) Uani 1 1 d . . . H89A H 0.1681 -0.0317 0.2407 0.094 Uiso 1 1 calc R . . H89B H 0.1719 0.0268 0.2431 0.094 Uiso 1 1 calc R . . H89C H 0.1297 0.0014 0.2012 0.094 Uiso 1 1 calc R . . C90 C 0.1144(2) 0.0925(3) 0.3420(6) 0.066(3) Uani 1 1 d . . . H90A H 0.1424 0.0992 0.3133 0.099 Uiso 1 1 calc R . . H90B H 0.1096 0.1163 0.3898 0.099 Uiso 1 1 calc R . . H90C H 0.0910 0.0953 0.2979 0.099 Uiso 1 1 calc R . . C91 C 0.06463(19) 0.0573(2) 0.5199(5) 0.0375(15) Uani 1 1 d . . . H91A H 0.0341 0.0485 0.5105 0.056 Uiso 1 1 calc R . . H91B H 0.0689 0.0921 0.5060 0.056 Uiso 1 1 calc R . . H91C H 0.0725 0.0513 0.5821 0.056 Uiso 1 1 calc R . . C92 C 0.0737(2) -0.0570(2) 0.5341(5) 0.0420(17) Uani 1 1 d . . . H92A H 0.0797 -0.0442 0.5938 0.063 Uiso 1 1 calc R . . H92B H 0.0846 -0.0906 0.5294 0.063 Uiso 1 1 calc R . . H92C H 0.0423 -0.0567 0.5233 0.063 Uiso 1 1 calc R . . C93 C 0.1247(2) -0.0950(3) 0.3601(6) 0.058(2) Uani 1 1 d . . . H93A H 0.1017 -0.1037 0.3178 0.087 Uiso 1 1 calc R . . H93B H 0.1224 -0.1158 0.4130 0.087 Uiso 1 1 calc R . . H93C H 0.1532 -0.0998 0.3322 0.087 Uiso 1 1 calc R . . C94 C 0.44421(17) 0.11450(17) 0.5375(4) 0.0180(12) Uani 1 1 d . . . C95 C 0.47017(16) 0.13098(19) 0.4675(5) 0.0236(12) Uani 1 1 d . . . H95 H 0.4869 0.1084 0.4338 0.028 Uiso 1 1 calc R . . C96 C 0.47133(17) 0.1805(2) 0.4475(4) 0.0285(13) Uani 1 1 d . . . C97 C 0.4457(2) 0.2140(2) 0.4932(5) 0.0359(15) Uani 1 1 d . . . H97 H 0.4459 0.2476 0.4768 0.043 Uiso 1 1 calc R . . C98 C 0.41989(19) 0.19809(18) 0.5623(4) 0.0276(13) Uani 1 1 d . E . C99 C 0.41925(18) 0.14780(18) 0.5847(5) 0.0230(13) Uani 1 1 d . . . H99 H 0.4016 0.1367 0.6325 0.028 Uiso 1 1 calc R . . C100 C 0.4991(2) 0.1966(3) 0.3703(6) 0.0459(18) Uani 1 1 d . . . C101 C 0.3893(3) 0.2312(2) 0.6112(6) 0.052(2) Uani 1 1 d . . . C102 C 0.46748(18) 0.05256(19) 0.6338(4) 0.0195(12) Uani 1 1 d . . . C103 C 0.49132(19) 0.09197(19) 0.6872(5) 0.0269(13) Uani 1 1 d . . . H10D H 0.5119 0.1091 0.6484 0.040 Uiso 1 1 calc R . . H10E H 0.5071 0.0766 0.7365 0.040 Uiso 1 1 calc R . . H10F H 0.4702 0.1154 0.7110 0.040 Uiso 1 1 calc R . . C104 C 0.4730(2) 0.00514(19) 0.6656(5) 0.0201(13) Uani 1 1 d . . . H104 H 0.4891 0.0020 0.7193 0.024 Uiso 1 1 calc R . . C105 C 0.45769(17) -0.03866(19) 0.6278(4) 0.0162(12) Uani 1 1 d . . . C106 C 0.47282(19) -0.0853(2) 0.6733(5) 0.0269(14) Uani 1 1 d . . . H10G H 0.4475 -0.1051 0.6900 0.040 Uiso 1 1 calc R . . H10H H 0.4894 -0.0769 0.7269 0.040 Uiso 1 1 calc R . . H10I H 0.4913 -0.1040 0.6326 0.040 Uiso 1 1 calc R . . C107 C 0.38035(18) -0.16187(17) 0.5414(4) 0.0226(12) Uani 1 1 d . . . C108 C 0.42115(16) -0.08813(17) 0.5255(4) 0.0143(11) Uani 1 1 d . . . C109 C 0.38878(15) -0.11519(17) 0.5674(4) 0.0171(11) Uani 1 1 d . . . H109 H 0.3725 -0.1010 0.6145 0.021 Uiso 1 1 calc R . . C111 C 0.40383(18) -0.18369(16) 0.4712(5) 0.0274(12) Uani 1 1 d . . . H111 H 0.3977 -0.2162 0.4525 0.033 Uiso 1 1 calc R . . C112 C 0.43554(19) -0.15687(18) 0.4311(4) 0.0249(13) Uani 1 1 d . . . C113 C 0.44469(17) -0.10982(18) 0.4558(4) 0.0206(12) Uani 1 1 d . . . H113 H 0.4668 -0.0919 0.4261 0.025 Uiso 1 1 calc R . . C114 C 0.3466(2) -0.1911(2) 0.5897(5) 0.0360(16) Uani 1 1 d . . . C115 C 0.4600(2) -0.1794(2) 0.3558(5) 0.0417(17) Uani 1 1 d . . . C116 C 0.38107(16) 0.03032(19) 0.3390(4) 0.0182(12) Uani 1 1 d . . . C117 C 0.37044(17) 0.07017(17) 0.3944(4) 0.0170(12) Uani 1 1 d . . . C118 C 0.34729(16) 0.05054(17) 0.4684(5) 0.0210(12) Uani 1 1 d . . . C119 C 0.34423(17) -0.00194(19) 0.4582(4) 0.0178(13) Uani 1 1 d . . . C120 C 0.36580(17) -0.01524(18) 0.3773(5) 0.0179(12) Uani 1 1 d . . . C121 C 0.4035(2) 0.0334(2) 0.2516(5) 0.0323(14) Uani 1 1 d . . . H12A H 0.3819 0.0383 0.2044 0.048 Uiso 1 1 calc R . . H12B H 0.4195 0.0029 0.2406 0.048 Uiso 1 1 calc R . . H12C H 0.4238 0.0611 0.2521 0.048 Uiso 1 1 calc R . . C122 C 0.3746(2) 0.12274(19) 0.3690(5) 0.0315(15) Uani 1 1 d . . . H12D H 0.3488 0.1328 0.3353 0.047 Uiso 1 1 calc R . . H12E H 0.4006 0.1272 0.3322 0.047 Uiso 1 1 calc R . . H12F H 0.3770 0.1428 0.4228 0.047 Uiso 1 1 calc R . . C123 C 0.3225(2) 0.0782(2) 0.5383(5) 0.0318(15) Uani 1 1 d . . . H12G H 0.3353 0.1108 0.5458 0.048 Uiso 1 1 calc R . . H12H H 0.3240 0.0603 0.5948 0.048 Uiso 1 1 calc R . . H12I H 0.2920 0.0814 0.5199 0.048 Uiso 1 1 calc R . . C124 C 0.31641(19) -0.03438(19) 0.5145(5) 0.0251(14) Uani 1 1 d . . . H12J H 0.2858 -0.0257 0.5060 0.038 Uiso 1 1 calc R . . H12K H 0.3243 -0.0301 0.5772 0.038 Uiso 1 1 calc R . . H12L H 0.3210 -0.0686 0.4972 0.038 Uiso 1 1 calc R . . C125 C 0.3667(2) -0.0641(2) 0.3321(5) 0.0299(14) Uani 1 1 d . . . H12M H 0.3642 -0.0901 0.3767 0.045 Uiso 1 1 calc R . . H12N H 0.3942 -0.0678 0.2998 0.045 Uiso 1 1 calc R . . H12O H 0.3424 -0.0664 0.2902 0.045 Uiso 1 1 calc R . . N1 N 0.07037(14) 0.55415(14) 0.1635(3) 0.0162(10) Uani 1 1 d . . . N2 N 0.05584(14) 0.44998(15) 0.1673(3) 0.0172(10) Uani 1 1 d . . . N3 N 0.31117(15) 0.53657(15) 0.1675(4) 0.0179(10) Uani 1 1 d . . . N4 N 0.31478(14) 0.43254(14) 0.1622(4) 0.0140(9) Uani 1 1 d . . . N5 N 0.18363(14) 0.06069(15) 0.5579(4) 0.0191(10) Uani 1 1 d . . . N6 N 0.19162(14) -0.04353(15) 0.5575(3) 0.0165(10) Uani 1 1 d . . . N7 N 0.44463(14) 0.06403(15) 0.5620(4) 0.0172(10) Uani 1 1 d . . . N8 N 0.43249(13) -0.04019(15) 0.5551(4) 0.0154(10) Uani 1 1 d . . . F1 F 0.0253(2) 0.71982(16) 0.0316(4) 0.0830(18) Uani 1 1 d . . . F2 F -0.01919(12) 0.71817(17) 0.1412(5) 0.0727(17) Uani 1 1 d U . . F3 F 0.03170(13) 0.77030(12) 0.1366(3) 0.0453(10) Uani 1 1 d . . . F4 F 0.11330(17) 0.6717(2) 0.4352(4) 0.0627(14) Uani 1 1 d . . . F5 F 0.14049(18) 0.72984(15) 0.3557(4) 0.086(2) Uani 1 1 d . . . F6 F 0.16901(14) 0.6590(2) 0.3554(4) 0.0751(15) Uani 1 1 d . . . F7A F -0.0315(2) 0.3064(2) 0.0470(4) 0.0867(19) Uani 1 1 d . A . F8A F -0.0707(3) 0.3022(7) 0.1750(10) 0.062(5) Uani 0.53(3) 1 d PDU A 1 F8B F -0.0735(3) 0.3273(8) 0.1365(15) 0.072(5) Uani 0.47(3) 1 d PDU A 2 F9A F -0.0307(2) 0.25330(19) 0.1437(5) 0.099(2) Uani 1 1 d . A . F10 F 0.06357(14) 0.33485(15) 0.4514(3) 0.0496(11) Uani 1 1 d . . . F11 F 0.06990(14) 0.26518(12) 0.3855(3) 0.0510(11) Uani 1 1 d . . . F12 F 0.11981(13) 0.31856(14) 0.3721(3) 0.0483(11) Uani 1 1 d . . . F13 F 0.2439(2) 0.6986(2) 0.0493(4) 0.094(2) Uani 1 1 d . B . F14A F 0.2243(8) 0.7363(7) 0.1841(19) 0.054(5) Uani 0.43(5) 1 d PU B 3 F14B F 0.2425(10) 0.7431(4) 0.1556(12) 0.066(5) Uani 0.57(5) 1 d PU B 4 F15 F 0.19791(19) 0.6758(2) 0.1393(5) 0.0948(19) Uani 1 1 d . B . F16 F 0.3601(2) 0.72346(13) 0.3496(3) 0.090(2) Uani 1 1 d . . . F17 F 0.33874(17) 0.66874(16) 0.4394(3) 0.0632(13) Uani 1 1 d . . . F18 F 0.39388(14) 0.65562(15) 0.3597(3) 0.0557(11) Uani 1 1 d . . . F19A F 0.2397(7) 0.2835(9) 0.0392(15) 0.028(7) Uani 0.27(6) 1 d PU C 5 F20A F 0.2029(9) 0.2850(12) 0.1597(15) 0.042(8) Uani 0.27(6) 1 d PU C 5 F19B F 0.2561(13) 0.2749(6) 0.0201(15) 0.092(7) Uani 0.73(6) 1 d P C 6 F20B F 0.2073(7) 0.2893(5) 0.117(4) 0.137(11) Uani 0.73(6) 1 d P C 6 F21 F 0.24892(17) 0.22561(13) 0.1315(3) 0.0716(14) Uani 1 1 d . C . F22 F 0.35749(17) 0.24794(14) 0.3637(4) 0.0836(18) Uani 1 1 d . . . F23 F 0.3487(2) 0.3153(2) 0.4286(4) 0.093(2) Uani 1 1 d . . . F24 F 0.40125(15) 0.3055(2) 0.3424(5) 0.113(3) Uani 1 1 d . . . F25 F 0.1025(2) 0.20773(19) 0.6784(4) 0.0825(19) Uani 1 1 d . . . F26 F 0.06260(14) 0.20261(17) 0.5620(4) 0.0742(16) Uani 1 1 d . . . F27 F 0.10584(13) 0.26252(14) 0.5798(3) 0.0509(10) Uani 1 1 d . . . F28 F 0.2030(2) 0.1757(2) 0.2793(4) 0.0873(19) Uani 1 1 d . . . F29 F 0.21097(19) 0.24600(17) 0.3441(4) 0.098(2) Uani 1 1 d . . . F30 F 0.25796(16) 0.18894(19) 0.3598(5) 0.097(2) Uani 1 1 d . . . F31A F 0.1015(6) -0.2182(7) 0.5481(15) 0.091(7) Uani 0.44(3) 1 d PDU D 7 F31B F 0.0927(4) -0.1955(7) 0.5961(14) 0.106(6) Uani 0.56(3) 1 d PDU D 8 F32 F 0.1382(2) -0.20732(19) 0.6829(4) 0.102(2) Uani 1 1 d . D . F33 F 0.1458(3) -0.25840(19) 0.5824(4) 0.122(3) Uani 1 1 d . D . F34 F 0.23141(16) -0.17051(18) 0.2891(3) 0.0583(12) Uani 1 1 d . . . F35 F 0.28557(11) -0.15098(14) 0.3666(3) 0.0448(10) Uani 1 1 d . . . F36 F 0.25812(17) -0.22322(13) 0.3772(3) 0.0691(14) Uani 1 1 d . . . F37 F 0.39537(16) 0.27850(13) 0.5919(3) 0.0675(14) Uani 1 1 d . E . F38A F 0.3462(3) 0.2224(5) 0.576(2) 0.072(7) Uani 0.58(4) 1 d P E 9 F38B F 0.3520(8) 0.2157(5) 0.630(2) 0.068(5) Uani 0.42(4) 1 d PU E 10 F39 F 0.3960(3) 0.22818(18) 0.6996(5) 0.096(2) Uani 1 1 d . E . F40 F 0.4878(3) 0.1777(3) 0.2980(5) 0.115(3) Uani 1 1 d . . . F41 F 0.54024(15) 0.1833(3) 0.3799(5) 0.139(4) Uani 1 1 d . . . F42 F 0.49919(19) 0.24343(17) 0.3590(4) 0.0919(18) Uani 1 1 d . . . F43 F 0.30821(13) -0.16989(17) 0.5849(4) 0.0686(15) Uani 1 1 d . . . F44 F 0.3409(2) -0.23444(17) 0.5604(5) 0.128(3) Uani 1 1 d . . . F45 F 0.35420(17) -0.1950(2) 0.6745(4) 0.089(2) Uani 1 1 d . . . F46 F 0.44700(15) -0.16388(16) 0.2771(3) 0.0536(12) Uani 1 1 d . . . F47 F 0.4572(2) -0.22843(14) 0.3543(4) 0.091(2) Uani 1 1 d . . . F48 F 0.50267(15) -0.16847(17) 0.3581(4) 0.0635(13) Uani 1 1 d . . . Cl1 Cl 0.10327(4) 0.49586(4) 0.33263(10) 0.0203(3) Uani 1 1 d . . . Cl2 Cl 0.35505(4) 0.48271(4) 0.33082(11) 0.0202(3) Uani 1 1 d . . . Cl3 Cl 0.22835(4) 0.01435(5) 0.39005(11) 0.0211(3) Uani 1 1 d . . . Cl4 Cl 0.47936(4) 0.00829(5) 0.39249(10) 0.0217(3) Uani 1 1 d . . . Ru1 Ru 0.036503(12) 0.507699(13) 0.24765(3) 0.01481(9) Uani 1 1 d . . . Ru2 Ru 0.286636(12) 0.482229(13) 0.24830(3) 0.01398(9) Uani 1 1 d . . . Ru3 Ru 0.161243(13) 0.005940(14) 0.47464(3) 0.01978(9) Uani 1 1 d . . . Ru4 Ru 0.412010(12) 0.017550(13) 0.47593(3) 0.01371(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.014(2) 0.017(2) 0.022(3) 0.000(2) 0.005(2) 0.0011(18) C2 0.017(2) 0.026(3) 0.021(3) 0.004(2) 0.002(2) 0.001(2) C3 0.018(2) 0.025(3) 0.027(3) 0.010(2) 0.001(2) 0.006(2) C4 0.011(2) 0.027(2) 0.032(3) -0.007(2) 0.002(2) 0.0009(18) C5 0.019(2) 0.018(2) 0.027(3) -0.003(2) 0.000(2) -0.0016(19) C6 0.016(2) 0.027(2) 0.020(3) 0.001(2) 0.000(2) 0.0016(19) C7 0.034(3) 0.021(3) 0.054(4) 0.009(3) -0.015(3) 0.012(2) C8 0.039(4) 0.032(3) 0.042(4) -0.010(3) -0.012(3) -0.007(3) C9 0.006(2) 0.023(3) 0.015(3) 0.002(2) 0.001(2) 0.0017(18) C10 0.020(3) 0.024(3) 0.021(3) 0.010(2) 0.007(2) -0.001(2) C11 0.012(2) 0.029(3) 0.018(4) 0.003(2) 0.002(3) 0.003(2) C12 0.013(2) 0.025(3) 0.016(3) -0.007(2) -0.001(2) 0.003(2) C13 0.016(2) 0.018(2) 0.017(3) 0.000(2) 0.005(2) 0.0070(19) C14 0.028(3) 0.020(2) 0.023(3) -0.005(2) 0.009(3) -0.001(2) C15 0.026(3) 0.027(3) 0.019(3) -0.005(2) -0.004(2) 0.002(2) C16 0.024(3) 0.032(3) 0.025(3) 0.001(2) 0.000(2) -0.017(2) C17 0.026(3) 0.032(3) 0.030(3) 0.003(3) -0.007(3) -0.023(2) C18 0.025(3) 0.021(3) 0.024(3) 0.002(2) -0.009(2) -0.012(2) C19 0.017(2) 0.021(2) 0.024(3) 0.000(2) -0.002(2) -0.0098(19) C20 0.0386(18) 0.0407(17) 0.0395(18) 0.0005(10) -0.0020(10) -0.0044(10) C21 0.047(4) 0.022(3) 0.042(4) 0.013(3) -0.017(3) -0.012(2) C22 0.015(2) 0.036(3) 0.011(3) 0.002(2) 0.003(2) 0.011(2) C23 0.022(3) 0.023(3) 0.017(3) 0.003(2) 0.007(2) 0.001(2) C24 0.011(2) 0.028(2) 0.025(4) -0.003(3) 0.008(2) 0.004(2) C25 0.010(2) 0.027(2) 0.016(3) -0.002(3) 0.004(2) 0.0051(17) C26 0.018(2) 0.020(2) 0.018(3) -0.004(2) 0.007(2) 0.0012(19) C27 0.023(3) 0.053(3) 0.017(3) -0.001(3) 0.000(2) 0.009(2) C28 0.039(3) 0.048(4) 0.032(4) 0.012(3) 0.017(3) 0.007(3) C29 0.012(2) 0.044(3) 0.030(3) -0.012(3) 0.000(2) -0.006(2) C30 0.017(3) 0.047(3) 0.028(4) 0.006(3) 0.002(2) 0.014(2) C31 0.039(3) 0.042(3) 0.039(4) -0.019(3) 0.013(3) 0.004(3) C32 0.024(3) 0.014(2) 0.021(3) 0.002(2) 0.006(2) -0.0002(19) C33 0.028(3) 0.014(2) 0.023(3) -0.002(2) -0.003(2) 0.0040(19) C34 0.054(4) 0.017(3) 0.033(3) 0.000(2) -0.006(3) 0.013(2) C35 0.086(5) 0.019(2) 0.022(3) -0.002(3) -0.001(4) 0.007(3) C36 0.054(4) 0.022(3) 0.018(3) 0.000(2) -0.002(3) 0.002(2) C37 0.037(3) 0.017(2) 0.022(3) 0.004(2) 0.002(2) 0.001(2) C38 0.098(7) 0.026(3) 0.047(5) -0.007(3) -0.030(5) 0.027(4) C39 0.065(5) 0.023(3) 0.041(4) -0.004(2) -0.019(4) 0.007(3) C40 0.012(2) 0.017(2) 0.023(4) 0.003(2) -0.001(3) -0.006(2) C41 0.031(3) 0.025(3) 0.023(3) 0.011(2) 0.003(3) -0.002(2) C42 0.012(2) 0.025(3) 0.018(4) -0.001(2) 0.002(3) -0.003(2) C43 0.014(2) 0.023(2) 0.015(3) -0.006(2) -0.001(2) 0.001(2) C44 0.029(3) 0.022(2) 0.022(3) -0.005(2) 0.009(2) 0.000(2) C45 0.021(2) 0.020(2) 0.019(3) 0.004(2) 0.004(2) 0.0008(19) C46 0.026(3) 0.022(3) 0.026(3) 0.002(2) 0.000(2) -0.003(2) C47 0.039(3) 0.030(3) 0.049(4) 0.003(3) -0.009(3) -0.012(3) C48 0.074(5) 0.016(2) 0.054(5) 0.015(3) -0.010(4) -0.013(3) C49 0.031(3) 0.028(3) 0.036(3) 0.010(2) -0.007(2) 0.000(2) C50 0.023(2) 0.018(2) 0.030(3) -0.001(2) -0.004(2) 0.0001(18) C51 0.114(8) 0.023(3) 0.094(8) 0.011(4) -0.065(7) -0.026(4) C52 0.079(6) 0.033(4) 0.068(6) 0.010(4) -0.035(5) 0.003(4) C53 0.015(3) 0.061(4) 0.012(3) 0.000(3) 0.001(2) -0.008(2) C54 0.014(2) 0.035(3) 0.023(3) 0.007(2) 0.007(2) 0.001(2) C55 0.015(2) 0.031(3) 0.014(3) 0.001(2) 0.008(2) -0.0028(19) C56 0.016(2) 0.030(3) 0.020(3) 0.003(2) 0.005(2) 0.006(2) C57 0.025(3) 0.035(3) 0.019(3) -0.012(2) 0.006(3) -0.003(2) C58 0.029(3) 0.083(4) 0.016(3) 0.008(3) -0.001(3) -0.003(3) C59 0.033(3) 0.060(4) 0.049(4) 0.035(4) 0.013(3) 0.000(3) C60 0.017(3) 0.034(3) 0.029(3) 0.007(2) 0.003(2) -0.009(2) C61 0.016(3) 0.032(3) 0.028(3) -0.001(2) -0.003(2) 0.005(2) C62 0.038(3) 0.068(4) 0.031(4) -0.031(3) 0.016(3) -0.006(3) C63 0.023(3) 0.026(3) 0.023(3) 0.003(2) 0.003(2) 0.012(2) C64 0.027(3) 0.038(3) 0.023(3) 0.005(2) 0.005(2) 0.014(2) C65 0.050(4) 0.039(3) 0.036(4) 0.010(3) 0.016(3) 0.026(3) C66 0.066(4) 0.051(4) 0.040(4) 0.020(3) 0.014(3) 0.035(3) C67 0.051(4) 0.047(4) 0.039(4) 0.019(3) 0.020(3) 0.021(3) C68 0.035(3) 0.035(3) 0.031(4) 0.007(3) 0.006(3) 0.014(2) C69 0.064(5) 0.048(4) 0.048(4) 0.018(3) 0.026(4) 0.046(4) C70 0.111(7) 0.046(4) 0.059(6) 0.034(4) 0.063(5) 0.043(4) C71 0.018(3) 0.022(3) 0.018(3) 0.002(2) 0.007(2) 0.001(2) C72 0.031(3) 0.023(3) 0.033(4) -0.006(2) -0.006(3) 0.003(2) C73 0.023(3) 0.021(3) 0.008(3) 0.000(2) -0.003(3) 0.004(2) C74 0.017(3) 0.030(3) 0.009(3) 0.006(2) 0.002(2) -0.003(2) C75 0.019(2) 0.018(2) 0.022(3) -0.001(2) 0.000(2) 0.0011(18) C76 0.015(2) 0.025(2) 0.014(3) 0.001(2) -0.002(2) -0.0046(19) C77 0.032(3) 0.043(3) 0.023(3) -0.002(2) 0.011(3) -0.011(3) C78 0.064(4) 0.046(4) 0.028(3) -0.003(3) 0.007(3) -0.035(3) C79 0.076(5) 0.021(3) 0.038(4) 0.002(3) -0.003(4) -0.019(3) C80 0.036(3) 0.022(3) 0.019(3) -0.002(2) -0.001(2) -0.006(2) C81 0.019(2) 0.019(2) 0.017(3) 0.000(2) -0.001(2) -0.0026(18) C82 0.128(9) 0.073(6) 0.056(6) -0.016(5) 0.026(6) -0.066(6) C83 0.0278(15) 0.0243(14) 0.0267(15) -0.0005(9) 0.0009(10) -0.0017(9) C84 0.021(3) 0.102(6) 0.021(4) -0.009(4) -0.011(3) 0.011(3) C85 0.021(3) 0.069(4) 0.024(3) 0.015(3) -0.009(2) 0.003(3) C86 0.014(2) 0.067(4) 0.017(3) -0.003(3) 0.000(2) 0.005(3) C87 0.013(2) 0.056(4) 0.016(3) -0.001(3) -0.001(2) -0.002(2) C88 0.015(3) 0.069(4) 0.028(3) -0.011(3) -0.009(2) 0.002(3) C89 0.025(3) 0.149(8) 0.014(3) -0.002(4) -0.003(3) 0.013(4) C90 0.041(4) 0.106(7) 0.052(5) 0.040(5) -0.013(3) 0.013(4) C91 0.018(3) 0.059(4) 0.036(4) -0.006(3) -0.001(3) 0.010(3) C92 0.023(3) 0.057(4) 0.046(4) 0.000(3) 0.002(3) -0.008(3) C93 0.022(3) 0.097(6) 0.055(5) -0.039(5) -0.015(3) 0.000(3) C94 0.019(2) 0.013(2) 0.023(3) -0.005(2) -0.006(2) -0.0034(18) C95 0.016(2) 0.030(3) 0.024(3) 0.001(2) 0.001(2) 0.0008(19) C96 0.020(3) 0.031(3) 0.035(4) 0.001(2) -0.001(2) -0.005(2) C97 0.043(3) 0.020(3) 0.045(4) 0.004(2) -0.011(3) -0.009(2) C98 0.038(3) 0.011(2) 0.034(3) -0.005(2) -0.008(3) 0.002(2) C99 0.024(3) 0.015(2) 0.030(3) 0.000(2) -0.001(2) 0.000(2) C100 0.048(4) 0.041(4) 0.048(5) 0.021(3) 0.009(3) -0.019(3) C101 0.066(5) 0.018(3) 0.072(6) -0.009(3) 0.012(4) 0.010(3) C102 0.020(3) 0.021(2) 0.017(3) -0.003(2) 0.000(2) -0.004(2) C103 0.029(3) 0.027(3) 0.025(3) -0.003(2) -0.002(3) -0.008(2) C104 0.023(3) 0.025(3) 0.012(3) 0.002(2) -0.006(3) -0.007(2) C105 0.011(2) 0.030(3) 0.008(3) 0.003(2) 0.000(2) -0.006(2) C106 0.025(3) 0.031(3) 0.025(4) 0.003(2) 0.001(3) 0.003(2) C107 0.030(3) 0.011(2) 0.026(3) 0.002(2) 0.006(2) 0.0045(19) C108 0.015(2) 0.010(2) 0.018(3) 0.005(2) 0.001(2) -0.0028(17) C109 0.013(2) 0.018(2) 0.021(3) 0.002(2) 0.001(2) 0.0003(18) C111 0.044(3) 0.006(2) 0.032(3) -0.005(2) -0.004(3) 0.0017(19) C112 0.036(3) 0.012(2) 0.026(3) 0.002(2) 0.007(2) 0.008(2) C113 0.023(2) 0.020(2) 0.019(3) 0.003(2) 0.007(2) -0.0024(19) C114 0.048(4) 0.018(3) 0.042(4) 0.001(2) 0.013(3) 0.001(2) C115 0.067(5) 0.023(3) 0.036(4) -0.001(2) 0.024(3) 0.001(3) C116 0.013(2) 0.019(2) 0.022(3) 0.009(2) -0.010(2) -0.005(2) C117 0.017(2) 0.013(2) 0.021(3) 0.002(2) -0.008(2) -0.0062(18) C118 0.011(2) 0.024(2) 0.028(3) -0.004(3) -0.005(2) -0.0022(18) C119 0.011(2) 0.024(2) 0.018(3) 0.000(2) 0.000(2) -0.0029(19) C120 0.016(3) 0.020(2) 0.018(3) 0.003(2) -0.005(2) -0.0029(19) C121 0.035(3) 0.043(3) 0.019(3) 0.006(3) -0.003(3) -0.003(3) C122 0.037(3) 0.021(3) 0.037(4) 0.010(2) -0.020(3) -0.009(2) C123 0.025(3) 0.036(3) 0.034(4) -0.011(3) 0.003(3) 0.001(2) C124 0.028(3) 0.018(2) 0.029(4) 0.012(2) -0.007(3) -0.009(2) C125 0.033(3) 0.025(3) 0.032(4) -0.007(3) -0.016(3) -0.001(2) N1 0.014(2) 0.0151(19) 0.019(3) 0.0028(18) -0.0015(19) 0.0012(15) N2 0.016(2) 0.021(2) 0.014(3) 0.0013(18) -0.0022(19) -0.0039(16) N3 0.020(2) 0.018(2) 0.015(3) -0.0027(18) 0.000(2) 0.0030(16) N4 0.0130(19) 0.0121(18) 0.017(3) -0.0014(17) 0.0010(18) -0.0005(15) N5 0.019(2) 0.024(2) 0.014(3) 0.0041(18) 0.0004(19) 0.0071(17) N6 0.016(2) 0.021(2) 0.012(2) -0.0010(17) 0.0024(19) -0.0032(16) N7 0.016(2) 0.021(2) 0.014(3) 0.0007(18) -0.0018(19) 0.0002(16) N8 0.010(2) 0.018(2) 0.018(3) 0.0015(18) 0.0004(19) -0.0031(15) F1 0.157(5) 0.044(2) 0.048(3) 0.010(2) -0.041(3) 0.035(3) F2 0.0147(17) 0.069(3) 0.134(5) 0.042(3) -0.014(2) 0.0132(17) F3 0.050(2) 0.0199(16) 0.066(3) 0.0116(16) -0.0090(19) 0.0119(15) F4 0.078(3) 0.077(3) 0.033(3) -0.002(2) -0.008(2) -0.017(2) F5 0.120(4) 0.039(2) 0.100(4) 0.008(2) -0.083(4) -0.031(2) F6 0.043(2) 0.103(4) 0.079(3) -0.029(3) -0.034(2) 0.010(2) F7A 0.109(4) 0.107(4) 0.044(3) 0.016(3) -0.043(3) -0.067(3) F8A 0.021(4) 0.091(8) 0.073(7) -0.031(6) 0.012(4) -0.020(4) F8B 0.024(4) 0.090(9) 0.102(9) -0.029(7) -0.028(5) -0.009(5) F9A 0.112(4) 0.065(3) 0.120(5) 0.008(3) -0.066(4) -0.048(3) F10 0.067(3) 0.051(2) 0.030(2) 0.0084(17) -0.0130(19) -0.0080(19) F11 0.078(3) 0.0232(17) 0.052(2) 0.0165(16) -0.034(2) -0.0222(17) F12 0.042(2) 0.044(2) 0.059(3) 0.0214(18) -0.028(2) -0.0082(16) F13 0.118(5) 0.103(4) 0.061(4) 0.022(3) -0.026(3) 0.055(4) F14A 0.044(8) 0.040(6) 0.079(9) -0.026(5) -0.026(6) 0.030(5) F14B 0.088(10) 0.032(4) 0.078(7) 0.001(4) -0.019(7) 0.037(5) F15 0.089(4) 0.071(3) 0.124(5) 0.030(3) -0.031(4) 0.030(3) F16 0.179(5) 0.0211(19) 0.071(3) -0.0006(18) -0.071(4) -0.013(2) F17 0.101(4) 0.061(3) 0.027(2) -0.0113(18) -0.013(2) 0.022(2) F18 0.063(3) 0.056(2) 0.048(2) -0.0085(19) -0.020(2) -0.010(2) F19A 0.044(10) 0.021(8) 0.018(8) -0.009(5) 0.000(5) -0.023(5) F20A 0.027(10) 0.049(9) 0.051(12) -0.011(6) -0.006(6) -0.023(6) F19B 0.155(17) 0.054(5) 0.066(8) 0.000(5) -0.038(10) -0.032(8) F20B 0.093(9) 0.059(6) 0.26(3) -0.011(12) -0.072(15) -0.038(6) F21 0.112(4) 0.0235(18) 0.079(3) 0.0065(19) -0.024(3) -0.029(2) F22 0.123(4) 0.0229(18) 0.105(4) 0.036(2) -0.058(3) -0.010(2) F23 0.131(5) 0.092(4) 0.057(4) 0.016(3) -0.034(3) 0.040(3) F24 0.041(3) 0.137(5) 0.160(6) 0.101(4) -0.048(3) -0.017(3) F25 0.119(4) 0.082(3) 0.046(3) 0.010(2) 0.032(3) 0.069(3) F26 0.045(3) 0.066(3) 0.112(4) -0.029(3) 0.017(3) 0.030(2) F27 0.055(2) 0.042(2) 0.056(2) -0.0003(18) 0.0098(19) 0.0315(17) F28 0.135(5) 0.083(3) 0.044(3) 0.022(2) 0.042(3) 0.018(3) F29 0.135(5) 0.055(3) 0.104(4) 0.051(3) 0.075(4) 0.044(3) F30 0.067(3) 0.093(4) 0.131(5) 0.068(4) 0.064(4) 0.034(3) F31A 0.096(9) 0.087(9) 0.089(10) 0.019(7) 0.010(7) -0.065(7) F31B 0.094(7) 0.115(9) 0.110(9) 0.013(7) 0.044(6) -0.062(6) F32 0.170(6) 0.066(3) 0.071(4) 0.007(3) 0.065(4) -0.049(3) F33 0.216(8) 0.057(3) 0.092(4) -0.006(3) 0.055(5) -0.073(4) F34 0.076(3) 0.076(3) 0.023(2) -0.014(2) 0.011(2) -0.011(2) F35 0.0358(19) 0.045(2) 0.054(3) -0.0167(18) 0.0163(18) -0.0047(15) F36 0.120(4) 0.0193(17) 0.068(3) -0.0007(18) 0.036(3) 0.020(2) F37 0.104(4) 0.0235(18) 0.075(3) -0.0037(19) 0.006(3) 0.016(2) F38A 0.039(5) 0.052(5) 0.126(18) -0.043(7) 0.002(6) 0.023(4) F38B 0.083(8) 0.047(6) 0.075(10) -0.021(6) 0.016(7) 0.003(5) F39 0.170(6) 0.044(3) 0.074(4) -0.003(2) 0.053(4) 0.033(3) F40 0.181(7) 0.106(5) 0.057(4) -0.006(3) 0.057(4) -0.058(5) F41 0.035(3) 0.208(7) 0.174(7) 0.131(6) 0.044(3) 0.022(3) F42 0.121(4) 0.053(3) 0.102(4) 0.020(3) 0.054(4) -0.011(3) F43 0.032(2) 0.064(3) 0.110(4) 0.038(3) 0.021(2) -0.0083(18) F44 0.169(6) 0.044(3) 0.171(7) -0.050(3) 0.142(5) -0.064(3) F45 0.063(3) 0.137(5) 0.066(4) 0.064(3) 0.001(3) -0.035(3) F46 0.080(3) 0.053(2) 0.027(2) -0.0110(17) 0.017(2) -0.015(2) F47 0.172(5) 0.0188(19) 0.083(4) -0.011(2) 0.082(4) 0.003(2) F48 0.057(3) 0.074(3) 0.059(3) -0.005(2) 0.030(2) 0.025(2) Cl1 0.0177(6) 0.0254(6) 0.0180(8) 0.0017(5) -0.0036(5) 0.0020(5) Cl2 0.0157(7) 0.0270(6) 0.0179(9) 0.0015(5) -0.0022(6) 0.0009(5) Cl3 0.0172(7) 0.0279(6) 0.0183(9) 0.0030(5) 0.0038(6) 0.0045(5) Cl4 0.0158(6) 0.0312(6) 0.0180(8) 0.0007(5) 0.0031(5) -0.0004(5) Ru1 0.01147(19) 0.02204(17) 0.0109(2) 0.00039(18) 0.00072(16) 0.00179(15) Ru2 0.0120(2) 0.01916(18) 0.0108(2) 0.0014(2) 0.00133(18) 0.00148(13) Ru3 0.0122(2) 0.0351(2) 0.0121(2) 0.00025(19) -0.00092(17) 0.00317(16) Ru4 0.0126(2) 0.01585(18) 0.0127(3) -0.0005(2) -0.00098(18) -0.00187(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.384(7) . ? C1 C6 1.398(8) . ? C1 N1 1.432(6) . ? C2 C3 1.367(8) . ? C2 H2 0.9500 . ? C3 C4 1.396(9) . ? C3 C7 1.490(7) . ? C4 C5 1.394(8) . ? C4 H4 0.9500 . ? C5 C6 1.380(7) . ? C5 C8 1.503(9) . ? C6 H6 0.9500 . ? C7 F1 1.323(10) . ? C7 F3 1.327(7) . ? C7 F2 1.333(8) . ? C8 F5 1.291(7) . ? C8 F6 1.303(8) . ? C8 F4 1.394(9) . ? C9 N1 1.352(8) . ? C9 C11 1.379(8) . ? C9 C10 1.514(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.370(8) . ? C11 H11 0.9500 . ? C12 N2 1.348(8) . ? C12 C14 1.505(7) . ? C13 C15 1.389(8) . ? C13 C19 1.395(8) . ? C13 N2 1.428(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.388(8) . ? C15 H15 0.9500 . ? C16 C17 1.381(9) . ? C16 C20 1.511(9) . ? C17 C18 1.400(7) . ? C17 H17 0.9500 . ? C18 C19 1.388(7) . ? C18 C21 1.490(9) . ? C19 H19 0.9500 . ? C20 F8A 1.286(10) . ? C20 F7A 1.290(10) . ? C20 F9A 1.345(8) . ? C20 F8B 1.386(12) . ? C21 F11 1.307(6) . ? C21 F12 1.326(8) . ? C21 F10 1.373(9) . ? C22 C23 1.411(8) . ? C22 C26 1.435(8) . ? C22 C27 1.490(9) . ? C22 Ru1 2.260(6) . ? C23 C24 1.402(9) . ? C23 C28 1.509(8) . ? C23 Ru1 2.224(6) . ? C24 C25 1.434(7) . ? C24 C29 1.491(8) . ? C24 Ru1 2.192(5) . ? C25 C26 1.419(9) . ? C25 C30 1.499(8) . ? C25 Ru1 2.178(5) . ? C26 C31 1.502(8) . ? C26 Ru1 2.257(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.372(9) . ? C32 C33 1.377(7) . ? C32 N3 1.450(6) . ? C33 C34 1.415(7) . ? C33 H33 0.9500 . ? C34 C35 1.372(9) . ? C34 C38 1.505(9) . ? C35 C36 1.370(9) . ? C35 H35 0.9500 . ? C36 C37 1.394(8) . ? C36 C39 1.485(9) . ? C37 H37 0.9500 . ? C38 F15 1.280(10) . ? C38 F14B 1.326(14) . ? C38 F14A 1.342(16) . ? C38 F13 1.359(11) . ? C39 F17 1.312(9) . ? C39 F16 1.313(7) . ? C39 F18 1.348(8) . ? C40 N3 1.344(8) . ? C40 C42 1.365(8) . ? C40 C41 1.517(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.385(8) . ? C42 H42 0.9500 . ? C43 N4 1.352(8) . ? C43 C44 1.497(7) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.381(8) . ? C45 C46 1.403(8) . ? C45 N4 1.421(6) . ? C46 C47 1.370(8) . ? C46 H46 0.9500 . ? C47 C48 1.370(9) . ? C47 C51 1.505(10) . ? C48 C49 1.398(9) . ? C48 H48 0.9500 . ? C49 C50 1.385(7) . ? C49 C52 1.499(10) . ? C50 H50 0.9500 . ? C51 F19A 1.22(2) . ? C51 F20B 1.22(2) . ? C51 F21 1.321(8) . ? C51 F20A 1.46(3) . ? C51 F19B 1.51(3) . ? C52 F24 1.279(10) . ? C52 F22 1.314(8) . ? C52 F23 1.339(12) . ? C53 C57 1.400(9) . ? C53 C54 1.415(8) . ? C53 C58 1.516(10) . ? C53 Ru2 2.256(6) . ? C54 C55 1.443(9) . ? C54 C59 1.516(8) . ? C54 Ru2 2.252(5) . ? C55 C56 1.423(8) . ? C55 C60 1.486(8) . ? C55 Ru2 2.189(5) . ? C56 C57 1.405(9) . ? C56 C61 1.508(8) . ? C56 Ru2 2.186(5) . ? C57 C62 1.497(8) . ? C57 Ru2 2.229(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C68 1.379(9) . ? C63 C64 1.386(8) . ? C63 N5 1.438(7) . ? C64 C65 1.392(8) . ? C64 H64 0.9500 . ? C65 C66 1.396(9) . ? C65 C69 1.503(8) . ? C66 C67 1.377(9) . ? C66 H66 0.9500 . ? C67 C68 1.390(8) . ? C67 C70 1.504(9) . ? C68 H68 0.9500 . ? C69 F25 1.305(10) . ? C69 F27 1.326(9) . ? C69 F26 1.329(10) . ? C70 F30 1.312(10) . ? C70 F29 1.329(8) . ? C70 F28 1.359(12) . ? C71 N5 1.337(9) . ? C71 C73 1.399(8) . ? C71 C72 1.522(8) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.402(8) . ? C73 H73 0.9500 . ? C74 N6 1.343(8) . ? C74 C75 1.511(7) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C81 1.388(8) . ? C76 C77 1.390(7) . ? C76 N6 1.424(7) . ? C77 C78 1.366(9) . ? C77 H77 0.9500 . ? C78 C79 1.356(10) . ? C78 C82 1.518(10) . ? C79 C80 1.408(8) . ? C79 H79 0.9500 . ? C80 C81 1.363(7) . ? C80 C83 1.492(9) . ? C81 H81 0.9500 . ? C82 F32 1.277(11) . ? C82 F31A 1.291(14) . ? C82 F33 1.354(12) . ? C82 F31B 1.367(14) . ? C83 F34 1.321(9) . ? C83 F36 1.326(6) . ? C83 F35 1.338(7) . ? C84 C88 1.379(10) . ? C84 C85 1.391(10) . ? C84 C89 1.521(10) . ? C84 Ru3 2.265(7) . ? C85 C86 1.423(9) . ? C85 C90 1.499(10) . ? C85 Ru3 2.241(6) . ? C86 C87 1.412(9) . ? C86 C91 1.527(8) . ? C86 Ru3 2.169(6) . ? C87 C88 1.470(9) . ? C87 C92 1.501(9) . ? C87 Ru3 2.184(5) . ? C88 C93 1.512(10) . ? C88 Ru3 2.251(6) . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 C99 1.384(8) . ? C94 C95 1.395(9) . ? C94 N7 1.425(6) . ? C95 C96 1.386(8) . ? C95 H95 0.9500 . ? C96 C97 1.387(8) . ? C96 C100 1.505(10) . ? C97 C98 1.378(9) . ? C97 H97 0.9500 . ? C98 C99 1.413(7) . ? C98 C101 1.496(9) . ? C99 H99 0.9500 . ? C100 F40 1.252(11) . ? C100 F42 1.290(8) . ? C100 F41 1.324(9) . ? C101 F38B 1.253(19) . ? C101 F37 1.336(8) . ? C101 F39 1.348(11) . ? C101 F38A 1.448(18) . ? C102 N7 1.324(8) . ? C102 C104 1.390(8) . ? C102 C103 1.529(7) . ? C103 H10D 0.9800 . ? C103 H10E 0.9800 . ? C103 H10F 0.9800 . ? C104 C105 1.405(8) . ? C104 H104 0.9500 . ? C105 N8 1.340(8) . ? C105 C106 1.517(7) . ? C106 H10G 0.9800 . ? C106 H10H 0.9800 . ? C106 H10I 0.9800 . ? C107 C109 1.357(7) . ? C107 C111 1.410(9) . ? C107 C114 1.497(8) . ? C108 C109 1.390(7) . ? C108 C113 1.404(8) . ? C108 N8 1.425(6) . ? C109 H109 0.9500 . ? C111 C112 1.360(8) . ? C111 H111 0.9500 . ? C112 C113 1.366(7) . ? C112 C115 1.491(9) . ? C113 H113 0.9500 . ? C114 F44 1.274(8) . ? C114 F45 1.300(10) . ? C114 F43 1.316(8) . ? C115 F46 1.319(9) . ? C115 F47 1.339(7) . ? C115 F48 1.347(8) . ? C116 C117 1.408(8) . ? C116 C120 1.448(7) . ? C116 C121 1.486(10) . ? C116 Ru4 2.294(6) . ? C117 C118 1.425(9) . ? C117 C122 1.489(7) . ? C117 Ru4 2.279(5) . ? C118 C119 1.443(7) . ? C118 C123 1.501(9) . ? C118 Ru4 2.186(5) . ? C119 C120 1.432(9) . ? C119 C124 1.493(8) . ? C119 Ru4 2.167(5) . ? C120 C125 1.496(8) . ? C120 Ru4 2.240(6) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? C123 H12G 0.9800 . ? C123 H12H 0.9800 . ? C123 H12I 0.9800 . ? C124 H12J 0.9800 . ? C124 H12K 0.9800 . ? C124 H12L 0.9800 . ? C125 H12M 0.9800 . ? C125 H12N 0.9800 . ? C125 H12O 0.9800 . ? N1 Ru1 2.071(4) . ? N2 Ru1 2.072(5) . ? N3 Ru2 2.060(5) . ? N4 Ru2 2.064(5) . ? N5 Ru3 2.067(5) . ? N6 Ru3 2.060(5) . ? N7 Ru4 2.071(5) . ? N8 Ru4 2.072(5) . ? F38B F39 1.74(3) . ? Cl1 Ru1 2.4388(14) . ? Cl2 Ru2 2.4414(14) . ? Cl3 Ru3 2.4337(15) . ? Cl4 Ru4 2.4336(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.7(5) . . ? C2 C1 N1 120.4(5) . . ? C6 C1 N1 119.8(5) . . ? C3 C2 C1 119.8(6) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 121.8(5) . . ? C2 C3 C7 118.6(6) . . ? C4 C3 C7 119.6(5) . . ? C5 C4 C3 117.8(5) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C6 C5 C4 121.0(5) . . ? C6 C5 C8 118.6(5) . . ? C4 C5 C8 120.4(5) . . ? C5 C6 C1 119.8(5) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? F1 C7 F3 105.0(6) . . ? F1 C7 F2 107.5(6) . . ? F3 C7 F2 105.3(5) . . ? F1 C7 C3 112.6(6) . . ? F3 C7 C3 114.5(5) . . ? F2 C7 C3 111.3(6) . . ? F5 C8 F6 109.7(6) . . ? F5 C8 F4 106.6(6) . . ? F6 C8 F4 103.5(6) . . ? F5 C8 C5 113.5(6) . . ? F6 C8 C5 114.1(5) . . ? F4 C8 C5 108.7(5) . . ? N1 C9 C11 122.8(5) . . ? N1 C9 C10 119.8(5) . . ? C11 C9 C10 117.4(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 130.4(6) . . ? C12 C11 H11 114.8 . . ? C9 C11 H11 114.8 . . ? N2 C12 C11 123.1(5) . . ? N2 C12 C14 120.2(5) . . ? C11 C12 C14 116.7(5) . . ? C15 C13 C19 119.4(5) . . ? C15 C13 N2 120.8(5) . . ? C19 C13 N2 119.8(5) . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C13 119.7(6) . . ? C16 C15 H15 120.2 . . ? C13 C15 H15 120.2 . . ? C17 C16 C15 121.8(5) . . ? C17 C16 C20 120.7(5) . . ? C15 C16 C20 117.5(6) . . ? C16 C17 C18 118.2(5) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? C19 C18 C17 120.7(5) . . ? C19 C18 C21 119.7(5) . . ? C17 C18 C21 119.6(5) . . ? C18 C19 C13 120.1(5) . . ? C18 C19 H19 119.9 . . ? C13 C19 H19 119.9 . . ? F8A C20 F7A 123.8(10) . . ? F8A C20 F9A 90.8(11) . . ? F7A C20 F9A 102.3(7) . . ? F8A C20 F8B 39.2(7) . . ? F7A C20 F8B 93.5(11) . . ? F9A C20 F8B 124.1(11) . . ? F8A C20 C16 113.1(7) . . ? F7A C20 C16 112.6(6) . . ? F9A C20 C16 110.4(6) . . ? F8B C20 C16 112.0(7) . . ? F11 C21 F12 107.5(5) . . ? F11 C21 F10 106.8(6) . . ? F12 C21 F10 105.3(6) . . ? F11 C21 C18 114.2(5) . . ? F12 C21 C18 112.5(6) . . ? F10 C21 C18 110.0(5) . . ? C23 C22 C26 108.4(5) . . ? C23 C22 C27 126.5(5) . . ? C26 C22 C27 124.8(5) . . ? C23 C22 Ru1 70.3(3) . . ? C26 C22 Ru1 71.4(3) . . ? C27 C22 Ru1 129.1(4) . . ? C24 C23 C22 108.3(5) . . ? C24 C23 C28 127.6(6) . . ? C22 C23 C28 123.1(6) . . ? C24 C23 Ru1 70.3(3) . . ? C22 C23 Ru1 73.1(3) . . ? C28 C23 Ru1 131.9(4) . . ? C23 C24 C25 108.4(5) . . ? C23 C24 C29 127.1(5) . . ? C25 C24 C29 124.1(6) . . ? C23 C24 Ru1 72.7(3) . . ? C25 C24 Ru1 70.3(3) . . ? C29 C24 Ru1 128.6(4) . . ? C26 C25 C24 107.7(5) . . ? C26 C25 C30 125.6(5) . . ? C24 C25 C30 125.8(6) . . ? C26 C25 Ru1 74.4(3) . . ? C24 C25 Ru1 71.4(3) . . ? C30 C25 Ru1 128.2(4) . . ? C25 C26 C22 107.1(5) . . ? C25 C26 C31 126.1(5) . . ? C22 C26 C31 126.0(6) . . ? C25 C26 Ru1 68.3(3) . . ? C22 C26 Ru1 71.6(3) . . ? C31 C26 Ru1 132.8(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 120.2(5) . . ? C37 C32 N3 120.1(5) . . ? C33 C32 N3 119.6(5) . . ? C32 C33 C34 119.5(5) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 119.8(5) . . ? C35 C34 C38 121.4(5) . . ? C33 C34 C38 118.8(6) . . ? C36 C35 C34 119.9(5) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.7(6) . . ? C35 C36 C39 118.4(5) . . ? C37 C36 C39 120.9(5) . . ? C32 C37 C36 119.8(5) . . ? C32 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? F15 C38 F14B 124.2(15) . . ? F15 C38 F14A 96.6(14) . . ? F14B C38 F14A 31.7(6) . . ? F15 C38 F13 102.0(7) . . ? F14B C38 F13 96.7(12) . . ? F14A C38 F13 121.0(15) . . ? F15 C38 C34 112.3(6) . . ? F14B C38 C34 109.8(10) . . ? F14A C38 C34 113.9(9) . . ? F13 C38 C34 109.4(7) . . ? F17 C39 F16 107.5(6) . . ? F17 C39 F18 104.7(5) . . ? F16 C39 F18 106.2(6) . . ? F17 C39 C36 113.6(6) . . ? F16 C39 C36 113.0(5) . . ? F18 C39 C36 111.2(5) . . ? N3 C40 C42 122.6(5) . . ? N3 C40 C41 120.6(5) . . ? C42 C40 C41 116.8(6) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 C43 130.0(6) . . ? C40 C42 H42 115.0 . . ? C43 C42 H42 115.0 . . ? N4 C43 C42 122.2(5) . . ? N4 C43 C44 121.0(5) . . ? C42 C43 C44 116.7(5) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 118.5(5) . . ? C50 C45 N4 120.4(5) . . ? C46 C45 N4 121.1(5) . . ? C47 C46 C45 120.5(6) . . ? C47 C46 H46 119.7 . . ? C45 C46 H46 119.7 . . ? C48 C47 C46 120.9(6) . . ? C48 C47 C51 122.3(6) . . ? C46 C47 C51 116.7(6) . . ? C47 C48 C49 119.6(5) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C50 C49 C48 119.6(6) . . ? C50 C49 C52 118.1(6) . . ? C48 C49 C52 122.3(5) . . ? C45 C50 C49 121.0(5) . . ? C45 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? F19A C51 F20B 79(2) . . ? F19A C51 F21 113.2(14) . . ? F20B C51 F21 117.0(13) . . ? F19A C51 F20A 105.5(16) . . ? F20B C51 F20A 27(2) . . ? F21 C51 F20A 104.0(14) . . ? F19A C51 C47 113.9(12) . . ? F20B C51 C47 117.8(14) . . ? F21 C51 C47 112.1(7) . . ? F20A C51 C47 107.2(13) . . ? F19A C51 F19B 23.6(11) . . ? F20B C51 F19B 102.1(17) . . ? F21 C51 F19B 99.2(11) . . ? F20A C51 F19B 128.7(15) . . ? C47 C51 F19B 105.2(11) . . ? F24 C52 F22 107.6(7) . . ? F24 C52 F23 105.9(8) . . ? F22 C52 F23 104.5(8) . . ? F24 C52 C49 113.8(8) . . ? F22 C52 C49 113.2(6) . . ? F23 C52 C49 111.1(7) . . ? C57 C53 C54 109.8(5) . . ? C57 C53 C58 126.6(6) . . ? C54 C53 C58 123.3(6) . . ? C57 C53 Ru2 70.8(4) . . ? C54 C53 Ru2 71.6(4) . . ? C58 C53 Ru2 129.9(4) . . ? C53 C54 C55 106.8(5) . . ? C53 C54 C59 127.6(6) . . ? C55 C54 C59 125.0(6) . . ? C53 C54 Ru2 71.8(3) . . ? C55 C54 Ru2 68.7(3) . . ? C59 C54 Ru2 131.3(4) . . ? C56 C55 C54 106.8(5) . . ? C56 C55 C60 127.2(6) . . ? C54 C55 C60 124.9(5) . . ? C56 C55 Ru2 70.9(3) . . ? C54 C55 Ru2 73.5(3) . . ? C60 C55 Ru2 130.1(4) . . ? C57 C56 C55 109.2(5) . . ? C57 C56 C61 128.3(5) . . ? C55 C56 C61 122.2(6) . . ? C57 C56 Ru2 73.1(3) . . ? C55 C56 Ru2 71.1(3) . . ? C61 C56 Ru2 127.0(4) . . ? C53 C57 C56 107.4(5) . . ? C53 C57 C62 123.9(6) . . ? C56 C57 C62 127.7(6) . . ? C53 C57 Ru2 72.8(3) . . ? C56 C57 Ru2 69.8(3) . . ? C62 C57 Ru2 131.5(4) . . ? C53 C58 H58A 109.5 . . ? C53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C53 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C54 C59 H59A 109.5 . . ? C54 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C54 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C55 C60 H60A 109.5 . . ? C55 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C56 C61 H61A 109.5 . . ? C56 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C56 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C68 C63 C64 119.9(5) . . ? C68 C63 N5 120.1(5) . . ? C64 C63 N5 120.0(5) . . ? C63 C64 C65 119.6(6) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C64 C65 C66 120.8(5) . . ? C64 C65 C69 117.7(6) . . ? C66 C65 C69 121.4(5) . . ? C67 C66 C65 118.5(6) . . ? C67 C66 H66 120.7 . . ? C65 C66 H66 120.7 . . ? C66 C67 C68 121.1(6) . . ? C66 C67 C70 120.3(6) . . ? C68 C67 C70 118.6(6) . . ? C63 C68 C67 120.1(6) . . ? C63 C68 H68 120.0 . . ? C67 C68 H68 120.0 . . ? F25 C69 F27 106.4(7) . . ? F25 C69 F26 108.8(7) . . ? F27 C69 F26 106.2(5) . . ? F25 C69 C65 112.1(6) . . ? F27 C69 C65 111.9(6) . . ? F26 C69 C65 111.2(7) . . ? F30 C70 F29 108.0(8) . . ? F30 C70 F28 104.3(7) . . ? F29 C70 F28 107.3(8) . . ? F30 C70 C67 113.3(7) . . ? F29 C70 C67 113.3(6) . . ? F28 C70 C67 109.9(8) . . ? N5 C71 C73 123.0(5) . . ? N5 C71 C72 121.4(5) . . ? C73 C71 C72 115.6(5) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 C74 127.3(6) . . ? C71 C73 H73 116.4 . . ? C74 C73 H73 116.4 . . ? N6 C74 C73 124.5(5) . . ? N6 C74 C75 120.2(5) . . ? C73 C74 C75 115.3(5) . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C81 C76 C77 117.9(5) . . ? C81 C76 N6 120.4(5) . . ? C77 C76 N6 121.7(5) . . ? C78 C77 C76 121.2(6) . . ? C78 C77 H77 119.4 . . ? C76 C77 H77 119.4 . . ? C79 C78 C77 121.6(6) . . ? C79 C78 C82 120.3(6) . . ? C77 C78 C82 118.1(7) . . ? C78 C79 C80 117.6(5) . . ? C78 C79 H79 121.2 . . ? C80 C79 H79 121.2 . . ? C81 C80 C79 121.5(6) . . ? C81 C80 C83 119.8(5) . . ? C79 C80 C83 118.7(5) . . ? C80 C81 C76 120.2(5) . . ? C80 C81 H81 119.9 . . ? C76 C81 H81 119.9 . . ? F32 C82 F31A 130.9(14) . . ? F32 C82 F33 103.6(8) . . ? F31A C82 F33 87.2(12) . . ? F32 C82 F31B 94.2(11) . . ? F31A C82 F31B 43.5(9) . . ? F33 C82 F31B 121.8(11) . . ? F32 C82 C78 112.0(7) . . ? F31A C82 C78 107.8(9) . . ? F33 C82 C78 111.2(8) . . ? F31B C82 C78 112.2(9) . . ? F34 C83 F36 106.4(5) . . ? F34 C83 F35 104.4(5) . . ? F36 C83 F35 107.6(5) . . ? F34 C83 C80 113.7(5) . . ? F36 C83 C80 112.3(5) . . ? F35 C83 C80 111.9(5) . . ? C88 C84 C85 111.4(6) . . ? C88 C84 C89 124.3(7) . . ? C85 C84 C89 124.2(8) . . ? C88 C84 Ru3 71.7(4) . . ? C85 C84 Ru3 71.1(4) . . ? C89 C84 Ru3 128.6(4) . . ? C84 C85 C86 106.6(6) . . ? C84 C85 C90 126.5(7) . . ? C86 C85 C90 126.3(7) . . ? C84 C85 Ru3 73.0(4) . . ? C86 C85 Ru3 68.5(3) . . ? C90 C85 Ru3 130.5(5) . . ? C87 C86 C85 109.4(6) . . ? C87 C86 C91 122.8(6) . . ? C85 C86 C91 126.9(6) . . ? C87 C86 Ru3 71.6(3) . . ? C85 C86 Ru3 73.9(3) . . ? C91 C86 Ru3 129.4(4) . . ? C86 C87 C88 105.9(6) . . ? C86 C87 C92 126.7(6) . . ? C88 C87 C92 127.0(6) . . ? C86 C87 Ru3 70.5(3) . . ? C88 C87 Ru3 73.2(3) . . ? C92 C87 Ru3 127.1(5) . . ? C84 C88 C87 106.8(6) . . ? C84 C88 C93 128.5(7) . . ? C87 C88 C93 124.0(6) . . ? C84 C88 Ru3 72.7(4) . . ? C87 C88 Ru3 68.2(3) . . ? C93 C88 Ru3 130.8(4) . . ? C84 C89 H89A 109.5 . . ? C84 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C84 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C85 C90 H90A 109.5 . . ? C85 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C85 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C86 C91 H91A 109.5 . . ? C86 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C86 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C87 C92 H92A 109.5 . . ? C87 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C87 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C88 C93 H93A 109.5 . . ? C88 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C88 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C99 C94 C95 119.5(5) . . ? C99 C94 N7 120.4(5) . . ? C95 C94 N7 120.1(5) . . ? C96 C95 C94 119.5(5) . . ? C96 C95 H95 120.2 . . ? C94 C95 H95 120.2 . . ? C95 C96 C97 121.3(6) . . ? C95 C96 C100 117.7(6) . . ? C97 C96 C100 120.8(6) . . ? C98 C97 C96 119.5(5) . . ? C98 C97 H97 120.2 . . ? C96 C97 H97 120.2 . . ? C97 C98 C99 119.6(6) . . ? C97 C98 C101 122.8(5) . . ? C99 C98 C101 117.4(6) . . ? C94 C99 C98 120.5(6) . . ? C94 C99 H99 119.7 . . ? C98 C99 H99 119.7 . . ? F40 C100 F42 107.1(7) . . ? F40 C100 F41 104.2(9) . . ? F42 C100 F41 106.4(6) . . ? F40 C100 C96 113.2(6) . . ? F42 C100 C96 113.0(7) . . ? F41 C100 C96 112.2(6) . . ? F38B C101 F37 120.2(11) . . ? F38B C101 F39 84.1(17) . . ? F37 C101 F39 104.6(6) . . ? F38B C101 F38A 35.8(8) . . ? F37 C101 F38A 102.0(10) . . ? F39 C101 F38A 119.4(15) . . ? F38B C101 C98 118.7(8) . . ? F37 C101 C98 112.9(7) . . ? F39 C101 C98 110.6(7) . . ? F38A C101 C98 107.2(9) . . ? N7 C102 C104 124.4(5) . . ? N7 C102 C103 121.0(5) . . ? C104 C102 C103 114.5(5) . . ? C102 C103 H10D 109.5 . . ? C102 C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? C102 C103 H10F 109.5 . . ? H10D C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? C102 C104 C105 127.7(6) . . ? C102 C104 H104 116.2 . . ? C105 C104 H104 116.2 . . ? N8 C105 C104 123.4(5) . . ? N8 C105 C106 121.3(5) . . ? C104 C105 C106 115.3(5) . . ? C105 C106 H10G 109.5 . . ? C105 C106 H10H 109.5 . . ? H10G C106 H10H 109.5 . . ? C105 C106 H10I 109.5 . . ? H10G C106 H10I 109.5 . . ? H10H C106 H10I 109.5 . . ? C109 C107 C111 121.0(5) . . ? C109 C107 C114 119.4(5) . . ? C111 C107 C114 119.6(5) . . ? C109 C108 C113 118.9(5) . . ? C109 C108 N8 121.4(5) . . ? C113 C108 N8 119.6(5) . . ? C107 C109 C108 120.3(5) . . ? C107 C109 H109 119.9 . . ? C108 C109 H109 119.9 . . ? C112 C111 C107 118.1(5) . . ? C112 C111 H111 120.9 . . ? C107 C111 H111 120.9 . . ? C111 C112 C113 122.2(6) . . ? C111 C112 C115 118.4(5) . . ? C113 C112 C115 119.4(5) . . ? C112 C113 C108 119.6(5) . . ? C112 C113 H113 120.2 . . ? C108 C113 H113 120.2 . . ? F44 C114 F45 106.6(7) . . ? F44 C114 F43 105.4(7) . . ? F45 C114 F43 104.6(6) . . ? F44 C114 C107 114.9(6) . . ? F45 C114 C107 113.3(6) . . ? F43 C114 C107 111.1(5) . . ? F46 C115 F47 106.7(6) . . ? F46 C115 F48 104.2(5) . . ? F47 C115 F48 106.5(6) . . ? F46 C115 C112 113.3(6) . . ? F47 C115 C112 113.2(5) . . ? F48 C115 C112 112.3(6) . . ? C117 C116 C120 110.7(5) . . ? C117 C116 C121 125.9(5) . . ? C120 C116 C121 123.4(5) . . ? C117 C116 Ru4 71.5(3) . . ? C120 C116 Ru4 69.4(3) . . ? C121 C116 Ru4 127.6(4) . . ? C116 C117 C118 106.7(4) . . ? C116 C117 C122 124.9(6) . . ? C118 C117 C122 127.2(5) . . ? C116 C117 Ru4 72.6(3) . . ? C118 C117 Ru4 67.9(3) . . ? C122 C117 Ru4 134.2(4) . . ? C117 C118 C119 108.8(6) . . ? C117 C118 C123 127.7(5) . . ? C119 C118 C123 122.7(6) . . ? C117 C118 Ru4 75.0(3) . . ? C119 C118 Ru4 69.9(3) . . ? C123 C118 Ru4 129.3(5) . . ? C120 C119 C118 108.2(5) . . ? C120 C119 C124 126.6(5) . . ? C118 C119 C124 124.4(6) . . ? C120 C119 Ru4 73.8(3) . . ? C118 C119 Ru4 71.4(3) . . ? C124 C119 Ru4 128.8(4) . . ? C119 C120 C116 105.7(5) . . ? C119 C120 C125 128.3(5) . . ? C116 C120 C125 125.3(6) . . ? C119 C120 Ru4 68.3(3) . . ? C116 C120 Ru4 73.4(3) . . ? C125 C120 Ru4 130.1(4) . . ? C116 C121 H12A 109.5 . . ? C116 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C116 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C117 C122 H12D 109.5 . . ? C117 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C117 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? C118 C123 H12G 109.5 . . ? C118 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C118 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? C119 C124 H12J 109.5 . . ? C119 C124 H12K 109.5 . . ? H12J C124 H12K 109.5 . . ? C119 C124 H12L 109.5 . . ? H12J C124 H12L 109.5 . . ? H12K C124 H12L 109.5 . . ? C120 C125 H12M 109.5 . . ? C120 C125 H12N 109.5 . . ? H12M C125 H12N 109.5 . . ? C120 C125 H12O 109.5 . . ? H12M C125 H12O 109.5 . . ? H12N C125 H12O 109.5 . . ? C9 N1 C1 115.5(4) . . ? C9 N1 Ru1 127.9(3) . . ? C1 N1 Ru1 116.6(4) . . ? C12 N2 C13 114.9(4) . . ? C12 N2 Ru1 127.9(3) . . ? C13 N2 Ru1 117.0(4) . . ? C40 N3 C32 114.1(5) . . ? C40 N3 Ru2 129.2(3) . . ? C32 N3 Ru2 116.4(4) . . ? C43 N4 C45 115.2(4) . . ? C43 N4 Ru2 128.8(3) . . ? C45 N4 Ru2 115.9(4) . . ? C71 N5 C63 114.8(5) . . ? C71 N5 Ru3 129.5(4) . . ? C63 N5 Ru3 115.4(4) . . ? C74 N6 C76 114.5(5) . . ? C74 N6 Ru3 128.2(4) . . ? C76 N6 Ru3 117.2(4) . . ? C102 N7 C94 116.3(5) . . ? C102 N7 Ru4 128.4(3) . . ? C94 N7 Ru4 115.2(4) . . ? C105 N8 C108 115.1(4) . . ? C105 N8 Ru4 128.3(3) . . ? C108 N8 Ru4 116.4(4) . . ? C101 F38B F39 50.2(12) . . ? C101 F39 F38B 45.6(8) . . ? N1 Ru1 N2 87.97(18) . . ? N1 Ru1 C25 102.58(19) . . ? N2 Ru1 C25 126.9(2) . . ? N1 Ru1 C24 133.8(2) . . ? N2 Ru1 C24 99.81(19) . . ? C25 Ru1 C24 38.30(19) . . ? N1 Ru1 C23 164.35(18) . . ? N2 Ru1 C23 105.39(19) . . ? C25 Ru1 C23 63.0(2) . . ? C24 Ru1 C23 37.0(2) . . ? N1 Ru1 C26 103.04(17) . . ? N2 Ru1 C26 162.07(18) . . ? C25 Ru1 C26 37.3(2) . . ? C24 Ru1 C26 62.3(2) . . ? C23 Ru1 C26 62.02(19) . . ? N1 Ru1 C22 132.88(19) . . ? N2 Ru1 C22 137.95(19) . . ? C25 Ru1 C22 62.3(2) . . ? C24 Ru1 C22 61.6(2) . . ? C23 Ru1 C22 36.7(2) . . ? C26 Ru1 C22 37.05(19) . . ? N1 Ru1 Cl1 88.73(13) . . ? N2 Ru1 Cl1 87.90(13) . . ? C25 Ru1 Cl1 143.14(18) . . ? C24 Ru1 Cl1 136.58(18) . . ? C23 Ru1 Cl1 99.66(17) . . ? C26 Ru1 Cl1 106.22(15) . . ? C22 Ru1 Cl1 84.21(15) . . ? N3 Ru2 N4 87.09(18) . . ? N3 Ru2 C56 100.29(19) . . ? N4 Ru2 C56 133.4(2) . . ? N3 Ru2 C55 128.1(2) . . ? N4 Ru2 C55 103.47(19) . . ? C56 Ru2 C55 38.0(2) . . ? N3 Ru2 C57 104.3(2) . . ? N4 Ru2 C57 165.82(18) . . ? C56 Ru2 C57 37.1(2) . . ? C55 Ru2 C57 62.9(2) . . ? N3 Ru2 C54 162.68(18) . . ? N4 Ru2 C54 105.29(19) . . ? C56 Ru2 C54 62.4(2) . . ? C55 Ru2 C54 37.9(2) . . ? C57 Ru2 C54 61.8(2) . . ? N3 Ru2 C53 136.1(2) . . ? N4 Ru2 C53 135.4(2) . . ? C56 Ru2 C53 61.2(2) . . ? C55 Ru2 C53 62.1(2) . . ? C57 Ru2 C53 36.4(2) . . ? C54 Ru2 C53 36.6(2) . . ? N3 Ru2 Cl2 88.88(14) . . ? N4 Ru2 Cl2 87.77(13) . . ? C56 Ru2 Cl2 137.74(18) . . ? C55 Ru2 Cl2 141.18(17) . . ? C57 Ru2 Cl2 100.65(18) . . ? C54 Ru2 Cl2 103.42(16) . . ? C53 Ru2 Cl2 83.67(16) . . ? N6 Ru3 N5 87.51(18) . . ? N6 Ru3 C86 131.8(2) . . ? N5 Ru3 C86 101.5(2) . . ? N6 Ru3 C87 101.3(2) . . ? N5 Ru3 C87 128.5(2) . . ? C86 Ru3 C87 37.9(2) . . ? N6 Ru3 C85 163.4(2) . . ? N5 Ru3 C85 106.4(2) . . ? C86 Ru3 C85 37.6(2) . . ? C87 Ru3 C85 63.0(2) . . ? N6 Ru3 C88 103.4(2) . . ? N5 Ru3 C88 164.2(2) . . ? C86 Ru3 C88 62.7(2) . . ? C87 Ru3 C88 38.7(2) . . ? C85 Ru3 C88 61.2(2) . . ? N6 Ru3 C84 133.4(3) . . ? N5 Ru3 C84 138.0(3) . . ? C86 Ru3 C84 61.1(2) . . ? C87 Ru3 C84 61.9(3) . . ? C85 Ru3 C84 36.0(3) . . ? C88 Ru3 C84 35.6(3) . . ? N6 Ru3 Cl3 89.62(13) . . ? N5 Ru3 Cl3 88.07(14) . . ? C86 Ru3 Cl3 137.30(19) . . ? C87 Ru3 Cl3 141.74(18) . . ? C85 Ru3 Cl3 99.72(17) . . ? C88 Ru3 Cl3 103.21(17) . . ? C84 Ru3 Cl3 83.94(19) . . ? N7 Ru4 N8 87.68(18) . . ? N7 Ru4 C119 133.9(2) . . ? N8 Ru4 C119 100.16(19) . . ? N7 Ru4 C118 102.75(19) . . ? N8 Ru4 C118 128.2(2) . . ? C119 Ru4 C118 38.72(19) . . ? N7 Ru4 C120 164.88(17) . . ? N8 Ru4 C120 105.62(18) . . ? C119 Ru4 C120 37.9(2) . . ? C118 Ru4 C120 63.5(2) . . ? N7 Ru4 C117 102.81(17) . . ? N8 Ru4 C117 163.30(17) . . ? C119 Ru4 C117 63.21(19) . . ? C118 Ru4 C117 37.1(2) . . ? C120 Ru4 C117 62.62(17) . . ? N7 Ru4 C116 131.95(18) . . ? N8 Ru4 C116 139.18(19) . . ? C119 Ru4 C116 61.8(2) . . ? C118 Ru4 C116 60.9(2) . . ? C120 Ru4 C116 37.22(18) . . ? C117 Ru4 C116 35.9(2) . . ? N7 Ru4 Cl4 88.50(13) . . ? N8 Ru4 Cl4 87.63(13) . . ? C119 Ru4 Cl4 136.80(18) . . ? C118 Ru4 Cl4 142.2(2) . . ? C120 Ru4 Cl4 99.02(17) . . ? C117 Ru4 Cl4 105.38(16) . . ? C116 Ru4 Cl4 84.61(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.2(8) . . . . ? N1 C1 C2 C3 -178.4(5) . . . . ? C1 C2 C3 C4 0.9(9) . . . . ? C1 C2 C3 C7 -177.2(6) . . . . ? C2 C3 C4 C5 -1.1(8) . . . . ? C7 C3 C4 C5 177.0(6) . . . . ? C3 C4 C5 C6 0.2(9) . . . . ? C3 C4 C5 C8 179.6(6) . . . . ? C4 C5 C6 C1 0.9(9) . . . . ? C8 C5 C6 C1 -178.5(5) . . . . ? C2 C1 C6 C5 -1.1(9) . . . . ? N1 C1 C6 C5 177.4(5) . . . . ? C2 C3 C7 F1 -50.9(8) . . . . ? C4 C3 C7 F1 131.0(6) . . . . ? C2 C3 C7 F3 -170.8(6) . . . . ? C4 C3 C7 F3 11.1(9) . . . . ? C2 C3 C7 F2 69.9(8) . . . . ? C4 C3 C7 F2 -108.2(7) . . . . ? C6 C5 C8 F5 165.0(6) . . . . ? C4 C5 C8 F5 -14.4(9) . . . . ? C6 C5 C8 F6 38.4(9) . . . . ? C4 C5 C8 F6 -141.0(6) . . . . ? C6 C5 C8 F4 -76.5(7) . . . . ? C4 C5 C8 F4 104.1(6) . . . . ? N1 C9 C11 C12 -1.4(10) . . . . ? C10 C9 C11 C12 175.5(6) . . . . ? C9 C11 C12 N2 2.3(11) . . . . ? C9 C11 C12 C14 -175.2(6) . . . . ? C19 C13 C15 C16 -2.6(8) . . . . ? N2 C13 C15 C16 179.0(5) . . . . ? C13 C15 C16 C17 1.8(9) . . . . ? C13 C15 C16 C20 179.2(6) . . . . ? C15 C16 C17 C18 -1.1(9) . . . . ? C20 C16 C17 C18 -178.4(6) . . . . ? C16 C17 C18 C19 1.2(9) . . . . ? C16 C17 C18 C21 179.4(6) . . . . ? C17 C18 C19 C13 -2.0(9) . . . . ? C21 C18 C19 C13 179.8(6) . . . . ? C15 C13 C19 C18 2.7(8) . . . . ? N2 C13 C19 C18 -178.9(5) . . . . ? C17 C16 C20 F8A 75.8(13) . . . . ? C15 C16 C20 F8A -101.6(13) . . . . ? C17 C16 C20 F7A -137.8(7) . . . . ? C15 C16 C20 F7A 44.7(9) . . . . ? C17 C16 C20 F9A -24.2(9) . . . . ? C15 C16 C20 F9A 158.4(7) . . . . ? C17 C16 C20 F8B 118.4(14) . . . . ? C15 C16 C20 F8B -59.0(15) . . . . ? C19 C18 C21 F11 -169.4(6) . . . . ? C17 C18 C21 F11 12.4(9) . . . . ? C19 C18 C21 F12 -46.4(8) . . . . ? C17 C18 C21 F12 135.4(6) . . . . ? C19 C18 C21 F10 70.6(7) . . . . ? C17 C18 C21 F10 -107.6(6) . . . . ? C26 C22 C23 C24 -0.3(6) . . . . ? C27 C22 C23 C24 173.6(5) . . . . ? Ru1 C22 C23 C24 -61.8(4) . . . . ? C26 C22 C23 C28 -169.1(5) . . . . ? C27 C22 C23 C28 4.9(9) . . . . ? Ru1 C22 C23 C28 129.5(6) . . . . ? C26 C22 C23 Ru1 61.5(4) . . . . ? C27 C22 C23 Ru1 -124.6(5) . . . . ? C22 C23 C24 C25 2.0(6) . . . . ? C28 C23 C24 C25 170.1(6) . . . . ? Ru1 C23 C24 C25 -61.6(4) . . . . ? C22 C23 C24 C29 -170.6(5) . . . . ? C28 C23 C24 C29 -2.6(10) . . . . ? Ru1 C23 C24 C29 125.7(6) . . . . ? C22 C23 C24 Ru1 63.6(4) . . . . ? C28 C23 C24 Ru1 -128.3(6) . . . . ? C23 C24 C25 C26 -2.9(6) . . . . ? C29 C24 C25 C26 170.0(5) . . . . ? Ru1 C24 C25 C26 -66.1(4) . . . . ? C23 C24 C25 C30 -172.6(5) . . . . ? C29 C24 C25 C30 0.3(9) . . . . ? Ru1 C24 C25 C30 124.2(6) . . . . ? C23 C24 C25 Ru1 63.2(4) . . . . ? C29 C24 C25 Ru1 -123.9(6) . . . . ? C24 C25 C26 C22 2.7(6) . . . . ? C30 C25 C26 C22 172.4(5) . . . . ? Ru1 C25 C26 C22 -61.4(4) . . . . ? C24 C25 C26 C31 -168.0(6) . . . . ? C30 C25 C26 C31 1.8(9) . . . . ? Ru1 C25 C26 C31 128.0(6) . . . . ? C24 C25 C26 Ru1 64.1(4) . . . . ? C30 C25 C26 Ru1 -126.2(6) . . . . ? C23 C22 C26 C25 -1.5(6) . . . . ? C27 C22 C26 C25 -175.5(5) . . . . ? Ru1 C22 C26 C25 59.3(4) . . . . ? C23 C22 C26 C31 169.2(5) . . . . ? C27 C22 C26 C31 -4.9(9) . . . . ? Ru1 C22 C26 C31 -130.0(6) . . . . ? C23 C22 C26 Ru1 -60.8(4) . . . . ? C27 C22 C26 Ru1 125.2(5) . . . . ? C37 C32 C33 C34 -1.8(9) . . . . ? N3 C32 C33 C34 -177.7(5) . . . . ? C32 C33 C34 C35 3.5(9) . . . . ? C32 C33 C34 C38 -177.9(6) . . . . ? C33 C34 C35 C36 -2.6(10) . . . . ? C38 C34 C35 C36 178.8(7) . . . . ? C34 C35 C36 C37 0.1(10) . . . . ? C34 C35 C36 C39 -178.6(6) . . . . ? C33 C32 C37 C36 -0.6(9) . . . . ? N3 C32 C37 C36 175.2(5) . . . . ? C35 C36 C37 C32 1.5(9) . . . . ? C39 C36 C37 C32 -179.8(6) . . . . ? C35 C34 C38 F15 -128.6(8) . . . . ? C33 C34 C38 F15 52.9(10) . . . . ? C35 C34 C38 F14B 14.0(18) . . . . ? C33 C34 C38 F14B -164.6(15) . . . . ? C35 C34 C38 F14A -20(2) . . . . ? C33 C34 C38 F14A 161.4(18) . . . . ? C35 C34 C38 F13 118.9(8) . . . . ? C33 C34 C38 F13 -59.7(9) . . . . ? C35 C36 C39 F17 94.7(7) . . . . ? C37 C36 C39 F17 -84.0(7) . . . . ? C35 C36 C39 F16 -28.2(10) . . . . ? C37 C36 C39 F16 153.1(6) . . . . ? C35 C36 C39 F18 -147.5(6) . . . . ? C37 C36 C39 F18 33.8(9) . . . . ? N3 C40 C42 C43 -3.7(11) . . . . ? C41 C40 C42 C43 175.1(6) . . . . ? C40 C42 C43 N4 2.8(10) . . . . ? C40 C42 C43 C44 -176.0(6) . . . . ? C50 C45 C46 C47 -0.6(9) . . . . ? N4 C45 C46 C47 178.9(6) . . . . ? C45 C46 C47 C48 -1.5(10) . . . . ? C45 C46 C47 C51 174.8(8) . . . . ? C46 C47 C48 C49 2.4(11) . . . . ? C51 C47 C48 C49 -173.7(9) . . . . ? C47 C48 C49 C50 -1.2(10) . . . . ? C47 C48 C49 C52 177.5(8) . . . . ? C46 C45 C50 C49 1.8(9) . . . . ? N4 C45 C50 C49 -177.7(5) . . . . ? C48 C49 C50 C45 -0.9(10) . . . . ? C52 C49 C50 C45 -179.7(7) . . . . ? C48 C47 C51 F19A -145.3(16) . . . . ? C46 C47 C51 F19A 38.4(19) . . . . ? C48 C47 C51 F20B 125(3) . . . . ? C46 C47 C51 F20B -51(3) . . . . ? C48 C47 C51 F21 -15.2(15) . . . . ? C46 C47 C51 F21 168.5(8) . . . . ? C48 C47 C51 F20A 98.4(15) . . . . ? C46 C47 C51 F20A -77.9(15) . . . . ? C48 C47 C51 F19B -121.9(14) . . . . ? C46 C47 C51 F19B 61.8(15) . . . . ? C50 C49 C52 F24 -53.7(10) . . . . ? C48 C49 C52 F24 127.5(8) . . . . ? C50 C49 C52 F22 -177.1(7) . . . . ? C48 C49 C52 F22 4.2(12) . . . . ? C50 C49 C52 F23 65.7(10) . . . . ? C48 C49 C52 F23 -113.1(8) . . . . ? C57 C53 C54 C55 0.7(6) . . . . ? C58 C53 C54 C55 173.7(5) . . . . ? Ru2 C53 C54 C55 -60.1(4) . . . . ? C57 C53 C54 C59 -170.6(6) . . . . ? C58 C53 C54 C59 2.4(9) . . . . ? Ru2 C53 C54 C59 128.6(6) . . . . ? C57 C53 C54 Ru2 60.8(4) . . . . ? C58 C53 C54 Ru2 -126.2(6) . . . . ? C53 C54 C55 C56 -1.4(6) . . . . ? C59 C54 C55 C56 170.2(5) . . . . ? Ru2 C54 C55 C56 -63.5(4) . . . . ? C53 C54 C55 C60 -170.1(5) . . . . ? C59 C54 C55 C60 1.5(9) . . . . ? Ru2 C54 C55 C60 127.7(6) . . . . ? C53 C54 C55 Ru2 62.2(4) . . . . ? C59 C54 C55 Ru2 -126.3(6) . . . . ? C54 C55 C56 C57 1.6(7) . . . . ? C60 C55 C56 C57 170.0(6) . . . . ? Ru2 C55 C56 C57 -63.6(4) . . . . ? C54 C55 C56 C61 -172.3(5) . . . . ? C60 C55 C56 C61 -3.9(10) . . . . ? Ru2 C55 C56 C61 122.5(6) . . . . ? C54 C55 C56 Ru2 65.2(4) . . . . ? C60 C55 C56 Ru2 -126.3(6) . . . . ? C54 C53 C57 C56 0.3(7) . . . . ? C58 C53 C57 C56 -172.5(6) . . . . ? Ru2 C53 C57 C56 61.5(4) . . . . ? C54 C53 C57 C62 169.8(6) . . . . ? C58 C53 C57 C62 -3.0(10) . . . . ? Ru2 C53 C57 C62 -128.9(6) . . . . ? C54 C53 C57 Ru2 -61.2(4) . . . . ? C58 C53 C57 Ru2 126.0(6) . . . . ? C55 C56 C57 C53 -1.2(7) . . . . ? C61 C56 C57 C53 172.2(6) . . . . ? Ru2 C56 C57 C53 -63.6(4) . . . . ? C55 C56 C57 C62 -170.2(6) . . . . ? C61 C56 C57 C62 3.2(10) . . . . ? Ru2 C56 C57 C62 127.5(7) . . . . ? C55 C56 C57 Ru2 62.4(4) . . . . ? C61 C56 C57 Ru2 -124.2(6) . . . . ? C68 C63 C64 C65 -0.2(9) . . . . ? N5 C63 C64 C65 177.8(6) . . . . ? C63 C64 C65 C66 0.2(10) . . . . ? C63 C64 C65 C69 177.7(7) . . . . ? C64 C65 C66 C67 0.0(11) . . . . ? C69 C65 C66 C67 -177.5(8) . . . . ? C65 C66 C67 C68 0.0(12) . . . . ? C65 C66 C67 C70 177.9(8) . . . . ? C64 C63 C68 C67 0.2(10) . . . . ? N5 C63 C68 C67 -177.8(6) . . . . ? C66 C67 C68 C63 -0.1(11) . . . . ? C70 C67 C68 C63 -178.0(7) . . . . ? C64 C65 C69 F25 43.2(11) . . . . ? C66 C65 C69 F25 -139.3(8) . . . . ? C64 C65 C69 F27 162.6(7) . . . . ? C66 C65 C69 F27 -19.8(11) . . . . ? C64 C65 C69 F26 -78.8(8) . . . . ? C66 C65 C69 F26 98.7(9) . . . . ? C66 C67 C70 F30 134.4(8) . . . . ? C68 C67 C70 F30 -47.7(12) . . . . ? C66 C67 C70 F29 10.8(13) . . . . ? C68 C67 C70 F29 -171.3(8) . . . . ? C66 C67 C70 F28 -109.3(8) . . . . ? C68 C67 C70 F28 68.6(9) . . . . ? N5 C71 C73 C74 3.2(10) . . . . ? C72 C71 C73 C74 -175.5(6) . . . . ? C71 C73 C74 N6 -2.5(10) . . . . ? C71 C73 C74 C75 175.4(6) . . . . ? C81 C76 C77 C78 1.3(9) . . . . ? N6 C76 C77 C78 -177.4(6) . . . . ? C76 C77 C78 C79 1.7(11) . . . . ? C76 C77 C78 C82 -178.9(7) . . . . ? C77 C78 C79 C80 -2.9(11) . . . . ? C82 C78 C79 C80 177.8(7) . . . . ? C78 C79 C80 C81 1.2(10) . . . . ? C78 C79 C80 C83 -177.2(6) . . . . ? C79 C80 C81 C76 1.8(9) . . . . ? C83 C80 C81 C76 -179.9(5) . . . . ? C77 C76 C81 C80 -2.9(8) . . . . ? N6 C76 C81 C80 175.7(5) . . . . ? C79 C78 C82 F32 127.8(9) . . . . ? C77 C78 C82 F32 -51.6(12) . . . . ? C79 C78 C82 F31A -81.5(16) . . . . ? C77 C78 C82 F31A 99.1(15) . . . . ? C79 C78 C82 F33 12.5(12) . . . . ? C77 C78 C82 F33 -166.9(7) . . . . ? C79 C78 C82 F31B -127.7(13) . . . . ? C77 C78 C82 F31B 52.9(14) . . . . ? C81 C80 C83 F34 -81.8(7) . . . . ? C79 C80 C83 F34 96.6(7) . . . . ? C81 C80 C83 F36 157.3(6) . . . . ? C79 C80 C83 F36 -24.3(8) . . . . ? C81 C80 C83 F35 36.2(8) . . . . ? C79 C80 C83 F35 -145.4(6) . . . . ? C88 C84 C85 C86 0.1(7) . . . . ? C89 C84 C85 C86 175.1(6) . . . . ? Ru3 C84 C85 C86 -60.6(4) . . . . ? C88 C84 C85 C90 -171.2(6) . . . . ? C89 C84 C85 C90 3.8(10) . . . . ? Ru3 C84 C85 C90 128.2(6) . . . . ? C88 C84 C85 Ru3 60.6(5) . . . . ? C89 C84 C85 Ru3 -124.4(6) . . . . ? C84 C85 C86 C87 0.2(7) . . . . ? C90 C85 C86 C87 171.5(6) . . . . ? Ru3 C85 C86 C87 -63.3(4) . . . . ? C84 C85 C86 C91 -168.9(6) . . . . ? C90 C85 C86 C91 2.4(10) . . . . ? Ru3 C85 C86 C91 127.6(6) . . . . ? C84 C85 C86 Ru3 63.5(4) . . . . ? C90 C85 C86 Ru3 -125.2(6) . . . . ? C85 C86 C87 C88 -0.4(7) . . . . ? C91 C86 C87 C88 169.2(5) . . . . ? Ru3 C86 C87 C88 -65.2(4) . . . . ? C85 C86 C87 C92 -172.9(6) . . . . ? C91 C86 C87 C92 -3.2(10) . . . . ? Ru3 C86 C87 C92 122.4(6) . . . . ? C85 C86 C87 Ru3 64.8(4) . . . . ? C91 C86 C87 Ru3 -125.6(6) . . . . ? C85 C84 C88 C87 -0.3(7) . . . . ? C89 C84 C88 C87 -175.3(6) . . . . ? Ru3 C84 C88 C87 60.0(4) . . . . ? C85 C84 C88 C93 170.9(6) . . . . ? C89 C84 C88 C93 -4.1(10) . . . . ? Ru3 C84 C88 C93 -128.9(6) . . . . ? C85 C84 C88 Ru3 -60.3(5) . . . . ? C89 C84 C88 Ru3 124.7(6) . . . . ? C86 C87 C88 C84 0.4(7) . . . . ? C92 C87 C88 C84 172.9(6) . . . . ? Ru3 C87 C88 C84 -62.9(4) . . . . ? C86 C87 C88 C93 -171.2(6) . . . . ? C92 C87 C88 C93 1.2(10) . . . . ? Ru3 C87 C88 C93 125.4(6) . . . . ? C86 C87 C88 Ru3 63.4(4) . . . . ? C92 C87 C88 Ru3 -124.2(6) . . . . ? C99 C94 C95 C96 1.4(9) . . . . ? N7 C94 C95 C96 -176.4(5) . . . . ? C94 C95 C96 C97 -2.9(9) . . . . ? C94 C95 C96 C100 -178.8(6) . . . . ? C95 C96 C97 C98 2.8(9) . . . . ? C100 C96 C97 C98 178.6(6) . . . . ? C96 C97 C98 C99 -1.2(9) . . . . ? C96 C97 C98 C101 -176.1(7) . . . . ? C95 C94 C99 C98 0.1(9) . . . . ? N7 C94 C99 C98 177.9(5) . . . . ? C97 C98 C99 C94 -0.2(9) . . . . ? C101 C98 C99 C94 175.0(6) . . . . ? C95 C96 C100 F40 60.3(9) . . . . ? C97 C96 C100 F40 -115.7(8) . . . . ? C95 C96 C100 F42 -177.8(7) . . . . ? C97 C96 C100 F42 6.3(10) . . . . ? C95 C96 C100 F41 -57.4(9) . . . . ? C97 C96 C100 F41 126.7(8) . . . . ? C97 C98 C101 F38B 137(2) . . . . ? C99 C98 C101 F38B -38(2) . . . . ? C97 C98 C101 F37 -11.3(11) . . . . ? C99 C98 C101 F37 173.6(6) . . . . ? C97 C98 C101 F39 -128.1(7) . . . . ? C99 C98 C101 F39 56.9(9) . . . . ? C97 C98 C101 F38A 100.3(14) . . . . ? C99 C98 C101 F38A -74.8(15) . . . . ? N7 C102 C104 C105 2.7(11) . . . . ? C103 C102 C104 C105 -175.6(6) . . . . ? C102 C104 C105 N8 -3.9(10) . . . . ? C102 C104 C105 C106 174.2(6) . . . . ? C111 C107 C109 C108 -0.5(9) . . . . ? C114 C107 C109 C108 177.5(6) . . . . ? C113 C108 C109 C107 0.3(8) . . . . ? N8 C108 C109 C107 -176.1(5) . . . . ? C109 C107 C111 C112 0.8(9) . . . . ? C114 C107 C111 C112 -177.3(6) . . . . ? C107 C111 C112 C113 -0.9(9) . . . . ? C107 C111 C112 C115 -179.0(6) . . . . ? C111 C112 C113 C108 0.7(9) . . . . ? C115 C112 C113 C108 178.7(6) . . . . ? C109 C108 C113 C112 -0.4(8) . . . . ? N8 C108 C113 C112 176.1(5) . . . . ? C109 C107 C114 F44 179.9(7) . . . . ? C111 C107 C114 F44 -2.0(10) . . . . ? C109 C107 C114 F45 -57.1(8) . . . . ? C111 C107 C114 F45 121.0(7) . . . . ? C109 C107 C114 F43 60.3(9) . . . . ? C111 C107 C114 F43 -121.6(7) . . . . ? C111 C112 C115 F46 101.9(7) . . . . ? C113 C112 C115 F46 -76.2(8) . . . . ? C111 C112 C115 F47 -19.7(10) . . . . ? C113 C112 C115 F47 162.1(6) . . . . ? C111 C112 C115 F48 -140.3(6) . . . . ? C113 C112 C115 F48 41.5(8) . . . . ? C120 C116 C117 C118 -1.2(6) . . . . ? C121 C116 C117 C118 176.9(5) . . . . ? Ru4 C116 C117 C118 -59.6(4) . . . . ? C120 C116 C117 C122 -169.3(5) . . . . ? C121 C116 C117 C122 8.7(9) . . . . ? Ru4 C116 C117 C122 132.2(5) . . . . ? C120 C116 C117 Ru4 58.5(4) . . . . ? C121 C116 C117 Ru4 -123.5(5) . . . . ? C116 C117 C118 C119 0.6(6) . . . . ? C122 C117 C118 C119 168.4(6) . . . . ? Ru4 C117 C118 C119 -62.2(4) . . . . ? C116 C117 C118 C123 -168.9(6) . . . . ? C122 C117 C118 C123 -1.1(10) . . . . ? Ru4 C117 C118 C123 128.4(6) . . . . ? C116 C117 C118 Ru4 62.7(4) . . . . ? C122 C117 C118 Ru4 -129.5(6) . . . . ? C117 C118 C119 C120 0.2(7) . . . . ? C123 C118 C119 C120 170.4(6) . . . . ? Ru4 C118 C119 C120 -65.2(4) . . . . ? C117 C118 C119 C124 -169.8(5) . . . . ? C123 C118 C119 C124 0.3(10) . . . . ? Ru4 C118 C119 C124 124.8(6) . . . . ? C117 C118 C119 Ru4 65.4(4) . . . . ? C123 C118 C119 Ru4 -124.5(6) . . . . ? C118 C119 C120 C116 -0.9(6) . . . . ? C124 C119 C120 C116 168.9(5) . . . . ? Ru4 C119 C120 C116 -64.5(4) . . . . ? C118 C119 C120 C125 -171.7(6) . . . . ? C124 C119 C120 C125 -1.9(10) . . . . ? Ru4 C119 C120 C125 124.7(6) . . . . ? C118 C119 C120 Ru4 63.6(4) . . . . ? C124 C119 C120 Ru4 -126.6(6) . . . . ? C117 C116 C120 C119 1.3(6) . . . . ? C121 C116 C120 C119 -176.8(5) . . . . ? Ru4 C116 C120 C119 61.0(4) . . . . ? C117 C116 C120 C125 172.5(5) . . . . ? C121 C116 C120 C125 -5.6(8) . . . . ? Ru4 C116 C120 C125 -127.8(6) . . . . ? C117 C116 C120 Ru4 -59.7(4) . . . . ? C121 C116 C120 Ru4 122.2(5) . . . . ? C11 C9 N1 C1 176.1(5) . . . . ? C10 C9 N1 C1 -0.7(7) . . . . ? C11 C9 N1 Ru1 0.4(8) . . . . ? C10 C9 N1 Ru1 -176.4(4) . . . . ? C2 C1 N1 C9 77.1(6) . . . . ? C6 C1 N1 C9 -101.4(6) . . . . ? C2 C1 N1 Ru1 -106.7(5) . . . . ? C6 C1 N1 Ru1 74.8(6) . . . . ? C11 C12 N2 C13 -176.5(6) . . . . ? C14 C12 N2 C13 0.9(7) . . . . ? C11 C12 N2 Ru1 -2.1(8) . . . . ? C14 C12 N2 Ru1 175.3(4) . . . . ? C15 C13 N2 C12 -77.9(6) . . . . ? C19 C13 N2 C12 103.7(6) . . . . ? C15 C13 N2 Ru1 107.0(5) . . . . ? C19 C13 N2 Ru1 -71.3(5) . . . . ? C42 C40 N3 C32 176.9(6) . . . . ? C41 C40 N3 C32 -1.8(8) . . . . ? C42 C40 N3 Ru2 3.3(9) . . . . ? C41 C40 N3 Ru2 -175.5(4) . . . . ? C37 C32 N3 C40 -97.1(7) . . . . ? C33 C32 N3 C40 78.8(6) . . . . ? C37 C32 N3 Ru2 77.4(6) . . . . ? C33 C32 N3 Ru2 -106.7(5) . . . . ? C42 C43 N4 C45 -177.5(6) . . . . ? C44 C43 N4 C45 1.2(8) . . . . ? C42 C43 N4 Ru2 -1.5(8) . . . . ? C44 C43 N4 Ru2 177.2(4) . . . . ? C50 C45 N4 C43 101.8(6) . . . . ? C46 C45 N4 C43 -77.7(7) . . . . ? C50 C45 N4 Ru2 -74.7(6) . . . . ? C46 C45 N4 Ru2 105.8(5) . . . . ? C73 C71 N5 C63 -176.4(6) . . . . ? C72 C71 N5 C63 2.3(8) . . . . ? C73 C71 N5 Ru3 -2.5(9) . . . . ? C72 C71 N5 Ru3 176.2(4) . . . . ? C68 C63 N5 C71 100.8(7) . . . . ? C64 C63 N5 C71 -77.2(7) . . . . ? C68 C63 N5 Ru3 -74.0(6) . . . . ? C64 C63 N5 Ru3 108.0(6) . . . . ? C73 C74 N6 C76 176.4(5) . . . . ? C75 C74 N6 C76 -1.3(7) . . . . ? C73 C74 N6 Ru3 1.0(8) . . . . ? C75 C74 N6 Ru3 -176.7(4) . . . . ? C81 C76 N6 C74 -100.6(6) . . . . ? C77 C76 N6 C74 78.0(7) . . . . ? C81 C76 N6 Ru3 75.3(6) . . . . ? C77 C76 N6 Ru3 -106.1(6) . . . . ? C104 C102 N7 C94 -177.4(6) . . . . ? C103 C102 N7 C94 0.9(8) . . . . ? C104 C102 N7 Ru4 -1.2(9) . . . . ? C103 C102 N7 Ru4 177.0(4) . . . . ? C99 C94 N7 C102 -75.6(7) . . . . ? C95 C94 N7 C102 102.2(7) . . . . ? C99 C94 N7 Ru4 107.8(5) . . . . ? C95 C94 N7 Ru4 -74.4(6) . . . . ? C104 C105 N8 C108 178.5(5) . . . . ? C106 C105 N8 C108 0.5(7) . . . . ? C104 C105 N8 Ru4 3.4(8) . . . . ? C106 C105 N8 Ru4 -174.5(4) . . . . ? C109 C108 N8 C105 78.0(6) . . . . ? C113 C108 N8 C105 -98.4(6) . . . . ? C109 C108 N8 Ru4 -106.3(5) . . . . ? C113 C108 N8 Ru4 77.3(5) . . . . ? F37 C101 F38B F39 -103.4(13) . . . . ? F38A C101 F38B F39 -170.3(14) . . . . ? C98 C101 F38B F39 110.3(12) . . . . ? F37 C101 F39 F38B 119.7(10) . . . . ? F38A C101 F39 F38B 6.5(9) . . . . ? C98 C101 F39 F38B -118.5(9) . . . . ? C9 N1 Ru1 N2 -0.2(5) . . . . ? C1 N1 Ru1 N2 -175.9(4) . . . . ? C9 N1 Ru1 C25 -127.7(5) . . . . ? C1 N1 Ru1 C25 56.7(4) . . . . ? C9 N1 Ru1 C24 -101.9(5) . . . . ? C1 N1 Ru1 C24 82.5(5) . . . . ? C9 N1 Ru1 C23 -149.4(7) . . . . ? C1 N1 Ru1 C23 35.0(10) . . . . ? C9 N1 Ru1 C26 -165.9(4) . . . . ? C1 N1 Ru1 C26 18.4(4) . . . . ? C9 N1 Ru1 C22 168.6(4) . . . . ? C1 N1 Ru1 C22 -7.0(5) . . . . ? C9 N1 Ru1 Cl1 87.7(4) . . . . ? C1 N1 Ru1 Cl1 -87.9(4) . . . . ? C12 N2 Ru1 N1 1.0(5) . . . . ? C13 N2 Ru1 N1 175.3(4) . . . . ? C12 N2 Ru1 C25 105.3(5) . . . . ? C13 N2 Ru1 C25 -80.4(4) . . . . ? C12 N2 Ru1 C24 135.2(5) . . . . ? C13 N2 Ru1 C24 -50.5(4) . . . . ? C12 N2 Ru1 C23 172.8(5) . . . . ? C13 N2 Ru1 C23 -12.9(4) . . . . ? C12 N2 Ru1 C26 129.7(6) . . . . ? C13 N2 Ru1 C26 -56.0(8) . . . . ? C12 N2 Ru1 C22 -166.7(4) . . . . ? C13 N2 Ru1 C22 7.6(5) . . . . ? C12 N2 Ru1 Cl1 -87.8(5) . . . . ? C13 N2 Ru1 Cl1 86.5(4) . . . . ? C26 C25 Ru1 N1 -95.1(3) . . . . ? C24 C25 Ru1 N1 149.6(4) . . . . ? C30 C25 Ru1 N1 28.3(5) . . . . ? C26 C25 Ru1 N2 167.9(3) . . . . ? C24 C25 Ru1 N2 52.6(5) . . . . ? C30 C25 Ru1 N2 -68.8(5) . . . . ? C26 C25 Ru1 C24 115.3(5) . . . . ? C30 C25 Ru1 C24 -121.3(7) . . . . ? C26 C25 Ru1 C23 78.5(4) . . . . ? C24 C25 Ru1 C23 -36.8(4) . . . . ? C30 C25 Ru1 C23 -158.2(6) . . . . ? C24 C25 Ru1 C26 -115.3(5) . . . . ? C30 C25 Ru1 C26 123.3(6) . . . . ? C26 C25 Ru1 C22 37.0(3) . . . . ? C24 C25 Ru1 C22 -78.3(4) . . . . ? C30 C25 Ru1 C22 160.4(6) . . . . ? C26 C25 Ru1 Cl1 10.0(4) . . . . ? C24 C25 Ru1 Cl1 -105.4(4) . . . . ? C30 C25 Ru1 Cl1 133.3(5) . . . . ? C23 C24 Ru1 N1 -160.7(3) . . . . ? C25 C24 Ru1 N1 -43.2(5) . . . . ? C29 C24 Ru1 N1 75.2(6) . . . . ? C23 C24 Ru1 N2 102.6(3) . . . . ? C25 C24 Ru1 N2 -139.9(4) . . . . ? C29 C24 Ru1 N2 -21.5(6) . . . . ? C23 C24 Ru1 C25 -117.5(5) . . . . ? C29 C24 Ru1 C25 118.4(8) . . . . ? C25 C24 Ru1 C23 117.5(5) . . . . ? C29 C24 Ru1 C23 -124.1(7) . . . . ? C23 C24 Ru1 C26 -79.3(4) . . . . ? C25 C24 Ru1 C26 38.1(4) . . . . ? C29 C24 Ru1 C26 156.6(6) . . . . ? C23 C24 Ru1 C22 -37.2(3) . . . . ? C25 C24 Ru1 C22 80.3(4) . . . . ? C29 C24 Ru1 C22 -161.3(6) . . . . ? C23 C24 Ru1 Cl1 5.2(4) . . . . ? C25 C24 Ru1 Cl1 122.7(4) . . . . ? C29 C24 Ru1 Cl1 -118.9(5) . . . . ? C24 C23 Ru1 N1 62.0(9) . . . . ? C22 C23 Ru1 N1 -55.2(9) . . . . ? C28 C23 Ru1 N1 -174.8(7) . . . . ? C24 C23 Ru1 N2 -85.9(3) . . . . ? C22 C23 Ru1 N2 156.9(3) . . . . ? C28 C23 Ru1 N2 37.3(7) . . . . ? C24 C23 Ru1 C25 38.1(3) . . . . ? C22 C23 Ru1 C25 -79.1(3) . . . . ? C28 C23 Ru1 C25 161.4(7) . . . . ? C22 C23 Ru1 C24 -117.2(4) . . . . ? C28 C23 Ru1 C24 123.3(8) . . . . ? C24 C23 Ru1 C26 80.3(3) . . . . ? C22 C23 Ru1 C26 -36.9(3) . . . . ? C28 C23 Ru1 C26 -156.4(7) . . . . ? C24 C23 Ru1 C22 117.2(4) . . . . ? C28 C23 Ru1 C22 -119.6(8) . . . . ? C24 C23 Ru1 Cl1 -176.4(3) . . . . ? C22 C23 Ru1 Cl1 66.4(3) . . . . ? C28 C23 Ru1 Cl1 -53.1(6) . . . . ? C25 C26 Ru1 N1 93.7(3) . . . . ? C22 C26 Ru1 N1 -148.5(3) . . . . ? C31 C26 Ru1 N1 -26.0(7) . . . . ? C25 C26 Ru1 N2 -33.0(8) . . . . ? C22 C26 Ru1 N2 84.8(7) . . . . ? C31 C26 Ru1 N2 -152.7(6) . . . . ? C22 C26 Ru1 C25 117.8(4) . . . . ? C31 C26 Ru1 C25 -119.7(8) . . . . ? C25 C26 Ru1 C24 -39.2(3) . . . . ? C22 C26 Ru1 C24 78.6(4) . . . . ? C31 C26 Ru1 C24 -159.0(7) . . . . ? C25 C26 Ru1 C23 -81.3(3) . . . . ? C22 C26 Ru1 C23 36.5(3) . . . . ? C31 C26 Ru1 C23 159.0(7) . . . . ? C25 C26 Ru1 C22 -117.8(4) . . . . ? C31 C26 Ru1 C22 122.5(8) . . . . ? C25 C26 Ru1 Cl1 -173.8(3) . . . . ? C22 C26 Ru1 Cl1 -56.0(3) . . . . ? C31 C26 Ru1 Cl1 66.5(6) . . . . ? C23 C22 Ru1 N1 162.4(3) . . . . ? C26 C22 Ru1 N1 44.0(4) . . . . ? C27 C22 Ru1 N1 -76.1(6) . . . . ? C23 C22 Ru1 N2 -34.4(4) . . . . ? C26 C22 Ru1 N2 -152.8(3) . . . . ? C27 C22 Ru1 N2 87.1(6) . . . . ? C23 C22 Ru1 C25 81.2(3) . . . . ? C26 C22 Ru1 C25 -37.2(3) . . . . ? C27 C22 Ru1 C25 -157.3(6) . . . . ? C23 C22 Ru1 C24 37.5(3) . . . . ? C26 C22 Ru1 C24 -80.9(3) . . . . ? C27 C22 Ru1 C24 159.0(6) . . . . ? C26 C22 Ru1 C23 -118.4(4) . . . . ? C27 C22 Ru1 C23 121.5(6) . . . . ? C23 C22 Ru1 C26 118.4(4) . . . . ? C27 C22 Ru1 C26 -120.1(7) . . . . ? C23 C22 Ru1 Cl1 -114.7(3) . . . . ? C26 C22 Ru1 Cl1 126.9(3) . . . . ? C27 C22 Ru1 Cl1 6.7(5) . . . . ? C40 N3 Ru2 N4 -1.8(5) . . . . ? C32 N3 Ru2 N4 -175.4(4) . . . . ? C40 N3 Ru2 C56 -135.5(5) . . . . ? C32 N3 Ru2 C56 50.9(4) . . . . ? C40 N3 Ru2 C55 -106.7(5) . . . . ? C32 N3 Ru2 C55 79.7(5) . . . . ? C40 N3 Ru2 C57 -173.3(5) . . . . ? C32 N3 Ru2 C57 13.2(5) . . . . ? C40 N3 Ru2 C54 -138.2(7) . . . . ? C32 N3 Ru2 C54 48.3(9) . . . . ? C40 N3 Ru2 C53 165.7(5) . . . . ? C32 N3 Ru2 C53 -7.9(5) . . . . ? C40 N3 Ru2 Cl2 86.0(5) . . . . ? C32 N3 Ru2 Cl2 -87.6(4) . . . . ? C43 N4 Ru2 N3 1.0(5) . . . . ? C45 N4 Ru2 N3 177.0(4) . . . . ? C43 N4 Ru2 C56 102.4(5) . . . . ? C45 N4 Ru2 C56 -81.6(5) . . . . ? C43 N4 Ru2 C55 129.6(5) . . . . ? C45 N4 Ru2 C55 -54.5(4) . . . . ? C43 N4 Ru2 C57 145.0(9) . . . . ? C45 N4 Ru2 C57 -39.0(11) . . . . ? C43 N4 Ru2 C54 168.7(5) . . . . ? C45 N4 Ru2 C54 -15.3(4) . . . . ? C43 N4 Ru2 C53 -166.7(4) . . . . ? C45 N4 Ru2 C53 9.3(5) . . . . ? C43 N4 Ru2 Cl2 -88.0(5) . . . . ? C45 N4 Ru2 Cl2 88.0(4) . . . . ? C57 C56 Ru2 N3 -100.2(4) . . . . ? C55 C56 Ru2 N3 142.0(4) . . . . ? C61 C56 Ru2 N3 25.4(5) . . . . ? C57 C56 Ru2 N4 164.0(3) . . . . ? C55 C56 Ru2 N4 46.2(5) . . . . ? C61 C56 Ru2 N4 -70.4(6) . . . . ? C57 C56 Ru2 C55 117.9(5) . . . . ? C61 C56 Ru2 C55 -116.5(7) . . . . ? C55 C56 Ru2 C57 -117.9(5) . . . . ? C61 C56 Ru2 C57 125.6(7) . . . . ? C57 C56 Ru2 C54 78.9(4) . . . . ? C55 C56 Ru2 C54 -38.9(4) . . . . ? C61 C56 Ru2 C54 -155.5(6) . . . . ? C57 C56 Ru2 C53 37.2(3) . . . . ? C55 C56 Ru2 C53 -80.6(4) . . . . ? C61 C56 Ru2 C53 162.8(6) . . . . ? C57 C56 Ru2 Cl2 -0.3(4) . . . . ? C55 C56 Ru2 Cl2 -118.2(4) . . . . ? C61 C56 Ru2 Cl2 125.2(5) . . . . ? C56 C55 Ru2 N3 -50.4(5) . . . . ? C54 C55 Ru2 N3 -165.3(3) . . . . ? C60 C55 Ru2 N3 72.6(6) . . . . ? C56 C55 Ru2 N4 -147.4(4) . . . . ? C54 C55 Ru2 N4 97.7(3) . . . . ? C60 C55 Ru2 N4 -24.4(6) . . . . ? C54 C55 Ru2 C56 -114.9(5) . . . . ? C60 C55 Ru2 C56 123.1(7) . . . . ? C56 C55 Ru2 C57 36.8(4) . . . . ? C54 C55 Ru2 C57 -78.1(4) . . . . ? C60 C55 Ru2 C57 159.8(6) . . . . ? C56 C55 Ru2 C54 114.9(5) . . . . ? C60 C55 Ru2 C54 -122.1(6) . . . . ? C56 C55 Ru2 C53 78.0(4) . . . . ? C54 C55 Ru2 C53 -36.9(3) . . . . ? C60 C55 Ru2 C53 -159.0(6) . . . . ? C56 C55 Ru2 Cl2 109.1(4) . . . . ? C54 C55 Ru2 Cl2 -5.8(4) . . . . ? C60 C55 Ru2 Cl2 -127.9(5) . . . . ? C53 C57 Ru2 N3 -155.2(3) . . . . ? C56 C57 Ru2 N3 88.2(3) . . . . ? C62 C57 Ru2 N3 -34.8(7) . . . . ? C53 C57 Ru2 N4 62.1(11) . . . . ? C56 C57 Ru2 N4 -54.6(11) . . . . ? C62 C57 Ru2 N4 -177.5(7) . . . . ? C53 C57 Ru2 C56 116.6(5) . . . . ? C62 C57 Ru2 C56 -123.0(8) . . . . ? C53 C57 Ru2 C55 79.0(4) . . . . ? C56 C57 Ru2 C55 -37.6(3) . . . . ? C62 C57 Ru2 C55 -160.6(8) . . . . ? C53 C57 Ru2 C54 36.0(3) . . . . ? C56 C57 Ru2 C54 -80.6(4) . . . . ? C62 C57 Ru2 C54 156.4(8) . . . . ? C56 C57 Ru2 C53 -116.6(5) . . . . ? C62 C57 Ru2 C53 120.4(8) . . . . ? C53 C57 Ru2 Cl2 -63.6(3) . . . . ? C56 C57 Ru2 Cl2 179.8(3) . . . . ? C62 C57 Ru2 Cl2 56.8(7) . . . . ? C53 C54 Ru2 N3 -75.0(8) . . . . ? C55 C54 Ru2 N3 42.0(9) . . . . ? C59 C54 Ru2 N3 160.5(7) . . . . ? C53 C54 Ru2 N4 150.6(3) . . . . ? C55 C54 Ru2 N4 -92.4(3) . . . . ? C59 C54 Ru2 N4 26.1(7) . . . . ? C53 C54 Ru2 C56 -78.0(4) . . . . ? C55 C54 Ru2 C56 39.0(3) . . . . ? C59 C54 Ru2 C56 157.5(7) . . . . ? C53 C54 Ru2 C55 -117.0(5) . . . . ? C59 C54 Ru2 C55 118.5(8) . . . . ? C53 C54 Ru2 C57 -35.8(3) . . . . ? C55 C54 Ru2 C57 81.2(4) . . . . ? C59 C54 Ru2 C57 -160.3(7) . . . . ? C55 C54 Ru2 C53 117.0(5) . . . . ? C59 C54 Ru2 C53 -124.5(8) . . . . ? C53 C54 Ru2 Cl2 59.2(3) . . . . ? C55 C54 Ru2 Cl2 176.2(3) . . . . ? C59 C54 Ru2 Cl2 -65.3(6) . . . . ? C57 C53 Ru2 N3 35.9(5) . . . . ? C54 C53 Ru2 N3 155.5(3) . . . . ? C58 C53 Ru2 N3 -86.1(6) . . . . ? C57 C53 Ru2 N4 -162.0(3) . . . . ? C54 C53 Ru2 N4 -42.5(4) . . . . ? C58 C53 Ru2 N4 75.9(7) . . . . ? C57 C53 Ru2 C56 -38.0(3) . . . . ? C54 C53 Ru2 C56 81.6(3) . . . . ? C58 C53 Ru2 C56 -160.0(7) . . . . ? C57 C53 Ru2 C55 -81.3(4) . . . . ? C54 C53 Ru2 C55 38.2(3) . . . . ? C58 C53 Ru2 C55 156.6(7) . . . . ? C54 C53 Ru2 C57 119.6(5) . . . . ? C58 C53 Ru2 C57 -122.0(7) . . . . ? C57 C53 Ru2 C54 -119.6(5) . . . . ? C58 C53 Ru2 C54 118.4(7) . . . . ? C57 C53 Ru2 Cl2 117.7(3) . . . . ? C54 C53 Ru2 Cl2 -122.8(3) . . . . ? C58 C53 Ru2 Cl2 -4.4(6) . . . . ? C74 N6 Ru3 N5 -0.3(5) . . . . ? C76 N6 Ru3 N5 -175.6(4) . . . . ? C74 N6 Ru3 C86 -103.6(5) . . . . ? C76 N6 Ru3 C86 81.1(5) . . . . ? C74 N6 Ru3 C87 -129.1(5) . . . . ? C76 N6 Ru3 C87 55.5(4) . . . . ? C74 N6 Ru3 C85 -147.6(7) . . . . ? C76 N6 Ru3 C85 37.1(10) . . . . ? C74 N6 Ru3 C88 -168.7(5) . . . . ? C76 N6 Ru3 C88 16.0(4) . . . . ? C74 N6 Ru3 C84 169.1(5) . . . . ? C76 N6 Ru3 C84 -6.3(5) . . . . ? C74 N6 Ru3 Cl3 87.8(5) . . . . ? C76 N6 Ru3 Cl3 -87.5(4) . . . . ? C71 N5 Ru3 N6 1.0(5) . . . . ? C63 N5 Ru3 N6 174.9(4) . . . . ? C71 N5 Ru3 C86 133.3(5) . . . . ? C63 N5 Ru3 C86 -52.8(4) . . . . ? C71 N5 Ru3 C87 103.5(5) . . . . ? C63 N5 Ru3 C87 -82.6(5) . . . . ? C71 N5 Ru3 C85 171.8(5) . . . . ? C63 N5 Ru3 C85 -14.4(4) . . . . ? C71 N5 Ru3 C88 135.3(8) . . . . ? C63 N5 Ru3 C88 -50.8(10) . . . . ? C71 N5 Ru3 C84 -167.4(5) . . . . ? C63 N5 Ru3 C84 6.5(6) . . . . ? C71 N5 Ru3 Cl3 -88.7(5) . . . . ? C63 N5 Ru3 Cl3 85.2(4) . . . . ? C87 C86 Ru3 N6 -43.6(5) . . . . ? C85 C86 Ru3 N6 -161.0(4) . . . . ? C91 C86 Ru3 N6 74.1(7) . . . . ? C87 C86 Ru3 N5 -140.7(4) . . . . ? C85 C86 Ru3 N5 101.9(4) . . . . ? C91 C86 Ru3 N5 -23.0(7) . . . . ? C85 C86 Ru3 C87 -117.4(6) . . . . ? C91 C86 Ru3 C87 117.7(8) . . . . ? C87 C86 Ru3 C85 117.4(6) . . . . ? C91 C86 Ru3 C85 -124.9(8) . . . . ? C87 C86 Ru3 C88 39.9(4) . . . . ? C85 C86 Ru3 C88 -77.5(4) . . . . ? C91 C86 Ru3 C88 157.6(7) . . . . ? C87 C86 Ru3 C84 80.4(5) . . . . ? C85 C86 Ru3 C84 -37.0(4) . . . . ? C91 C86 Ru3 C84 -161.9(7) . . . . ? C87 C86 Ru3 Cl3 119.5(4) . . . . ? C85 C86 Ru3 Cl3 2.1(5) . . . . ? C91 C86 Ru3 Cl3 -122.8(6) . . . . ? C86 C87 Ru3 N6 148.4(4) . . . . ? C88 C87 Ru3 N6 -97.4(4) . . . . ? C92 C87 Ru3 N6 26.6(6) . . . . ? C86 C87 Ru3 N5 52.5(5) . . . . ? C88 C87 Ru3 N5 166.7(3) . . . . ? C92 C87 Ru3 N5 -69.3(6) . . . . ? C88 C87 Ru3 C86 114.2(6) . . . . ? C92 C87 Ru3 C86 -121.8(8) . . . . ? C86 C87 Ru3 C85 -37.4(4) . . . . ? C88 C87 Ru3 C85 76.8(4) . . . . ? C92 C87 Ru3 C85 -159.2(6) . . . . ? C86 C87 Ru3 C88 -114.2(6) . . . . ? C92 C87 Ru3 C88 124.0(7) . . . . ? C86 C87 Ru3 C84 -78.1(5) . . . . ? C88 C87 Ru3 C84 36.1(4) . . . . ? C92 C87 Ru3 C84 160.0(7) . . . . ? C86 C87 Ru3 Cl3 -107.6(4) . . . . ? C88 C87 Ru3 Cl3 6.6(5) . . . . ? C92 C87 Ru3 Cl3 130.6(5) . . . . ? C84 C85 Ru3 N6 -58.2(9) . . . . ? C86 C85 Ru3 N6 58.0(10) . . . . ? C90 C85 Ru3 N6 178.0(7) . . . . ? C84 C85 Ru3 N5 156.1(4) . . . . ? C86 C85 Ru3 N5 -87.7(4) . . . . ? C90 C85 Ru3 N5 32.3(7) . . . . ? C84 C85 Ru3 C86 -116.2(6) . . . . ? C90 C85 Ru3 C86 120.0(9) . . . . ? C84 C85 Ru3 C87 -78.5(5) . . . . ? C86 C85 Ru3 C87 37.7(4) . . . . ? C90 C85 Ru3 C87 157.7(8) . . . . ? C84 C85 Ru3 C88 -34.6(4) . . . . ? C86 C85 Ru3 C88 81.6(4) . . . . ? C90 C85 Ru3 C88 -158.4(8) . . . . ? C86 C85 Ru3 C84 116.2(6) . . . . ? C90 C85 Ru3 C84 -123.8(9) . . . . ? C84 C85 Ru3 Cl3 65.3(4) . . . . ? C86 C85 Ru3 Cl3 -178.6(4) . . . . ? C90 C85 Ru3 Cl3 -58.5(7) . . . . ? C84 C88 Ru3 N6 -151.8(4) . . . . ? C87 C88 Ru3 N6 91.4(4) . . . . ? C93 C88 Ru3 N6 -25.4(7) . . . . ? C84 C88 Ru3 N5 75.5(10) . . . . ? C87 C88 Ru3 N5 -41.3(10) . . . . ? C93 C88 Ru3 N5 -158.1(7) . . . . ? C84 C88 Ru3 C86 77.7(4) . . . . ? C87 C88 Ru3 C86 -39.1(4) . . . . ? C93 C88 Ru3 C86 -155.8(8) . . . . ? C84 C88 Ru3 C87 116.8(5) . . . . ? C93 C88 Ru3 C87 -116.8(8) . . . . ? C84 C88 Ru3 C85 34.9(4) . . . . ? C87 C88 Ru3 C85 -81.9(4) . . . . ? C93 C88 Ru3 C85 161.4(8) . . . . ? C87 C88 Ru3 C84 -116.8(5) . . . . ? C93 C88 Ru3 C84 126.4(8) . . . . ? C84 C88 Ru3 Cl3 -59.0(4) . . . . ? C87 C88 Ru3 Cl3 -175.8(3) . . . . ? C93 C88 Ru3 Cl3 67.4(7) . . . . ? C88 C84 Ru3 N6 39.2(5) . . . . ? C85 C84 Ru3 N6 160.5(3) . . . . ? C89 C84 Ru3 N6 -80.4(9) . . . . ? C88 C84 Ru3 N5 -156.8(4) . . . . ? C85 C84 Ru3 N5 -35.5(6) . . . . ? C89 C84 Ru3 N5 83.6(8) . . . . ? C88 C84 Ru3 C86 -82.5(4) . . . . ? C85 C84 Ru3 C86 38.7(4) . . . . ? C89 C84 Ru3 C86 157.8(9) . . . . ? C88 C84 Ru3 C87 -39.2(4) . . . . ? C85 C84 Ru3 C87 82.0(4) . . . . ? C89 C84 Ru3 C87 -158.9(9) . . . . ? C88 C84 Ru3 C85 -121.3(6) . . . . ? C89 C84 Ru3 C85 119.1(10) . . . . ? C85 C84 Ru3 C88 121.3(6) . . . . ? C89 C84 Ru3 C88 -119.7(9) . . . . ? C88 C84 Ru3 Cl3 122.9(4) . . . . ? C85 C84 Ru3 Cl3 -115.8(4) . . . . ? C89 C84 Ru3 Cl3 3.3(7) . . . . ? C102 N7 Ru4 N8 0.6(5) . . . . ? C94 N7 Ru4 N8 176.8(4) . . . . ? C102 N7 Ru4 C119 102.5(5) . . . . ? C94 N7 Ru4 C119 -81.3(5) . . . . ? C102 N7 Ru4 C118 129.4(5) . . . . ? C94 N7 Ru4 C118 -54.4(4) . . . . ? C102 N7 Ru4 C120 152.6(7) . . . . ? C94 N7 Ru4 C120 -31.2(10) . . . . ? C102 N7 Ru4 C117 167.5(5) . . . . ? C94 N7 Ru4 C117 -16.3(4) . . . . ? C102 N7 Ru4 C116 -168.5(5) . . . . ? C94 N7 Ru4 C116 7.7(5) . . . . ? C102 N7 Ru4 Cl4 -87.1(5) . . . . ? C94 N7 Ru4 Cl4 89.1(4) . . . . ? C105 N8 Ru4 N7 -1.7(5) . . . . ? C108 N8 Ru4 N7 -176.7(4) . . . . ? C105 N8 Ru4 C119 -135.9(5) . . . . ? C108 N8 Ru4 C119 49.1(4) . . . . ? C105 N8 Ru4 C118 -106.1(5) . . . . ? C108 N8 Ru4 C118 78.9(5) . . . . ? C105 N8 Ru4 C120 -174.4(5) . . . . ? C108 N8 Ru4 C120 10.6(4) . . . . ? C105 N8 Ru4 C117 -131.3(7) . . . . ? C108 N8 Ru4 C117 53.7(9) . . . . ? C105 N8 Ru4 C116 165.8(4) . . . . ? C108 N8 Ru4 C116 -9.2(5) . . . . ? C105 N8 Ru4 Cl4 86.9(5) . . . . ? C108 N8 Ru4 Cl4 -88.1(4) . . . . ? C120 C119 Ru4 N7 161.0(3) . . . . ? C118 C119 Ru4 N7 44.8(5) . . . . ? C124 C119 Ru4 N7 -74.8(6) . . . . ? C120 C119 Ru4 N8 -102.4(3) . . . . ? C118 C119 Ru4 N8 141.4(4) . . . . ? C124 C119 Ru4 N8 21.8(6) . . . . ? C120 C119 Ru4 C118 116.1(5) . . . . ? C124 C119 Ru4 C118 -119.6(7) . . . . ? C118 C119 Ru4 C120 -116.1(5) . . . . ? C124 C119 Ru4 C120 124.3(6) . . . . ? C120 C119 Ru4 C117 79.0(3) . . . . ? C118 C119 Ru4 C117 -37.1(4) . . . . ? C124 C119 Ru4 C117 -156.7(6) . . . . ? C120 C119 Ru4 C116 38.5(3) . . . . ? C118 C119 Ru4 C116 -77.7(4) . . . . ? C124 C119 Ru4 C116 162.7(6) . . . . ? C120 C119 Ru4 Cl4 -5.0(4) . . . . ? C118 C119 Ru4 Cl4 -121.1(4) . . . . ? C124 C119 Ru4 Cl4 119.3(5) . . . . ? C117 C118 Ru4 N7 94.5(3) . . . . ? C119 C118 Ru4 N7 -148.6(4) . . . . ? C123 C118 Ru4 N7 -32.3(5) . . . . ? C117 C118 Ru4 N8 -168.3(3) . . . . ? C119 C118 Ru4 N8 -51.4(5) . . . . ? C123 C118 Ru4 N8 65.0(5) . . . . ? C117 C118 Ru4 C119 -117.0(6) . . . . ? C123 C118 Ru4 C119 116.3(7) . . . . ? C117 C118 Ru4 C120 -78.9(4) . . . . ? C119 C118 Ru4 C120 38.0(4) . . . . ? C123 C118 Ru4 C120 154.4(6) . . . . ? C119 C118 Ru4 C117 117.0(6) . . . . ? C123 C118 Ru4 C117 -126.7(6) . . . . ? C117 C118 Ru4 C116 -36.7(3) . . . . ? C119 C118 Ru4 C116 80.2(4) . . . . ? C123 C118 Ru4 C116 -163.4(6) . . . . ? C117 C118 Ru4 Cl4 -9.9(4) . . . . ? C119 C118 Ru4 Cl4 107.1(4) . . . . ? C123 C118 Ru4 Cl4 -136.6(5) . . . . ? C119 C120 Ru4 N7 -64.4(9) . . . . ? C116 C120 Ru4 N7 50.6(10) . . . . ? C125 C120 Ru4 N7 173.1(7) . . . . ? C119 C120 Ru4 N8 86.5(3) . . . . ? C116 C120 Ru4 N8 -158.6(3) . . . . ? C125 C120 Ru4 N8 -36.0(6) . . . . ? C116 C120 Ru4 C119 114.9(4) . . . . ? C125 C120 Ru4 C119 -122.5(7) . . . . ? C119 C120 Ru4 C118 -38.9(3) . . . . ? C116 C120 Ru4 C118 76.1(3) . . . . ? C125 C120 Ru4 C118 -161.4(7) . . . . ? C119 C120 Ru4 C117 -80.7(3) . . . . ? C116 C120 Ru4 C117 34.2(3) . . . . ? C125 C120 Ru4 C117 156.7(7) . . . . ? C119 C120 Ru4 C116 -114.9(4) . . . . ? C125 C120 Ru4 C116 122.5(7) . . . . ? C119 C120 Ru4 Cl4 176.5(3) . . . . ? C116 C120 Ru4 Cl4 -68.5(3) . . . . ? C125 C120 Ru4 Cl4 54.0(6) . . . . ? C116 C117 Ru4 N7 148.8(3) . . . . ? C118 C117 Ru4 N7 -94.3(3) . . . . ? C122 C117 Ru4 N7 26.7(7) . . . . ? C116 C117 Ru4 N8 -83.3(8) . . . . ? C118 C117 Ru4 N8 33.6(8) . . . . ? C122 C117 Ru4 N8 154.6(7) . . . . ? C116 C117 Ru4 C119 -78.2(3) . . . . ? C118 C117 Ru4 C119 38.7(3) . . . . ? C122 C117 Ru4 C119 159.6(7) . . . . ? C116 C117 Ru4 C118 -116.9(4) . . . . ? C122 C117 Ru4 C118 121.0(8) . . . . ? C116 C117 Ru4 C120 -35.5(3) . . . . ? C118 C117 Ru4 C120 81.4(3) . . . . ? C122 C117 Ru4 C120 -157.6(7) . . . . ? C118 C117 Ru4 C116 116.9(4) . . . . ? C122 C117 Ru4 C116 -122.1(8) . . . . ? C116 C117 Ru4 Cl4 56.9(3) . . . . ? C118 C117 Ru4 Cl4 173.7(3) . . . . ? C122 C117 Ru4 Cl4 -65.3(7) . . . . ? C117 C116 Ru4 N7 -42.7(4) . . . . ? C120 C116 Ru4 N7 -164.3(3) . . . . ? C121 C116 Ru4 N7 78.8(5) . . . . ? C117 C116 Ru4 N8 154.1(3) . . . . ? C120 C116 Ru4 N8 32.6(5) . . . . ? C121 C116 Ru4 N8 -84.3(5) . . . . ? C117 C116 Ru4 C119 82.4(3) . . . . ? C120 C116 Ru4 C119 -39.2(3) . . . . ? C121 C116 Ru4 C119 -156.0(5) . . . . ? C117 C116 Ru4 C118 38.0(3) . . . . ? C120 C116 Ru4 C118 -83.5(3) . . . . ? C121 C116 Ru4 C118 159.6(5) . . . . ? C117 C116 Ru4 C120 121.6(5) . . . . ? C121 C116 Ru4 C120 -116.9(6) . . . . ? C120 C116 Ru4 C117 -121.6(5) . . . . ? C121 C116 Ru4 C117 121.5(6) . . . . ? C117 C116 Ru4 Cl4 -125.8(3) . . . . ? C120 C116 Ru4 Cl4 112.6(3) . . . . ? C121 C116 Ru4 Cl4 -4.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.649 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.073 data_adp445 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*RuCl(3,5-(CH3)2C6H3NC(CF3))2CH)' _chemical_melting_point ? _chemical_formula_moiety 'C31 H34 Cl F6 N2 Ru' _chemical_formula_sum 'C31 H34 Cl F6 N2 Ru' _chemical_formula_weight 685.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6771(7) _cell_length_b 8.2347(5) _cell_length_c 30.471(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.430(5) _cell_angle_gamma 90.00 _cell_volume 2980.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 6886 _cell_measurement_theta_min 2.8626 _cell_measurement_theta_max 27.3277 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.378 _exptl_crystal_size_mid 0.168 _exptl_crystal_size_min 0.106 _exptl_absorpt_correction_T_min 0.66549 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 0.677 _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_measurement_method '\w and \p scans' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_detector_area_resol_mean 8.2812 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21857 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5224 _reflns_number_gt 3260 _reflns_threshold_expression I>2/s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick G.M., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick G.M., 2008)' _computing_molecular_graphics 'ORTEP-3 for windows 2.02 (Farrugia, 2008)' _computing_publication_material 'WinGX 1.80.05 (Farrugia, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5224 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1913(4) 0.1339(6) 0.83080(17) 0.0210(11) Uani 1 1 d . . . C2 C -0.2222(4) 0.0557(6) 0.86470(19) 0.0271(13) Uani 1 1 d . . . H2 H -0.1682 -0.0042 0.8889 0.033 Uiso 1 1 calc R . . C3 C -0.3334(4) 0.0659(6) 0.8630(2) 0.0294(13) Uani 1 1 d . . . C4 C -0.4105(4) 0.1506(7) 0.8268(2) 0.0315(14) Uani 1 1 d . . . H4 H -0.4865 0.1559 0.8254 0.038 Uiso 1 1 calc R . . C5 C -0.3804(4) 0.2286(6) 0.79230(19) 0.0297(12) Uani 1 1 d . . . C6 C -0.2679(4) 0.2191(5) 0.79497(18) 0.0243(12) Uani 1 1 d . . . H6 H -0.2448 0.2714 0.7721 0.029 Uiso 1 1 calc R . . C7 C -0.3671(5) -0.0150(8) 0.9005(2) 0.0463(17) Uani 1 1 d . . . H7A H -0.4260 0.0493 0.9064 0.069 Uiso 1 1 calc R . . H7B H -0.3015 -0.0227 0.9294 0.069 Uiso 1 1 calc R . . H7C H -0.3959 -0.1242 0.8902 0.069 Uiso 1 1 calc R . . C8 C -0.4647(5) 0.3209(8) 0.7537(2) 0.0446(16) Uani 1 1 d . . . H8A H -0.4780 0.2646 0.7239 0.067 Uiso 1 1 calc R . . H8B H -0.4361 0.4304 0.7520 0.067 Uiso 1 1 calc R . . H8C H -0.5355 0.3282 0.7598 0.067 Uiso 1 1 calc R . . C9 C -0.0462(4) 0.0223(6) 0.80571(17) 0.0204(11) Uani 1 1 d . . . C10 C -0.1366(4) -0.0670(6) 0.7663(2) 0.0297(13) Uani 1 1 d . . . C11 C 0.0625(4) -0.0140(6) 0.80843(17) 0.0207(11) Uani 1 1 d . . . H11 H 0.0698 -0.0941 0.7872 0.025 Uiso 1 1 calc R . . C12 C 0.1625(4) 0.0530(6) 0.83859(17) 0.0171(11) Uani 1 1 d . . . C13 C 0.2678(4) -0.0192(6) 0.8317(2) 0.0288(13) Uani 1 1 d . . . C14 C 0.2818(4) 0.2330(6) 0.89520(17) 0.0204(11) Uani 1 1 d . . . C15 C 0.3300(4) 0.3408(6) 0.87309(18) 0.0235(12) Uani 1 1 d . . . H15 H 0.2905 0.3720 0.8416 0.028 Uiso 1 1 calc R . . C16 C 0.4375(4) 0.4045(6) 0.89707(19) 0.0250(12) Uani 1 1 d . . . C17 C 0.4917(4) 0.3582(6) 0.9424(2) 0.0280(13) Uani 1 1 d . . . H17 H 0.5646 0.4005 0.9587 0.034 Uiso 1 1 calc R . . C18 C 0.4437(4) 0.2504(7) 0.96581(17) 0.0249(10) Uani 1 1 d . . . C19 C 0.3364(4) 0.1908(6) 0.94142(18) 0.0225(12) Uani 1 1 d . . . H19 H 0.3006 0.1208 0.9567 0.027 Uiso 1 1 calc R . . C20 C 0.4886(5) 0.5228(6) 0.8725(2) 0.0358(14) Uani 1 1 d . . . H20A H 0.4476 0.6259 0.8679 0.054 Uiso 1 1 calc R . . H20B H 0.4839 0.4782 0.8421 0.054 Uiso 1 1 calc R . . H20C H 0.5677 0.5412 0.8917 0.054 Uiso 1 1 calc R . . C21 C 0.5044(5) 0.2076(6) 1.01646(19) 0.0362(15) Uani 1 1 d . . . H21A H 0.5095 0.3040 1.0360 0.054 Uiso 1 1 calc R . . H21B H 0.5803 0.1688 1.0205 0.054 Uiso 1 1 calc R . . H21C H 0.4629 0.1220 1.0259 0.054 Uiso 1 1 calc R . . C22 C 0.0167(4) 0.5076(5) 0.88983(18) 0.0202(11) Uani 1 1 d . . . C23 C 0.1163(4) 0.4756(6) 0.92870(19) 0.0254(12) Uani 1 1 d . . . C24 C 0.0891(4) 0.3689(6) 0.95960(18) 0.0282(13) Uani 1 1 d . . . C25 C -0.0335(4) 0.3472(6) 0.94113(18) 0.0231(12) Uani 1 1 d . . . C26 C -0.0758(4) 0.4390(6) 0.90001(18) 0.0245(12) Uani 1 1 d . . . C27 C 0.0084(5) 0.6179(7) 0.8505(2) 0.0415(15) Uani 1 1 d . . . H27A H 0.0027 0.7304 0.8600 0.062 Uiso 1 1 calc R . . H27B H -0.0587 0.5905 0.8235 0.062 Uiso 1 1 calc R . . H27C H 0.0756 0.6061 0.8419 0.062 Uiso 1 1 calc R . . C28 C 0.2259(5) 0.5599(7) 0.9382(2) 0.0442(17) Uani 1 1 d . . . H28A H 0.2394 0.5758 0.9087 0.066 Uiso 1 1 calc R . . H28B H 0.2865 0.4938 0.9595 0.066 Uiso 1 1 calc R . . H28C H 0.2239 0.6656 0.9527 0.066 Uiso 1 1 calc R . . C29 C 0.1655(5) 0.3079(8) 1.0060(2) 0.0513(18) Uani 1 1 d . . . H29A H 0.2439 0.3279 1.0090 0.077 Uiso 1 1 calc R . . H29B H 0.1538 0.1910 1.0083 0.077 Uiso 1 1 calc R . . H29C H 0.1489 0.3647 1.0311 0.077 Uiso 1 1 calc R . . C30 C -0.0966(5) 0.2585(7) 0.96699(19) 0.0391(14) Uani 1 1 d . . . H30A H -0.0889 0.3167 0.9960 0.059 Uiso 1 1 calc R . . H30B H -0.0660 0.1486 0.9745 0.059 Uiso 1 1 calc R . . H30C H -0.1764 0.2521 0.9474 0.059 Uiso 1 1 calc R . . C31 C -0.1973(4) 0.4803(7) 0.8739(2) 0.0340(14) Uani 1 1 d . . . H31A H -0.2456 0.3955 0.8793 0.051 Uiso 1 1 calc R . . H31B H -0.2101 0.4875 0.8403 0.051 Uiso 1 1 calc R . . H31C H -0.2152 0.5848 0.8850 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.06897(11) -0.01337(15) 0.93245(5) 0.0268(3) Uani 1 1 d . . . F1 F -0.1939(3) 0.0346(4) 0.73173(11) 0.0433(9) Uani 1 1 d . . . F2 F -0.2139(2) -0.1423(4) 0.78057(11) 0.0391(8) Uani 1 1 d . . . F3 F -0.0956(2) -0.1831(4) 0.74647(11) 0.0364(8) Uani 1 1 d . . . F4 F 0.2471(2) -0.1634(4) 0.81051(12) 0.0388(8) Uani 1 1 d . . . F5 F 0.3522(3) -0.0449(4) 0.87167(12) 0.0464(9) Uani 1 1 d . . . F6 F 0.3065(3) 0.0758(4) 0.80521(13) 0.0498(10) Uani 1 1 d . . . N1 N -0.0726(3) 0.1210(5) 0.83491(14) 0.0188(9) Uani 1 1 d . . . N2 N 0.1713(3) 0.1658(5) 0.86994(14) 0.0190(9) Uani 1 1 d . . . Ru1 Ru 0.04012(3) 0.24309(5) 0.890382(13) 0.01765(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.013(2) 0.028(3) 0.027(3) -0.004(2) 0.013(2) -0.004(2) C2 0.017(3) 0.037(3) 0.031(3) 0.000(3) 0.013(2) -0.001(2) C3 0.021(3) 0.034(3) 0.041(3) -0.001(3) 0.020(3) -0.004(2) C4 0.014(3) 0.038(3) 0.045(4) -0.004(3) 0.013(3) -0.001(2) C5 0.020(3) 0.035(3) 0.033(3) 0.001(3) 0.008(2) 0.001(3) C6 0.026(3) 0.025(3) 0.025(3) -0.001(2) 0.011(2) 0.001(2) C7 0.029(3) 0.057(4) 0.066(5) 0.024(4) 0.034(3) 0.004(3) C8 0.026(3) 0.061(4) 0.046(4) 0.003(3) 0.011(3) 0.010(3) C9 0.024(3) 0.021(3) 0.019(3) -0.001(2) 0.011(2) 0.000(2) C10 0.028(3) 0.028(3) 0.035(3) -0.003(3) 0.015(3) 0.000(2) C11 0.020(3) 0.026(3) 0.021(3) -0.005(2) 0.013(2) 0.000(2) C12 0.017(3) 0.021(3) 0.022(3) 0.006(2) 0.017(2) 0.003(2) C13 0.023(3) 0.033(3) 0.034(3) -0.004(3) 0.016(3) 0.002(2) C14 0.015(2) 0.022(3) 0.028(3) 0.000(3) 0.011(2) 0.001(2) C15 0.026(3) 0.022(3) 0.025(3) 0.000(2) 0.012(2) 0.001(2) C16 0.017(3) 0.028(3) 0.036(3) -0.003(3) 0.016(2) -0.002(2) C17 0.014(3) 0.030(3) 0.041(4) -0.005(3) 0.011(3) 0.000(2) C18 0.021(2) 0.026(2) 0.026(3) -0.006(3) 0.007(2) 0.000(3) C19 0.024(3) 0.024(3) 0.025(3) -0.001(2) 0.016(2) 0.000(2) C20 0.035(3) 0.033(3) 0.047(4) -0.005(3) 0.023(3) -0.014(3) C21 0.034(3) 0.036(3) 0.030(3) -0.002(3) 0.001(3) -0.001(2) C22 0.028(3) 0.014(2) 0.025(3) 0.002(2) 0.016(2) 0.003(2) C23 0.023(3) 0.019(3) 0.036(3) -0.010(2) 0.013(3) -0.005(2) C24 0.033(3) 0.035(3) 0.016(3) -0.004(2) 0.007(2) 0.006(3) C25 0.026(3) 0.022(3) 0.027(3) -0.005(2) 0.016(2) 0.005(2) C26 0.023(3) 0.028(3) 0.027(3) -0.003(2) 0.015(2) 0.004(2) C27 0.055(4) 0.037(3) 0.039(4) 0.004(3) 0.025(3) 0.002(3) C28 0.031(3) 0.036(3) 0.070(5) -0.023(3) 0.022(3) -0.005(3) C29 0.062(4) 0.063(4) 0.018(3) -0.009(3) 0.002(3) 0.025(3) C30 0.059(4) 0.044(3) 0.034(3) -0.005(3) 0.041(3) -0.001(3) C31 0.021(3) 0.039(3) 0.043(4) -0.006(3) 0.011(3) 0.009(3) Cl1 0.0295(7) 0.0288(7) 0.0271(7) 0.0042(6) 0.0162(6) 0.0030(6) F1 0.046(2) 0.051(2) 0.0233(18) -0.0075(16) -0.0009(16) 0.0110(17) F2 0.0246(17) 0.0421(19) 0.052(2) -0.0159(17) 0.0146(16) -0.0139(15) F3 0.0257(17) 0.0430(17) 0.040(2) -0.0215(15) 0.0114(15) 0.0005(14) F4 0.0265(17) 0.0427(18) 0.052(2) -0.0218(17) 0.0191(16) 0.0010(15) F5 0.0261(18) 0.060(2) 0.047(2) -0.0181(18) 0.0049(16) 0.0196(16) F6 0.042(2) 0.059(2) 0.070(3) -0.009(2) 0.047(2) -0.0080(17) N1 0.012(2) 0.029(2) 0.017(2) -0.0004(19) 0.0071(18) 0.0009(17) N2 0.016(2) 0.023(2) 0.021(2) 0.0000(19) 0.0101(19) -0.0011(17) Ru1 0.01535(18) 0.0244(2) 0.01683(19) -0.0012(2) 0.01014(14) 0.0001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.374(7) . ? C1 C2 1.384(7) . ? C1 N1 1.470(5) . ? C2 C3 1.395(7) . ? C2 H2 0.9500 . ? C3 C4 1.380(7) . ? C3 C7 1.510(7) . ? C4 C5 1.394(7) . ? C4 H4 0.9500 . ? C5 C6 1.402(7) . ? C5 C8 1.492(7) . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.331(6) . ? C9 C11 1.384(6) . ? C9 C10 1.528(7) . ? C10 F3 1.330(6) . ? C10 F1 1.343(6) . ? C10 F2 1.353(6) . ? C11 C12 1.394(7) . ? C11 H11 0.9500 . ? C12 N2 1.309(6) . ? C12 C13 1.541(6) . ? C13 F5 1.328(6) . ? C13 F4 1.333(6) . ? C13 F6 1.335(6) . ? C14 C19 1.379(7) . ? C14 C15 1.380(7) . ? C14 N2 1.453(6) . ? C15 C16 1.403(7) . ? C15 H15 0.9500 . ? C16 C17 1.364(7) . ? C16 C20 1.506(7) . ? C17 C18 1.404(7) . ? C17 H17 0.9500 . ? C18 C19 1.392(7) . ? C18 C21 1.506(7) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.422(7) . ? C22 C26 1.430(6) . ? C22 C27 1.479(7) . ? C22 Ru1 2.197(4) . ? C23 C24 1.416(7) . ? C23 C28 1.488(7) . ? C23 Ru1 2.275(5) . ? C24 C25 1.468(7) . ? C24 C29 1.494(7) . ? C24 Ru1 2.234(5) . ? C25 C26 1.400(7) . ? C25 C30 1.495(7) . ? C25 Ru1 2.237(5) . ? C26 C31 1.505(7) . ? C26 Ru1 2.269(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? Cl1 Ru1 2.4310(13) . ? N1 Ru1 2.055(4) . ? N2 Ru1 2.069(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 121.7(4) . . ? C6 C1 N1 121.6(4) . . ? C2 C1 N1 116.8(4) . . ? C1 C2 C3 119.3(5) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? C4 C3 C2 119.0(5) . . ? C4 C3 C7 121.3(5) . . ? C2 C3 C7 119.7(5) . . ? C3 C4 C5 122.1(5) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C4 C5 C6 118.1(5) . . ? C4 C5 C8 121.3(5) . . ? C6 C5 C8 120.6(5) . . ? C1 C6 C5 119.8(5) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C11 124.7(5) . . ? N1 C9 C10 121.7(4) . . ? C11 C9 C10 113.6(4) . . ? F3 C10 F1 106.4(4) . . ? F3 C10 F2 105.0(4) . . ? F1 C10 F2 106.5(4) . . ? F3 C10 C9 113.5(4) . . ? F1 C10 C9 111.6(4) . . ? F2 C10 C9 113.3(4) . . ? C9 C11 C12 127.7(5) . . ? C9 C11 H11 116.2 . . ? C12 C11 H11 116.2 . . ? N2 C12 C11 126.0(4) . . ? N2 C12 C13 121.0(4) . . ? C11 C12 C13 112.9(4) . . ? F5 C13 F4 105.2(4) . . ? F5 C13 F6 107.4(4) . . ? F4 C13 F6 106.3(4) . . ? F5 C13 C12 113.3(4) . . ? F4 C13 C12 112.1(4) . . ? F6 C13 C12 112.1(4) . . ? C19 C14 C15 120.7(5) . . ? C19 C14 N2 119.5(4) . . ? C15 C14 N2 119.8(4) . . ? C14 C15 C16 120.1(5) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 118.5(5) . . ? C17 C16 C20 122.1(5) . . ? C15 C16 C20 119.4(5) . . ? C16 C17 C18 122.5(5) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C19 C18 C17 117.9(5) . . ? C19 C18 C21 121.3(5) . . ? C17 C18 C21 120.8(4) . . ? C14 C19 C18 120.3(5) . . ? C14 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C26 107.7(4) . . ? C23 C22 C27 125.5(5) . . ? C26 C22 C27 125.9(5) . . ? C23 C22 Ru1 74.5(3) . . ? C26 C22 Ru1 74.1(3) . . ? C27 C22 Ru1 125.9(4) . . ? C24 C23 C22 108.5(4) . . ? C24 C23 C28 126.0(5) . . ? C22 C23 C28 125.0(5) . . ? C24 C23 Ru1 70.2(3) . . ? C22 C23 Ru1 68.5(3) . . ? C28 C23 Ru1 133.9(4) . . ? C23 C24 C25 106.9(4) . . ? C23 C24 C29 127.6(5) . . ? C25 C24 C29 124.9(5) . . ? C23 C24 Ru1 73.3(3) . . ? C25 C24 Ru1 70.9(3) . . ? C29 C24 Ru1 127.7(4) . . ? C26 C25 C24 107.5(4) . . ? C26 C25 C30 128.8(5) . . ? C24 C25 C30 123.2(5) . . ? C26 C25 Ru1 73.2(3) . . ? C24 C25 Ru1 70.7(3) . . ? C30 C25 Ru1 127.3(3) . . ? C25 C26 C22 108.7(4) . . ? C25 C26 C31 126.7(5) . . ? C22 C26 C31 124.1(5) . . ? C25 C26 Ru1 70.7(3) . . ? C22 C26 Ru1 68.6(3) . . ? C31 C26 Ru1 132.9(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C9 N1 C1 118.4(4) . . ? C9 N1 Ru1 125.7(3) . . ? C1 N1 Ru1 115.6(3) . . ? C12 N2 C14 118.5(4) . . ? C12 N2 Ru1 124.4(3) . . ? C14 N2 Ru1 116.8(3) . . ? N1 Ru1 N2 90.17(15) . . ? N1 Ru1 C22 115.17(17) . . ? N2 Ru1 C22 115.04(16) . . ? N1 Ru1 C24 152.58(17) . . ? N2 Ru1 C24 116.03(18) . . ? C22 Ru1 C24 62.62(19) . . ? N1 Ru1 C25 114.71(17) . . ? N2 Ru1 C25 154.03(17) . . ? C22 Ru1 C25 62.45(18) . . ? C24 Ru1 C25 38.33(18) . . ? N1 Ru1 C26 99.11(17) . . ? N2 Ru1 C26 151.95(17) . . ? C22 Ru1 C26 37.31(17) . . ? C24 Ru1 C26 61.82(18) . . ? C25 Ru1 C26 36.18(18) . . ? N1 Ru1 C23 151.96(17) . . ? N2 Ru1 C23 99.88(17) . . ? C22 Ru1 C23 37.03(18) . . ? C24 Ru1 C23 36.58(18) . . ? C25 Ru1 C23 61.80(18) . . ? C26 Ru1 C23 60.89(18) . . ? N1 Ru1 Cl1 86.69(11) . . ? N2 Ru1 Cl1 84.41(11) . . ? C22 Ru1 Cl1 149.33(13) . . ? C24 Ru1 Cl1 87.93(14) . . ? C25 Ru1 Cl1 89.47(13) . . ? C26 Ru1 Cl1 122.30(14) . . ? C23 Ru1 Cl1 120.12(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.1(8) . . . . ? N1 C1 C2 C3 179.0(4) . . . . ? C1 C2 C3 C4 1.5(8) . . . . ? C1 C2 C3 C7 -178.3(5) . . . . ? C2 C3 C4 C5 -1.0(8) . . . . ? C7 C3 C4 C5 178.8(5) . . . . ? C3 C4 C5 C6 0.1(8) . . . . ? C3 C4 C5 C8 -179.5(5) . . . . ? C2 C1 C6 C5 0.2(7) . . . . ? N1 C1 C6 C5 -179.9(4) . . . . ? C4 C5 C6 C1 0.3(7) . . . . ? C8 C5 C6 C1 179.9(5) . . . . ? N1 C9 C10 F3 -167.7(4) . . . . ? C11 C9 C10 F3 10.4(6) . . . . ? N1 C9 C10 F1 72.1(6) . . . . ? C11 C9 C10 F1 -109.8(5) . . . . ? N1 C9 C10 F2 -48.1(6) . . . . ? C11 C9 C10 F2 130.0(5) . . . . ? N1 C9 C11 C12 -5.7(8) . . . . ? C10 C9 C11 C12 176.3(5) . . . . ? C9 C11 C12 N2 -0.9(8) . . . . ? C9 C11 C12 C13 179.4(5) . . . . ? N2 C12 C13 F5 40.7(6) . . . . ? C11 C12 C13 F5 -139.5(5) . . . . ? N2 C12 C13 F4 159.6(4) . . . . ? C11 C12 C13 F4 -20.7(6) . . . . ? N2 C12 C13 F6 -81.1(6) . . . . ? C11 C12 C13 F6 98.7(5) . . . . ? C19 C14 C15 C16 2.3(7) . . . . ? N2 C14 C15 C16 -179.1(4) . . . . ? C14 C15 C16 C17 -0.5(7) . . . . ? C14 C15 C16 C20 -179.7(4) . . . . ? C15 C16 C17 C18 -0.4(8) . . . . ? C20 C16 C17 C18 178.8(5) . . . . ? C16 C17 C18 C19 -0.5(8) . . . . ? C16 C17 C18 C21 -177.5(5) . . . . ? C15 C14 C19 C18 -3.2(7) . . . . ? N2 C14 C19 C18 178.2(4) . . . . ? C17 C18 C19 C14 2.3(7) . . . . ? C21 C18 C19 C14 179.3(5) . . . . ? C26 C22 C23 C24 8.3(5) . . . . ? C27 C22 C23 C24 177.8(5) . . . . ? Ru1 C22 C23 C24 -58.9(3) . . . . ? C26 C22 C23 C28 -163.5(5) . . . . ? C27 C22 C23 C28 6.0(8) . . . . ? Ru1 C22 C23 C28 129.3(5) . . . . ? C26 C22 C23 Ru1 67.2(3) . . . . ? C27 C22 C23 Ru1 -123.3(5) . . . . ? C22 C23 C24 C25 -5.5(5) . . . . ? C28 C23 C24 C25 166.2(5) . . . . ? Ru1 C23 C24 C25 -63.4(3) . . . . ? C22 C23 C24 C29 -177.0(5) . . . . ? C28 C23 C24 C29 -5.3(8) . . . . ? Ru1 C23 C24 C29 125.1(5) . . . . ? C22 C23 C24 Ru1 57.9(3) . . . . ? C28 C23 C24 Ru1 -130.4(5) . . . . ? C23 C24 C25 C26 0.6(6) . . . . ? C29 C24 C25 C26 172.4(5) . . . . ? Ru1 C24 C25 C26 -64.4(3) . . . . ? C23 C24 C25 C30 -172.5(4) . . . . ? C29 C24 C25 C30 -0.7(8) . . . . ? Ru1 C24 C25 C30 122.6(5) . . . . ? C23 C24 C25 Ru1 64.9(3) . . . . ? C29 C24 C25 Ru1 -123.3(5) . . . . ? C24 C25 C26 C22 4.5(6) . . . . ? C30 C25 C26 C22 177.1(5) . . . . ? Ru1 C25 C26 C22 -58.2(3) . . . . ? C24 C25 C26 C31 -167.5(5) . . . . ? C30 C25 C26 C31 5.0(9) . . . . ? Ru1 C25 C26 C31 129.7(5) . . . . ? C24 C25 C26 Ru1 62.8(3) . . . . ? C30 C25 C26 Ru1 -124.7(5) . . . . ? C23 C22 C26 C25 -8.0(5) . . . . ? C27 C22 C26 C25 -177.4(5) . . . . ? Ru1 C22 C26 C25 59.5(3) . . . . ? C23 C22 C26 C31 164.3(5) . . . . ? C27 C22 C26 C31 -5.1(8) . . . . ? Ru1 C22 C26 C31 -128.2(5) . . . . ? C23 C22 C26 Ru1 -67.5(3) . . . . ? C27 C22 C26 Ru1 123.1(5) . . . . ? C11 C9 N1 C1 -173.4(5) . . . . ? C10 C9 N1 C1 4.5(7) . . . . ? C11 C9 N1 Ru1 0.2(7) . . . . ? C10 C9 N1 Ru1 178.1(3) . . . . ? C6 C1 N1 C9 -74.9(6) . . . . ? C2 C1 N1 C9 105.0(5) . . . . ? C6 C1 N1 Ru1 110.8(4) . . . . ? C2 C1 N1 Ru1 -69.3(5) . . . . ? C11 C12 N2 C14 -173.9(4) . . . . ? C13 C12 N2 C14 5.8(7) . . . . ? C11 C12 N2 Ru1 11.4(7) . . . . ? C13 C12 N2 Ru1 -168.9(3) . . . . ? C19 C14 N2 C12 -106.4(5) . . . . ? C15 C14 N2 C12 75.0(6) . . . . ? C19 C14 N2 Ru1 68.6(5) . . . . ? C15 C14 N2 Ru1 -110.0(4) . . . . ? C9 N1 Ru1 N2 6.6(4) . . . . ? C1 N1 Ru1 N2 -179.6(3) . . . . ? C9 N1 Ru1 C22 124.6(4) . . . . ? C1 N1 Ru1 C22 -61.7(4) . . . . ? C9 N1 Ru1 C24 -156.8(4) . . . . ? C1 N1 Ru1 C24 16.9(6) . . . . ? C9 N1 Ru1 C25 -165.7(4) . . . . ? C1 N1 Ru1 C25 8.1(4) . . . . ? C9 N1 Ru1 C26 160.0(4) . . . . ? C1 N1 Ru1 C26 -26.2(4) . . . . ? C9 N1 Ru1 C23 118.3(5) . . . . ? C1 N1 Ru1 C23 -67.9(5) . . . . ? C9 N1 Ru1 Cl1 -77.8(4) . . . . ? C1 N1 Ru1 Cl1 96.0(3) . . . . ? C12 N2 Ru1 N1 -12.0(4) . . . . ? C14 N2 Ru1 N1 173.2(3) . . . . ? C12 N2 Ru1 C22 -130.1(4) . . . . ? C14 N2 Ru1 C22 55.2(4) . . . . ? C12 N2 Ru1 C24 159.6(4) . . . . ? C14 N2 Ru1 C24 -15.2(4) . . . . ? C12 N2 Ru1 C25 151.8(4) . . . . ? C14 N2 Ru1 C25 -22.9(6) . . . . ? C12 N2 Ru1 C26 -122.0(4) . . . . ? C14 N2 Ru1 C26 63.2(5) . . . . ? C12 N2 Ru1 C23 -165.7(4) . . . . ? C14 N2 Ru1 C23 19.5(4) . . . . ? C12 N2 Ru1 Cl1 74.6(4) . . . . ? C14 N2 Ru1 Cl1 -100.1(3) . . . . ? C23 C22 Ru1 N1 -175.1(3) . . . . ? C26 C22 Ru1 N1 70.9(3) . . . . ? C27 C22 Ru1 N1 -52.3(5) . . . . ? C23 C22 Ru1 N2 -72.3(3) . . . . ? C26 C22 Ru1 N2 173.7(3) . . . . ? C27 C22 Ru1 N2 50.6(5) . . . . ? C23 C22 Ru1 C24 35.4(3) . . . . ? C26 C22 Ru1 C24 -78.6(3) . . . . ? C27 C22 Ru1 C24 158.3(5) . . . . ? C23 C22 Ru1 C25 78.8(3) . . . . ? C26 C22 Ru1 C25 -35.2(3) . . . . ? C27 C22 Ru1 C25 -158.3(5) . . . . ? C23 C22 Ru1 C26 114.0(4) . . . . ? C27 C22 Ru1 C26 -123.2(6) . . . . ? C26 C22 Ru1 C23 -114.0(4) . . . . ? C27 C22 Ru1 C23 122.8(6) . . . . ? C23 C22 Ru1 Cl1 53.0(4) . . . . ? C26 C22 Ru1 Cl1 -61.0(4) . . . . ? C27 C22 Ru1 Cl1 175.8(3) . . . . ? C23 C24 Ru1 N1 -128.2(4) . . . . ? C25 C24 Ru1 N1 -13.0(5) . . . . ? C29 C24 Ru1 N1 106.8(6) . . . . ? C23 C24 Ru1 N2 70.3(3) . . . . ? C25 C24 Ru1 N2 -174.5(3) . . . . ? C29 C24 Ru1 N2 -54.7(6) . . . . ? C23 C24 Ru1 C22 -35.8(3) . . . . ? C25 C24 Ru1 C22 79.4(3) . . . . ? C29 C24 Ru1 C22 -160.8(6) . . . . ? C23 C24 Ru1 C25 -115.2(4) . . . . ? C29 C24 Ru1 C25 119.9(7) . . . . ? C23 C24 Ru1 C26 -78.2(3) . . . . ? C25 C24 Ru1 C26 37.0(3) . . . . ? C29 C24 Ru1 C26 156.8(6) . . . . ? C25 C24 Ru1 C23 115.2(4) . . . . ? C29 C24 Ru1 C23 -125.0(6) . . . . ? C23 C24 Ru1 Cl1 153.0(3) . . . . ? C25 C24 Ru1 Cl1 -91.8(3) . . . . ? C29 C24 Ru1 Cl1 28.1(5) . . . . ? C26 C25 Ru1 N1 -70.5(3) . . . . ? C24 C25 Ru1 N1 173.4(3) . . . . ? C30 C25 Ru1 N1 55.9(5) . . . . ? C26 C25 Ru1 N2 127.4(4) . . . . ? C24 C25 Ru1 N2 11.3(5) . . . . ? C30 C25 Ru1 N2 -106.3(5) . . . . ? C26 C25 Ru1 C22 36.3(3) . . . . ? C24 C25 Ru1 C22 -79.8(3) . . . . ? C30 C25 Ru1 C22 162.6(5) . . . . ? C26 C25 Ru1 C24 116.1(4) . . . . ? C30 C25 Ru1 C24 -117.5(6) . . . . ? C24 C25 Ru1 C26 -116.1(4) . . . . ? C30 C25 Ru1 C26 126.4(6) . . . . ? C26 C25 Ru1 C23 78.3(3) . . . . ? C24 C25 Ru1 C23 -37.7(3) . . . . ? C30 C25 Ru1 C23 -155.3(5) . . . . ? C26 C25 Ru1 Cl1 -156.6(3) . . . . ? C24 C25 Ru1 Cl1 87.3(3) . . . . ? C30 C25 Ru1 Cl1 -30.2(5) . . . . ? C25 C26 Ru1 N1 119.9(3) . . . . ? C22 C26 Ru1 N1 -120.0(3) . . . . ? C31 C26 Ru1 N1 -2.8(5) . . . . ? C25 C26 Ru1 N2 -132.2(4) . . . . ? C22 C26 Ru1 N2 -12.1(5) . . . . ? C31 C26 Ru1 N2 105.1(6) . . . . ? C25 C26 Ru1 C22 -120.1(4) . . . . ? C31 C26 Ru1 C22 117.3(6) . . . . ? C25 C26 Ru1 C24 -39.2(3) . . . . ? C22 C26 Ru1 C24 80.9(3) . . . . ? C31 C26 Ru1 C24 -161.8(6) . . . . ? C22 C26 Ru1 C25 120.1(4) . . . . ? C31 C26 Ru1 C25 -122.6(7) . . . . ? C25 C26 Ru1 C23 -81.1(3) . . . . ? C22 C26 Ru1 C23 39.0(3) . . . . ? C31 C26 Ru1 C23 156.3(6) . . . . ? C25 C26 Ru1 Cl1 28.0(3) . . . . ? C22 C26 Ru1 Cl1 148.1(2) . . . . ? C31 C26 Ru1 Cl1 -94.6(5) . . . . ? C24 C23 Ru1 N1 129.7(4) . . . . ? C22 C23 Ru1 N1 9.4(5) . . . . ? C28 C23 Ru1 N1 -109.0(6) . . . . ? C24 C23 Ru1 N2 -120.8(3) . . . . ? C22 C23 Ru1 N2 118.8(3) . . . . ? C28 C23 Ru1 N2 0.4(6) . . . . ? C24 C23 Ru1 C22 120.3(4) . . . . ? C28 C23 Ru1 C22 -118.4(7) . . . . ? C22 C23 Ru1 C24 -120.3(4) . . . . ? C28 C23 Ru1 C24 121.3(7) . . . . ? C24 C23 Ru1 C25 39.6(3) . . . . ? C22 C23 Ru1 C25 -80.8(3) . . . . ? C28 C23 Ru1 C25 160.8(6) . . . . ? C24 C23 Ru1 C26 81.0(3) . . . . ? C22 C23 Ru1 C26 -39.3(3) . . . . ? C28 C23 Ru1 C26 -157.7(6) . . . . ? C24 C23 Ru1 Cl1 -31.6(3) . . . . ? C22 C23 Ru1 Cl1 -151.9(2) . . . . ? C28 C23 Ru1 Cl1 89.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.324 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.105 data_adp640 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cp*RuCl((3,5-(CF3)2C6H3NC(CF3))2CH)' _chemical_melting_point ? _chemical_formula_moiety 'C31 H22 Cl F18 N2 Ru' _chemical_formula_sum 'C31 H22 Cl F18 N2 Ru' _chemical_formula_weight 901.03 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 13.3244(2) _cell_length_b 8.1593(1) _cell_length_c 15.5064(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.807(2) _cell_angle_gamma 90.00 _cell_volume 1643.88(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12292 _cell_measurement_theta_min 3.3988 _cell_measurement_theta_max 76.8584 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.2119 _exptl_crystal_size_mid 0.0461 _exptl_crystal_size_min 0.0324 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 5.822 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.523 _exptl_absorpt_correction_T_max 0.851 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; 2969 Friedel pairs were measured. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3196 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15151 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 77.06 _reflns_number_total 6666 _reflns_number_gt 6507 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick G.M., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick G.M., 2008)' _computing_molecular_graphics 'ORTEP-3 for windows 2.02 (Farrugia, 2008)' _computing_publication_material 'WinGX 1.80.05 (Farrugia, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+1.1287P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(7) _refine_ls_number_reflns 6666 _refine_ls_number_parameters 483 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.011159(15) 0.08863(3) 0.233321(14) 0.01588(7) Uani 1 1 d . . . Cl1 Cl 0.00030(7) 0.35334(10) 0.15999(6) 0.02166(16) Uani 1 1 d . . . N1 N -0.1120(2) 0.1713(3) 0.28262(19) 0.0148(5) Uani 1 1 d . . . C1 C -0.2124(2) 0.1261(4) 0.2317(2) 0.0175(7) Uani 1 1 d . . . C2 C -0.2692(3) 0.0061(4) 0.2612(2) 0.0190(6) Uani 1 1 d . . . H2 H -0.2423 -0.0494 0.3152 0.023 Uiso 1 1 calc R . . C3 C -0.3668(3) -0.0333(5) 0.2110(3) 0.0225(7) Uani 1 1 d . . . C7 C -0.4261(3) -0.1725(5) 0.2391(3) 0.0278(8) Uani 1 1 d . . . F1 F -0.4012(3) -0.1972(5) 0.3256(2) 0.0612(10) Uani 1 1 d . . . F2 F -0.4082(2) -0.3118(3) 0.2005(2) 0.0428(6) Uani 1 1 d . . . F3 F -0.5272(2) -0.1470(4) 0.2162(2) 0.0424(7) Uani 1 1 d . . . C4 C -0.4072(3) 0.0483(4) 0.1322(3) 0.0249(8) Uani 1 1 d . . . H4 H -0.4738 0.0218 0.0983 0.030 Uiso 1 1 calc R . . C5 C -0.3486(3) 0.1691(5) 0.1041(3) 0.0255(7) Uani 1 1 d . . . C8 C -0.3898(3) 0.2598(6) 0.0197(3) 0.0357(9) Uani 1 1 d . . . F4 F -0.4882(3) 0.2428(6) -0.0096(3) 0.0810(15) Uani 1 1 d . . . F5 F -0.3727(5) 0.4167(5) 0.0270(4) 0.121(3) Uani 1 1 d . . . F6 F -0.3466(5) 0.2179(10) -0.0424(3) 0.142(3) Uani 1 1 d . . . C6 C -0.2507(3) 0.2085(4) 0.1526(2) 0.0206(7) Uani 1 1 d . . . H6 H -0.2107 0.2901 0.1321 0.025 Uiso 1 1 calc R . . C9 C -0.1066(3) 0.2786(4) 0.3475(2) 0.0191(6) Uani 1 1 d . . . C10 C -0.2054(3) 0.3526(5) 0.3663(3) 0.0237(7) Uani 1 1 d . . . F7 F -0.18478(19) 0.4621(4) 0.4323(2) 0.0413(7) Uani 1 1 d . . . F8 F -0.26758(17) 0.2423(3) 0.39045(18) 0.0337(5) Uani 1 1 d . . . F9 F -0.2599(2) 0.4319(3) 0.29623(18) 0.0373(6) Uani 1 1 d . . . C11 C -0.0163(3) 0.3389(5) 0.4008(2) 0.0209(7) Uani 1 1 d . . . H11 H -0.0243 0.4135 0.4458 0.025 Uiso 1 1 calc R . . C12 C 0.0846(3) 0.3025(4) 0.3959(2) 0.0186(6) Uani 1 1 d . . . C13 C 0.1659(3) 0.3930(5) 0.4651(3) 0.0257(8) Uani 1 1 d . . . F10 F 0.2191(2) 0.2906(3) 0.52568(17) 0.0386(6) Uani 1 1 d . . . F11 F 0.12452(18) 0.5047(3) 0.50979(18) 0.0370(6) Uani 1 1 d . . . F12 F 0.23336(18) 0.4733(3) 0.42908(18) 0.0337(5) Uani 1 1 d . . . N2 N 0.1114(2) 0.2028(4) 0.33705(19) 0.0168(5) Uani 1 1 d . . . C14 C 0.2195(2) 0.1860(4) 0.3393(2) 0.0178(6) Uani 1 1 d . . . C15 C 0.2810(2) 0.0836(6) 0.4007(2) 0.0220(6) Uani 1 1 d . . . H15 H 0.2515 0.0204 0.4402 0.026 Uiso 1 1 calc R . . C16 C 0.3860(2) 0.0742(6) 0.4040(2) 0.0232(7) Uani 1 1 d . . . C20 C 0.4486(3) -0.0379(5) 0.4723(3) 0.0324(9) Uani 1 1 d . . . F13 F 0.4359(2) -0.0050(4) 0.5537(2) 0.0487(7) Uani 1 1 d . . . F14 F 0.4211(2) -0.1938(3) 0.4552(3) 0.0559(9) Uani 1 1 d . . . F15 F 0.54922(19) -0.0292(4) 0.4748(2) 0.0440(7) Uani 1 1 d . . . C17 C 0.4299(3) 0.1624(5) 0.3460(3) 0.0261(8) Uani 1 1 d . . . H17 H 0.5016 0.1550 0.3484 0.031 Uiso 1 1 calc R . . C18 C 0.3673(3) 0.2619(5) 0.2838(3) 0.0253(7) Uani 1 1 d . . . C21 C 0.4110(3) 0.3607(6) 0.2194(4) 0.0377(10) Uani 1 1 d . . . F16 F 0.3837(3) 0.5155(4) 0.2179(3) 0.0758(14) Uani 1 1 d . . . F17 F 0.5126(2) 0.3576(4) 0.2360(2) 0.0471(9) Uani 1 1 d . . . F18 F 0.3803(3) 0.2998(6) 0.1370(2) 0.0720(12) Uani 1 1 d . . . C19 C 0.2620(3) 0.2737(4) 0.2789(3) 0.0215(7) Uani 1 1 d . . . H19 H 0.2198 0.3402 0.2351 0.026 Uiso 1 1 calc R . . C22 C 0.0363(4) -0.1747(4) 0.2256(3) 0.0278(8) Uani 1 1 d . . . C23 C 0.1181(3) -0.1004(5) 0.1939(3) 0.0281(8) Uani 1 1 d . . . C24 C 0.0730(3) -0.0058(5) 0.1188(3) 0.0237(7) Uani 1 1 d . . . C25 C -0.0374(3) -0.0300(5) 0.1009(3) 0.0237(7) Uani 1 1 d . . . C26 C -0.0578(3) -0.1409(4) 0.1649(3) 0.0245(8) Uani 1 1 d . . . C27 C 0.0482(6) -0.2839(6) 0.3049(4) 0.0516(14) Uani 1 1 d . . . H27A H -0.0072 -0.2615 0.3356 0.077 Uiso 1 1 calc R . . H27B H 0.1149 -0.2628 0.3451 0.077 Uiso 1 1 calc R . . H27C H 0.0448 -0.3987 0.2860 0.077 Uiso 1 1 calc R . . C28 C 0.2301(4) -0.1385(7) 0.2253(4) 0.0509(14) Uani 1 1 d . . . H28A H 0.2463 -0.2396 0.1971 0.076 Uiso 1 1 calc R . . H28B H 0.2462 -0.1529 0.2896 0.076 Uiso 1 1 calc R . . H28C H 0.2710 -0.0480 0.2097 0.076 Uiso 1 1 calc R . . C29 C 0.1298(4) 0.0833(8) 0.0608(3) 0.0403(9) Uani 1 1 d . . . H29A H 0.1946 0.1258 0.0965 0.060 Uiso 1 1 calc R . . H29B H 0.0877 0.1747 0.0318 0.060 Uiso 1 1 calc R . . H29C H 0.1444 0.0083 0.0158 0.060 Uiso 1 1 calc R . . C30 C -0.1100(4) 0.0351(6) 0.0214(3) 0.0371(10) Uani 1 1 d . . . H30A H -0.1806 0.0057 0.0240 0.056 Uiso 1 1 calc R . . H30B H -0.0936 -0.0122 -0.0319 0.056 Uiso 1 1 calc R . . H30C H -0.1037 0.1546 0.0198 0.056 Uiso 1 1 calc R . . C31 C -0.1576(4) -0.2301(6) 0.1611(4) 0.0442(12) Uani 1 1 d . . . H31A H -0.2143 -0.1681 0.1245 0.066 Uiso 1 1 calc R . . H31B H -0.1694 -0.2412 0.2211 0.066 Uiso 1 1 calc R . . H31C H -0.1541 -0.3392 0.1355 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01425(10) 0.01801(11) 0.01602(11) -0.00277(10) 0.00475(7) -0.00079(10) Cl1 0.0240(4) 0.0215(4) 0.0202(4) 0.0008(3) 0.0065(3) 0.0000(3) N1 0.0088(11) 0.0210(13) 0.0147(13) -0.0016(10) 0.0027(10) 0.0015(10) C1 0.0145(14) 0.0229(18) 0.0140(15) -0.0017(11) 0.0010(12) 0.0016(11) C2 0.0166(15) 0.0240(16) 0.0161(16) -0.0009(13) 0.0026(13) -0.0014(13) C3 0.0196(16) 0.0257(16) 0.0211(18) -0.0028(14) 0.0021(13) -0.0009(13) C7 0.0216(18) 0.0328(19) 0.0265(19) 0.0016(16) 0.0003(15) -0.0069(15) F1 0.0606(19) 0.090(2) 0.0291(14) 0.0133(15) 0.0020(13) -0.0499(19) F2 0.0413(14) 0.0248(12) 0.0652(19) 0.0025(12) 0.0182(13) -0.0032(10) F3 0.0179(13) 0.0409(15) 0.068(2) -0.0010(14) 0.0092(12) -0.0057(11) C4 0.0192(15) 0.030(2) 0.0215(17) -0.0017(13) -0.0040(13) 0.0003(12) C5 0.0253(18) 0.0258(18) 0.0227(19) 0.0002(15) -0.0006(15) 0.0034(15) C8 0.028(2) 0.045(2) 0.029(2) 0.0083(18) -0.0041(17) -0.0002(18) F4 0.0441(18) 0.110(3) 0.069(3) 0.055(2) -0.0298(18) -0.021(2) F5 0.175(6) 0.051(2) 0.087(3) 0.039(2) -0.082(4) -0.031(3) F6 0.149(5) 0.247(8) 0.037(2) 0.066(3) 0.036(3) 0.132(6) C6 0.0198(16) 0.0238(15) 0.0182(16) 0.0005(13) 0.0041(13) -0.0005(13) C9 0.0186(16) 0.0226(16) 0.0168(16) -0.0005(13) 0.0055(13) 0.0010(13) C10 0.0200(16) 0.0287(18) 0.0227(18) -0.0055(14) 0.0049(14) 0.0030(14) F7 0.0258(11) 0.0533(16) 0.0467(16) -0.0330(14) 0.0116(11) -0.0009(11) F8 0.0228(10) 0.0379(13) 0.0446(15) -0.0035(11) 0.0166(10) 0.0002(9) F9 0.0353(13) 0.0393(13) 0.0372(14) 0.0022(11) 0.0082(11) 0.0191(11) C11 0.0180(15) 0.0260(17) 0.0193(17) -0.0070(14) 0.0050(13) 0.0023(13) C12 0.0164(15) 0.0213(15) 0.0176(16) -0.0021(12) 0.0024(12) -0.0018(12) C13 0.0199(16) 0.0315(18) 0.0230(18) -0.0083(15) -0.0010(14) -0.0001(14) F10 0.0415(14) 0.0410(13) 0.0246(13) -0.0034(10) -0.0112(11) 0.0036(11) F11 0.0252(11) 0.0458(14) 0.0375(14) -0.0259(12) 0.0016(10) -0.0017(10) F12 0.0220(10) 0.0359(12) 0.0414(14) -0.0123(11) 0.0034(10) -0.0119(9) N2 0.0140(12) 0.0193(12) 0.0164(13) 0.0003(11) 0.0022(10) -0.0010(10) C14 0.0120(14) 0.0197(15) 0.0211(17) -0.0013(13) 0.0023(12) -0.0012(12) C15 0.0189(13) 0.0223(13) 0.0239(15) -0.0019(19) 0.0024(11) 0.0018(18) C16 0.0181(13) 0.0216(17) 0.0265(16) -0.0030(17) -0.0022(12) 0.0016(16) C20 0.0220(18) 0.0317(19) 0.039(2) 0.0013(18) -0.0028(16) 0.0043(16) F13 0.0445(15) 0.0655(19) 0.0323(15) 0.0118(13) 0.0005(12) 0.0192(14) F14 0.0478(16) 0.0263(13) 0.077(2) 0.0084(14) -0.0210(16) 0.0026(11) F15 0.0193(11) 0.0525(16) 0.0546(18) 0.0046(14) -0.0039(11) 0.0104(11) C17 0.0150(15) 0.0262(17) 0.037(2) -0.0046(16) 0.0059(15) 0.0004(13) C18 0.0215(17) 0.0261(17) 0.030(2) 0.0000(15) 0.0104(15) -0.0020(14) C21 0.027(2) 0.038(2) 0.053(3) 0.013(2) 0.017(2) -0.0009(17) F16 0.069(2) 0.0405(15) 0.142(4) 0.040(2) 0.075(3) 0.0214(16) F17 0.0265(16) 0.0445(18) 0.078(3) 0.0086(14) 0.0274(17) -0.0069(11) F18 0.065(2) 0.113(3) 0.0419(19) 0.016(2) 0.0197(16) -0.036(2) C19 0.0160(15) 0.0220(15) 0.0275(19) 0.0013(14) 0.0073(14) 0.0017(13) C22 0.050(2) 0.0062(13) 0.0251(19) -0.0048(12) 0.0044(17) 0.0055(15) C23 0.0270(18) 0.0228(17) 0.032(2) -0.0136(15) 0.0011(16) 0.0070(14) C24 0.0264(17) 0.0263(18) 0.0232(18) -0.0084(14) 0.0159(14) -0.0009(14) C25 0.0237(17) 0.0264(17) 0.0216(18) -0.0097(14) 0.0065(14) 0.0035(14) C26 0.0263(18) 0.0201(16) 0.031(2) -0.0144(14) 0.0146(15) -0.0100(14) C27 0.094(4) 0.026(2) 0.034(3) 0.0040(19) 0.013(3) 0.002(2) C28 0.030(2) 0.052(3) 0.063(4) -0.029(3) -0.005(2) 0.017(2) C29 0.054(2) 0.0351(18) 0.041(2) -0.012(3) 0.0301(19) -0.010(3) C30 0.046(2) 0.038(2) 0.025(2) -0.0102(16) 0.0014(18) 0.0132(17) C31 0.046(3) 0.036(2) 0.058(3) -0.025(2) 0.028(2) -0.019(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N2 2.070(3) . ? Ru1 N1 2.071(3) . ? Ru1 C22 2.182(3) . ? Ru1 C25 2.233(4) . ? Ru1 C26 2.246(3) . ? Ru1 C24 2.252(3) . ? Ru1 C23 2.273(4) . ? Ru1 Cl1 2.4302(8) . ? N1 C9 1.323(5) . ? N1 C1 1.442(4) . ? C1 C2 1.376(5) . ? C1 C6 1.393(5) . ? C2 C3 1.397(5) . ? C2 H2 0.9500 . ? C3 C4 1.391(6) . ? C3 C7 1.503(5) . ? C7 F1 1.323(5) . ? C7 F2 1.331(5) . ? C7 F3 1.331(5) . ? C4 C5 1.387(6) . ? C4 H4 0.9500 . ? C5 C6 1.392(5) . ? C5 C8 1.497(6) . ? C8 F6 1.274(7) . ? C8 F4 1.296(6) . ? C8 F5 1.301(7) . ? C6 H6 0.9500 . ? C9 C11 1.389(5) . ? C9 C10 1.535(5) . ? C10 F8 1.331(5) . ? C10 F9 1.333(5) . ? C10 F7 1.340(4) . ? C11 C12 1.397(5) . ? C11 H11 0.9500 . ? C12 N2 1.328(5) . ? C12 C13 1.535(5) . ? C13 F12 1.331(5) . ? C13 F11 1.335(5) . ? C13 F10 1.337(5) . ? N2 C14 1.439(4) . ? C14 C15 1.390(5) . ? C14 C19 1.394(5) . ? C15 C16 1.391(4) . ? C15 H15 0.9500 . ? C16 C17 1.379(6) . ? C16 C20 1.505(6) . ? C20 F14 1.334(5) . ? C20 F15 1.335(5) . ? C20 F13 1.336(6) . ? C17 C18 1.388(6) . ? C17 H17 0.9500 . ? C18 C19 1.391(5) . ? C18 C21 1.498(6) . ? C21 F16 1.313(6) . ? C21 F17 1.322(5) . ? C21 F18 1.347(7) . ? C19 H19 0.9500 . ? C22 C26 1.417(6) . ? C22 C23 1.426(6) . ? C22 C27 1.499(6) . ? C23 C24 1.415(6) . ? C23 C28 1.496(6) . ? C24 C25 1.448(5) . ? C24 C29 1.487(6) . ? C25 C26 1.414(6) . ? C25 C30 1.485(6) . ? C26 C31 1.506(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N1 89.66(11) . . ? N2 Ru1 C22 113.93(14) . . ? N1 Ru1 C22 119.02(15) . . ? N2 Ru1 C25 156.23(12) . . ? N1 Ru1 C25 112.90(12) . . ? C22 Ru1 C25 62.56(14) . . ? N2 Ru1 C26 150.24(14) . . ? N1 Ru1 C26 99.88(12) . . ? C22 Ru1 C26 37.30(16) . . ? C25 Ru1 C26 36.80(15) . . ? N2 Ru1 C24 118.73(13) . . ? N1 Ru1 C24 149.39(13) . . ? C22 Ru1 C24 62.11(15) . . ? C25 Ru1 C24 37.68(13) . . ? C26 Ru1 C24 61.65(13) . . ? N2 Ru1 C23 100.34(13) . . ? N1 Ru1 C23 156.26(14) . . ? C22 Ru1 C23 37.26(17) . . ? C25 Ru1 C23 61.94(14) . . ? C26 Ru1 C23 61.46(14) . . ? C24 Ru1 C23 36.44(15) . . ? N2 Ru1 Cl1 85.68(8) . . ? N1 Ru1 Cl1 85.03(8) . . ? C22 Ru1 Cl1 147.49(11) . . ? C25 Ru1 Cl1 88.83(11) . . ? C26 Ru1 Cl1 122.98(11) . . ? C24 Ru1 Cl1 85.95(10) . . ? C23 Ru1 Cl1 116.94(12) . . ? C9 N1 C1 118.3(3) . . ? C9 N1 Ru1 125.6(2) . . ? C1 N1 Ru1 115.4(2) . . ? C2 C1 C6 121.0(3) . . ? C2 C1 N1 120.8(3) . . ? C6 C1 N1 118.2(3) . . ? C1 C2 C3 119.4(3) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 120.7(3) . . ? C4 C3 C7 119.3(3) . . ? C2 C3 C7 119.8(3) . . ? F1 C7 F2 107.2(4) . . ? F1 C7 F3 107.8(4) . . ? F2 C7 F3 106.6(3) . . ? F1 C7 C3 112.3(3) . . ? F2 C7 C3 110.9(3) . . ? F3 C7 C3 111.8(3) . . ? C5 C4 C3 118.8(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.3(4) . . ? C4 C5 C8 120.2(4) . . ? C6 C5 C8 118.4(4) . . ? F6 C8 F4 107.3(6) . . ? F6 C8 F5 103.3(6) . . ? F4 C8 F5 106.3(5) . . ? F6 C8 C5 112.8(4) . . ? F4 C8 C5 113.6(4) . . ? F5 C8 C5 112.8(4) . . ? C5 C6 C1 118.8(3) . . ? C5 C6 H6 120.6 . . ? C1 C6 H6 120.6 . . ? N1 C9 C11 125.5(3) . . ? N1 C9 C10 120.0(3) . . ? C11 C9 C10 114.4(3) . . ? F8 C10 F9 107.3(3) . . ? F8 C10 F7 105.7(3) . . ? F9 C10 F7 106.4(3) . . ? F8 C10 C9 113.6(3) . . ? F9 C10 C9 111.8(3) . . ? F7 C10 C9 111.6(3) . . ? C9 C11 C12 127.5(3) . . ? C9 C11 H11 116.2 . . ? C12 C11 H11 116.2 . . ? N2 C12 C11 125.2(3) . . ? N2 C12 C13 121.3(3) . . ? C11 C12 C13 113.5(3) . . ? F12 C13 F11 106.1(3) . . ? F12 C13 F10 107.5(3) . . ? F11 C13 F10 106.1(3) . . ? F12 C13 C12 112.3(3) . . ? F11 C13 C12 112.5(3) . . ? F10 C13 C12 111.9(3) . . ? C12 N2 C14 117.5(3) . . ? C12 N2 Ru1 125.7(2) . . ? C14 N2 Ru1 116.4(2) . . ? C15 C14 C19 120.2(3) . . ? C15 C14 N2 120.6(3) . . ? C19 C14 N2 119.2(3) . . ? C14 C15 C16 119.6(4) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 121.1(4) . . ? C17 C16 C20 121.8(3) . . ? C15 C16 C20 117.1(4) . . ? F14 C20 F15 106.6(3) . . ? F14 C20 F13 107.0(4) . . ? F15 C20 F13 107.4(4) . . ? F14 C20 C16 110.8(4) . . ? F15 C20 C16 112.6(4) . . ? F13 C20 C16 112.1(3) . . ? C16 C17 C18 118.8(3) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C17 C18 C19 121.5(4) . . ? C17 C18 C21 121.0(4) . . ? C19 C18 C21 117.5(4) . . ? F16 C21 F17 106.8(4) . . ? F16 C21 F18 108.2(5) . . ? F17 C21 F18 105.1(4) . . ? F16 C21 C18 112.5(4) . . ? F17 C21 C18 113.1(4) . . ? F18 C21 C18 110.7(4) . . ? C18 C19 C14 118.8(3) . . ? C18 C19 H19 120.6 . . ? C14 C19 H19 120.6 . . ? C26 C22 C23 108.7(3) . . ? C26 C22 C27 125.3(5) . . ? C23 C22 C27 125.8(4) . . ? C26 C22 Ru1 73.8(2) . . ? C23 C22 Ru1 74.9(2) . . ? C27 C22 Ru1 122.0(3) . . ? C24 C23 C22 107.3(3) . . ? C24 C23 C28 126.3(5) . . ? C22 C23 C28 125.7(5) . . ? C24 C23 Ru1 71.0(2) . . ? C22 C23 Ru1 67.9(2) . . ? C28 C23 Ru1 133.9(3) . . ? C23 C24 C25 108.2(3) . . ? C23 C24 C29 125.8(4) . . ? C25 C24 C29 125.5(4) . . ? C23 C24 Ru1 72.6(2) . . ? C25 C24 Ru1 70.44(19) . . ? C29 C24 Ru1 129.3(3) . . ? C26 C25 C24 107.3(3) . . ? C26 C25 C30 128.3(4) . . ? C24 C25 C30 123.9(4) . . ? C26 C25 Ru1 72.1(2) . . ? C24 C25 Ru1 71.9(2) . . ? C30 C25 Ru1 127.6(3) . . ? C25 C26 C22 108.1(3) . . ? C25 C26 C31 126.0(4) . . ? C22 C26 C31 125.1(4) . . ? C25 C26 Ru1 71.1(2) . . ? C22 C26 Ru1 68.88(19) . . ? C31 C26 Ru1 133.3(3) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru1 N1 C9 9.6(3) . . . . ? C22 Ru1 N1 C9 127.0(3) . . . . ? C25 Ru1 N1 C9 -162.8(3) . . . . ? C26 Ru1 N1 C9 161.2(3) . . . . ? C24 Ru1 N1 C9 -149.5(3) . . . . ? C23 Ru1 N1 C9 125.2(4) . . . . ? Cl1 Ru1 N1 C9 -76.1(3) . . . . ? N2 Ru1 N1 C1 179.3(2) . . . . ? C22 Ru1 N1 C1 -63.3(3) . . . . ? C25 Ru1 N1 C1 7.0(3) . . . . ? C26 Ru1 N1 C1 -29.0(3) . . . . ? C24 Ru1 N1 C1 20.2(4) . . . . ? C23 Ru1 N1 C1 -65.1(4) . . . . ? Cl1 Ru1 N1 C1 93.6(2) . . . . ? C9 N1 C1 C2 -83.7(4) . . . . ? Ru1 N1 C1 C2 105.8(3) . . . . ? C9 N1 C1 C6 95.5(4) . . . . ? Ru1 N1 C1 C6 -75.1(3) . . . . ? C6 C1 C2 C3 -0.1(5) . . . . ? N1 C1 C2 C3 179.1(3) . . . . ? C1 C2 C3 C4 -0.6(5) . . . . ? C1 C2 C3 C7 175.4(3) . . . . ? C4 C3 C7 F1 -156.3(4) . . . . ? C2 C3 C7 F1 27.6(6) . . . . ? C4 C3 C7 F2 83.8(4) . . . . ? C2 C3 C7 F2 -92.3(4) . . . . ? C4 C3 C7 F3 -35.0(5) . . . . ? C2 C3 C7 F3 148.9(4) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? C7 C3 C4 C5 -175.7(4) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C3 C4 C5 C8 -179.8(4) . . . . ? C4 C5 C8 F6 -107.0(6) . . . . ? C6 C5 C8 F6 72.7(7) . . . . ? C4 C5 C8 F4 15.4(7) . . . . ? C6 C5 C8 F4 -164.8(5) . . . . ? C4 C5 C8 F5 136.4(6) . . . . ? C6 C5 C8 F5 -43.9(7) . . . . ? C4 C5 C6 C1 -1.1(6) . . . . ? C8 C5 C6 C1 179.2(4) . . . . ? C2 C1 C6 C5 0.9(5) . . . . ? N1 C1 C6 C5 -178.3(3) . . . . ? C1 N1 C9 C11 -177.9(3) . . . . ? Ru1 N1 C9 C11 -8.4(5) . . . . ? C1 N1 C9 C10 -0.6(5) . . . . ? Ru1 N1 C9 C10 168.9(2) . . . . ? N1 C9 C10 F8 62.5(5) . . . . ? C11 C9 C10 F8 -119.9(4) . . . . ? N1 C9 C10 F9 -59.1(4) . . . . ? C11 C9 C10 F9 118.4(4) . . . . ? N1 C9 C10 F7 -178.1(3) . . . . ? C11 C9 C10 F7 -0.5(5) . . . . ? N1 C9 C11 C12 1.5(6) . . . . ? C10 C9 C11 C12 -175.9(4) . . . . ? C9 C11 C12 N2 0.8(6) . . . . ? C9 C11 C12 C13 179.5(4) . . . . ? N2 C12 C13 F12 51.3(5) . . . . ? C11 C12 C13 F12 -127.4(3) . . . . ? N2 C12 C13 F11 171.0(3) . . . . ? C11 C12 C13 F11 -7.8(5) . . . . ? N2 C12 C13 F10 -69.7(5) . . . . ? C11 C12 C13 F10 111.6(4) . . . . ? C11 C12 N2 C14 177.1(3) . . . . ? C13 C12 N2 C14 -1.5(5) . . . . ? C11 C12 N2 Ru1 4.2(5) . . . . ? C13 C12 N2 Ru1 -174.3(3) . . . . ? N1 Ru1 N2 C12 -7.6(3) . . . . ? C22 Ru1 N2 C12 -129.5(3) . . . . ? C25 Ru1 N2 C12 154.6(3) . . . . ? C26 Ru1 N2 C12 -117.2(3) . . . . ? C24 Ru1 N2 C12 160.4(3) . . . . ? C23 Ru1 N2 C12 -165.9(3) . . . . ? Cl1 Ru1 N2 C12 77.4(3) . . . . ? N1 Ru1 N2 C14 179.5(2) . . . . ? C22 Ru1 N2 C14 57.6(3) . . . . ? C25 Ru1 N2 C14 -18.3(5) . . . . ? C26 Ru1 N2 C14 69.9(3) . . . . ? C24 Ru1 N2 C14 -12.5(3) . . . . ? C23 Ru1 N2 C14 21.2(3) . . . . ? Cl1 Ru1 N2 C14 -95.5(2) . . . . ? C12 N2 C14 C15 80.2(4) . . . . ? Ru1 N2 C14 C15 -106.3(3) . . . . ? C12 N2 C14 C19 -99.9(4) . . . . ? Ru1 N2 C14 C19 73.6(4) . . . . ? C19 C14 C15 C16 2.6(6) . . . . ? N2 C14 C15 C16 -177.4(3) . . . . ? C14 C15 C16 C17 -1.4(6) . . . . ? C14 C15 C16 C20 179.6(4) . . . . ? C17 C16 C20 F14 -113.5(5) . . . . ? C15 C16 C20 F14 65.5(5) . . . . ? C17 C16 C20 F15 5.7(6) . . . . ? C15 C16 C20 F15 -175.3(4) . . . . ? C17 C16 C20 F13 127.0(4) . . . . ? C15 C16 C20 F13 -54.0(5) . . . . ? C15 C16 C17 C18 0.2(6) . . . . ? C20 C16 C17 C18 179.2(4) . . . . ? C16 C17 C18 C19 -0.3(6) . . . . ? C16 C17 C18 C21 179.8(4) . . . . ? C17 C18 C21 F16 -129.1(5) . . . . ? C19 C18 C21 F16 50.9(6) . . . . ? C17 C18 C21 F17 -8.0(6) . . . . ? C19 C18 C21 F17 172.1(4) . . . . ? C17 C18 C21 F18 109.7(5) . . . . ? C19 C18 C21 F18 -70.3(5) . . . . ? C17 C18 C19 C14 1.5(6) . . . . ? C21 C18 C19 C14 -178.6(4) . . . . ? C15 C14 C19 C18 -2.7(6) . . . . ? N2 C14 C19 C18 177.4(3) . . . . ? N2 Ru1 C22 C26 170.0(2) . . . . ? N1 Ru1 C22 C26 66.1(3) . . . . ? C25 Ru1 C22 C26 -36.2(2) . . . . ? C24 Ru1 C22 C26 -78.9(2) . . . . ? C23 Ru1 C22 C26 -115.1(3) . . . . ? Cl1 Ru1 C22 C26 -67.2(3) . . . . ? N2 Ru1 C22 C23 -75.0(2) . . . . ? N1 Ru1 C22 C23 -178.8(2) . . . . ? C25 Ru1 C22 C23 78.9(2) . . . . ? C26 Ru1 C22 C23 115.1(3) . . . . ? C24 Ru1 C22 C23 36.1(2) . . . . ? Cl1 Ru1 C22 C23 47.9(3) . . . . ? N2 Ru1 C22 C27 48.1(5) . . . . ? N1 Ru1 C22 C27 -55.7(5) . . . . ? C25 Ru1 C22 C27 -158.0(5) . . . . ? C26 Ru1 C22 C27 -121.9(5) . . . . ? C24 Ru1 C22 C27 159.2(5) . . . . ? C23 Ru1 C22 C27 123.1(5) . . . . ? Cl1 Ru1 C22 C27 171.0(3) . . . . ? C26 C22 C23 C24 6.4(4) . . . . ? C27 C22 C23 C24 -179.1(4) . . . . ? Ru1 C22 C23 C24 -60.3(2) . . . . ? C26 C22 C23 C28 -164.3(4) . . . . ? C27 C22 C23 C28 10.2(6) . . . . ? Ru1 C22 C23 C28 129.0(4) . . . . ? C26 C22 C23 Ru1 66.7(2) . . . . ? C27 C22 C23 Ru1 -118.8(4) . . . . ? N2 Ru1 C23 C24 -125.1(2) . . . . ? N1 Ru1 C23 C24 121.3(3) . . . . ? C22 Ru1 C23 C24 118.7(3) . . . . ? C25 Ru1 C23 C24 38.0(2) . . . . ? C26 Ru1 C23 C24 80.0(2) . . . . ? Cl1 Ru1 C23 C24 -34.7(2) . . . . ? N2 Ru1 C23 C22 116.2(2) . . . . ? N1 Ru1 C23 C22 2.6(4) . . . . ? C25 Ru1 C23 C22 -80.7(2) . . . . ? C26 Ru1 C23 C22 -38.7(2) . . . . ? C24 Ru1 C23 C22 -118.7(3) . . . . ? Cl1 Ru1 C23 C22 -153.4(2) . . . . ? N2 Ru1 C23 C28 -2.7(6) . . . . ? N1 Ru1 C23 C28 -116.2(5) . . . . ? C22 Ru1 C23 C28 -118.9(6) . . . . ? C25 Ru1 C23 C28 160.5(6) . . . . ? C26 Ru1 C23 C28 -157.5(6) . . . . ? C24 Ru1 C23 C28 122.5(6) . . . . ? Cl1 Ru1 C23 C28 87.7(6) . . . . ? C22 C23 C24 C25 -3.5(4) . . . . ? C28 C23 C24 C25 167.2(4) . . . . ? Ru1 C23 C24 C25 -61.8(2) . . . . ? C22 C23 C24 C29 -175.3(4) . . . . ? C28 C23 C24 C29 -4.7(6) . . . . ? Ru1 C23 C24 C29 126.3(4) . . . . ? C22 C23 C24 Ru1 58.4(2) . . . . ? C28 C23 C24 Ru1 -131.0(4) . . . . ? N2 Ru1 C24 C23 66.6(3) . . . . ? N1 Ru1 C24 C23 -137.5(3) . . . . ? C22 Ru1 C24 C23 -36.9(2) . . . . ? C25 Ru1 C24 C23 -117.3(3) . . . . ? C26 Ru1 C24 C23 -79.5(3) . . . . ? Cl1 Ru1 C24 C23 149.4(2) . . . . ? N2 Ru1 C24 C25 -176.2(2) . . . . ? N1 Ru1 C24 C25 -20.2(4) . . . . ? C22 Ru1 C24 C25 80.3(2) . . . . ? C26 Ru1 C24 C25 37.8(2) . . . . ? C23 Ru1 C24 C25 117.3(3) . . . . ? Cl1 Ru1 C24 C25 -93.3(2) . . . . ? N2 Ru1 C24 C29 -55.8(4) . . . . ? N1 Ru1 C24 C29 100.2(4) . . . . ? C22 Ru1 C24 C29 -159.3(5) . . . . ? C25 Ru1 C24 C29 120.4(5) . . . . ? C26 Ru1 C24 C29 158.2(5) . . . . ? C23 Ru1 C24 C29 -122.3(5) . . . . ? Cl1 Ru1 C24 C29 27.1(4) . . . . ? C23 C24 C25 C26 -0.7(4) . . . . ? C29 C24 C25 C26 171.2(4) . . . . ? Ru1 C24 C25 C26 -63.9(2) . . . . ? C23 C24 C25 C30 -173.1(3) . . . . ? C29 C24 C25 C30 -1.3(6) . . . . ? Ru1 C24 C25 C30 123.6(4) . . . . ? C23 C24 C25 Ru1 63.2(2) . . . . ? C29 C24 C25 Ru1 -124.9(4) . . . . ? N2 Ru1 C25 C26 124.1(3) . . . . ? N1 Ru1 C25 C26 -75.3(2) . . . . ? C22 Ru1 C25 C26 36.7(2) . . . . ? C24 Ru1 C25 C26 115.7(3) . . . . ? C23 Ru1 C25 C26 79.0(2) . . . . ? Cl1 Ru1 C25 C26 -159.4(2) . . . . ? N2 Ru1 C25 C24 8.4(4) . . . . ? N1 Ru1 C25 C24 169.0(2) . . . . ? C22 Ru1 C25 C24 -79.1(2) . . . . ? C26 Ru1 C25 C24 -115.7(3) . . . . ? C23 Ru1 C25 C24 -36.7(2) . . . . ? Cl1 Ru1 C25 C24 84.9(2) . . . . ? N2 Ru1 C25 C30 -110.9(4) . . . . ? N1 Ru1 C25 C30 49.7(4) . . . . ? C22 Ru1 C25 C30 161.7(4) . . . . ? C26 Ru1 C25 C30 125.0(5) . . . . ? C24 Ru1 C25 C30 -119.3(5) . . . . ? C23 Ru1 C25 C30 -156.0(4) . . . . ? Cl1 Ru1 C25 C30 -34.4(4) . . . . ? C24 C25 C26 C22 4.6(4) . . . . ? C30 C25 C26 C22 176.6(3) . . . . ? Ru1 C25 C26 C22 -59.1(2) . . . . ? C24 C25 C26 C31 -165.9(4) . . . . ? C30 C25 C26 C31 6.1(6) . . . . ? Ru1 C25 C26 C31 130.4(4) . . . . ? C24 C25 C26 Ru1 63.7(2) . . . . ? C30 C25 C26 Ru1 -124.2(4) . . . . ? C23 C22 C26 C25 -6.8(4) . . . . ? C27 C22 C26 C25 178.6(4) . . . . ? Ru1 C22 C26 C25 60.5(3) . . . . ? C23 C22 C26 C31 163.8(4) . . . . ? C27 C22 C26 C31 -10.8(6) . . . . ? Ru1 C22 C26 C31 -128.9(4) . . . . ? C23 C22 C26 Ru1 -67.4(2) . . . . ? C27 C22 C26 Ru1 118.1(4) . . . . ? N2 Ru1 C26 C25 -137.7(3) . . . . ? N1 Ru1 C26 C25 115.3(2) . . . . ? C22 Ru1 C26 C25 -119.0(3) . . . . ? C24 Ru1 C26 C25 -38.7(2) . . . . ? C23 Ru1 C26 C25 -80.4(2) . . . . ? Cl1 Ru1 C26 C25 24.8(3) . . . . ? N2 Ru1 C26 C22 -18.7(4) . . . . ? N1 Ru1 C26 C22 -125.7(2) . . . . ? C25 Ru1 C26 C22 119.0(3) . . . . ? C24 Ru1 C26 C22 80.3(3) . . . . ? C23 Ru1 C26 C22 38.6(2) . . . . ? Cl1 Ru1 C26 C22 143.8(2) . . . . ? N2 Ru1 C26 C31 100.2(5) . . . . ? N1 Ru1 C26 C31 -6.8(5) . . . . ? C22 Ru1 C26 C31 118.9(6) . . . . ? C25 Ru1 C26 C31 -122.1(6) . . . . ? C24 Ru1 C26 C31 -160.8(5) . . . . ? C23 Ru1 C26 C31 157.5(5) . . . . ? Cl1 Ru1 C26 C31 -97.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 77.06 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.268 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.079 data_adp211 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*Ru((2,6-Me2C6H3NCMe)2CH)' _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 N2 Ru' _chemical_formula_sum 'C31 H40 N2 Ru' _chemical_formula_weight 541.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1867(12) _cell_length_b 15.6006(17) _cell_length_c 17.0345(13) _cell_angle_alpha 96.753(6) _cell_angle_beta 103.186(8) _cell_angle_gamma 104.813(8) _cell_volume 2749.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 117 _cell_measurement_theta_min 5.882 _cell_measurement_theta_max 20.569 _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.459 _exptl_crystal_size_mid 0.208 _exptl_crystal_size_min 0.142 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.773122 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; Bruker Nonius Area Detector Scaling and Absorption Correction SADABS 2.10 (Bruker, 2003) based on an algorithm described by R.H. Blessing, Acta Cryst. (1995), a51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonus KappaCCD with \k-goniostat' _diffrn_detector 'Bruker Apex II CCD' _diffrn_measurement_method '\f & \w scans' _diffrn_source 'Enraf Nonius FR590' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51833 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9641 _reflns_number_gt 7450 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'Collect (Hooft, R.W.W., 1998. Nonius B.V., 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg A.J.M., Nonius B.V., 1989-2000)' _computing_data_reduction 'EvalCCD (Hooft R.W.W., Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick G.M., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick G.M., 2008)' _computing_molecular_graphics 'ORTEP-3 for windows 2.02 (Farrugia, 2008)' _computing_publication_material 'WinGX 1.80.05 (Farrugia, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+3.6403P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9641 _refine_ls_number_parameters 635 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4525(3) 0.7615(2) 0.07741(18) 0.0156(7) Uani 1 1 d . . . C2 C 0.3668(3) 0.7889(2) 0.11650(19) 0.0215(7) Uani 1 1 d . . . C3 C 0.2918(3) 0.8389(2) 0.0763(2) 0.0320(9) Uani 1 1 d . . . H3 H 0.2314 0.8568 0.1007 0.038 Uiso 1 1 calc R . . C4 C 0.3039(3) 0.8626(2) 0.0021(2) 0.0364(10) Uani 1 1 d . . . H4 H 0.2542 0.8980 -0.0230 0.044 Uiso 1 1 calc R . . C5 C 0.3884(3) 0.8346(2) -0.0354(2) 0.0321(9) Uani 1 1 d . . . H5 H 0.3967 0.8516 -0.0861 0.039 Uiso 1 1 calc R . . C6 C 0.4618(3) 0.7817(2) 0.00029(18) 0.0200(7) Uani 1 1 d . . . C7 C 0.3564(3) 0.7648(3) 0.1985(2) 0.0338(9) Uani 1 1 d . . . H7A H 0.3244 0.6991 0.1925 0.051 Uiso 1 1 calc R . . H7B H 0.2968 0.7927 0.2181 0.051 Uiso 1 1 calc R . . H7C H 0.4412 0.7870 0.2382 0.051 Uiso 1 1 calc R . . C8 C 0.5451(3) 0.7436(2) -0.04406(19) 0.0288(8) Uani 1 1 d . . . H8A H 0.5013 0.6799 -0.0683 0.043 Uiso 1 1 calc R . . H8B H 0.6272 0.7489 -0.0051 0.043 Uiso 1 1 calc R . . H8C H 0.5608 0.7773 -0.0876 0.043 Uiso 1 1 calc R . . C9 C 0.4705(3) 0.6181(2) 0.09664(18) 0.0183(7) Uani 1 1 d . . . C10 C 0.3368(3) 0.5808(2) 0.0372(2) 0.0266(8) Uani 1 1 d . . . H10A H 0.2765 0.6060 0.0590 0.040 Uiso 1 1 calc R . . H10B H 0.3088 0.5149 0.0308 0.040 Uiso 1 1 calc R . . H10C H 0.3391 0.5976 -0.0162 0.040 Uiso 1 1 calc R . . C11 C 0.5260(3) 0.5551(2) 0.12907(19) 0.0199(7) Uani 1 1 d . . . H11 H 0.4752 0.4938 0.1122 0.024 Uiso 1 1 calc R . . C12 C 0.6469(3) 0.5707(2) 0.18315(18) 0.0160(7) Uani 1 1 d . . . C13 C 0.6809(3) 0.4882(2) 0.20952(19) 0.0218(7) Uani 1 1 d . . . H13A H 0.7553 0.4814 0.1911 0.033 Uiso 1 1 calc R . . H13B H 0.6077 0.4343 0.1850 0.033 Uiso 1 1 calc R . . H13C H 0.7015 0.4956 0.2695 0.033 Uiso 1 1 calc R . . C14 C 0.8531(3) 0.6536(2) 0.26411(17) 0.0133(6) Uani 1 1 d . . . C15 C 0.9513(3) 0.6429(2) 0.22935(18) 0.0181(7) Uani 1 1 d . . . C16 C 1.0670(3) 0.6414(2) 0.2819(2) 0.0245(8) Uani 1 1 d . . . H16 H 1.1361 0.6363 0.2598 0.029 Uiso 1 1 calc R . . C17 C 1.0820(3) 0.6474(2) 0.3659(2) 0.0279(8) Uani 1 1 d . . . H17 H 1.1608 0.6458 0.4006 0.033 Uiso 1 1 calc R . . C18 C 0.9826(3) 0.6555(2) 0.39886(19) 0.0236(8) Uani 1 1 d . . . H18 H 0.9935 0.6588 0.4562 0.028 Uiso 1 1 calc R . . C19 C 0.8662(3) 0.6590(2) 0.34930(18) 0.0172(7) Uani 1 1 d . . . C20 C 0.9319(3) 0.6288(2) 0.13701(19) 0.0251(8) Uani 1 1 d . . . H20A H 0.8888 0.5649 0.1130 0.038 Uiso 1 1 calc R . . H20B H 1.0154 0.6468 0.1250 0.038 Uiso 1 1 calc R . . H20C H 0.8789 0.6655 0.1134 0.038 Uiso 1 1 calc R . . C21 C 0.7576(3) 0.6680(2) 0.38439(19) 0.0234(8) Uani 1 1 d . . . H21A H 0.7838 0.6721 0.4440 0.035 Uiso 1 1 calc R . . H21B H 0.6828 0.6152 0.3600 0.035 Uiso 1 1 calc R . . H21C H 0.7354 0.7227 0.3720 0.035 Uiso 1 1 calc R . . C22 C 0.7624(3) 0.8996(2) 0.28069(17) 0.0163(6) Uani 1 1 d . . . C23 C 0.7140(3) 0.9204(2) 0.20159(18) 0.0167(7) Uani 1 1 d . . . C24 C 0.7932(3) 0.9016(2) 0.15137(17) 0.0157(6) Uani 1 1 d . . . C25 C 0.8950(3) 0.8736(2) 0.20047(18) 0.0165(7) Uani 1 1 d . . . C26 C 0.8781(3) 0.8754(2) 0.28096(17) 0.0149(6) Uani 1 1 d . . . C27 C 0.7138(3) 0.9160(2) 0.35505(18) 0.0223(7) Uani 1 1 d . . . H27A H 0.7288 0.8722 0.3901 0.034 Uiso 1 1 calc R . . H27B H 0.6216 0.9092 0.3375 0.034 Uiso 1 1 calc R . . H27C H 0.7594 0.9773 0.3859 0.034 Uiso 1 1 calc R . . C28 C 0.6104(3) 0.9661(2) 0.18055(19) 0.0205(7) Uani 1 1 d . . . H28A H 0.6475 1.0314 0.1993 0.031 Uiso 1 1 calc R . . H28B H 0.5434 0.9436 0.2077 0.031 Uiso 1 1 calc R . . H28C H 0.5729 0.9529 0.1210 0.031 Uiso 1 1 calc R . . C29 C 0.7878(3) 0.9225(2) 0.06669(18) 0.0230(7) Uani 1 1 d . . . H29A H 0.7000 0.9208 0.0392 0.035 Uiso 1 1 calc R . . H29B H 0.8140 0.8776 0.0348 0.035 Uiso 1 1 calc R . . H29C H 0.8460 0.9827 0.0710 0.035 Uiso 1 1 calc R . . C30 C 1.0100(3) 0.8601(2) 0.1748(2) 0.0241(7) Uani 1 1 d . . . H30A H 1.0762 0.9183 0.1858 0.036 Uiso 1 1 calc R . . H30B H 0.9846 0.8347 0.1160 0.036 Uiso 1 1 calc R . . H30C H 1.0442 0.8187 0.2059 0.036 Uiso 1 1 calc R . . C31 C 0.9759(3) 0.8684(2) 0.35569(18) 0.0213(7) Uani 1 1 d . . . H31A H 1.0216 0.8264 0.3395 0.032 Uiso 1 1 calc R . . H31B H 0.9321 0.8461 0.3962 0.032 Uiso 1 1 calc R . . H31C H 1.0373 0.9280 0.3797 0.032 Uiso 1 1 calc R . . C32 C 0.1354(3) 0.3490(2) 0.23931(18) 0.0160(7) Uani 1 1 d . . . C33 C 0.1167(3) 0.3371(2) 0.15367(18) 0.0200(7) Uani 1 1 d . . . C34 C -0.0035(3) 0.3356(2) 0.1046(2) 0.0299(8) Uani 1 1 d . . . H34 H -0.0191 0.3260 0.0466 0.036 Uiso 1 1 calc R . . C35 C -0.0990(3) 0.3479(2) 0.1393(2) 0.0308(9) Uani 1 1 d . . . H35 H -0.1798 0.3467 0.1053 0.037 Uiso 1 1 calc R . . C36 C -0.0773(3) 0.3620(2) 0.2241(2) 0.0270(8) Uani 1 1 d . . . H36 H -0.1432 0.3716 0.2475 0.032 Uiso 1 1 calc R . . C37 C 0.0391(3) 0.3623(2) 0.27531(19) 0.0193(7) Uani 1 1 d . . . C38 C 0.2253(3) 0.3314(3) 0.1165(2) 0.0292(8) Uani 1 1 d . . . H38A H 0.2845 0.3919 0.1240 0.044 Uiso 1 1 calc R . . H38B H 0.1906 0.3059 0.0577 0.044 Uiso 1 1 calc R . . H38C H 0.2713 0.2926 0.1435 0.044 Uiso 1 1 calc R . . C39 C 0.0609(3) 0.3776(2) 0.36780(19) 0.0264(8) Uani 1 1 d . . . H39A H 0.1157 0.4393 0.3919 0.040 Uiso 1 1 calc R . . H39B H 0.1029 0.3346 0.3904 0.040 Uiso 1 1 calc R . . H39C H -0.0218 0.3690 0.3808 0.040 Uiso 1 1 calc R . . C40 C 0.3420(3) 0.4332(2) 0.31718(18) 0.0180(7) Uani 1 1 d . . . C41 C 0.3047(3) 0.5143(2) 0.2896(2) 0.0230(7) Uani 1 1 d . . . H41A H 0.2786 0.5043 0.2296 0.034 Uiso 1 1 calc R . . H41B H 0.3783 0.5686 0.3108 0.034 Uiso 1 1 calc R . . H41C H 0.2330 0.5223 0.3109 0.034 Uiso 1 1 calc R . . C42 C 0.4654(3) 0.4509(2) 0.36961(18) 0.0195(7) Uani 1 1 d . . . H42 H 0.5140 0.5126 0.3871 0.023 Uiso 1 1 calc R . . C43 C 0.5251(3) 0.3883(2) 0.39908(18) 0.0175(7) Uani 1 1 d . . . C44 C 0.6631(3) 0.4275(2) 0.4524(2) 0.0244(8) Uani 1 1 d . . . H44A H 0.6697 0.4094 0.5060 0.037 Uiso 1 1 calc R . . H44B H 0.6875 0.4935 0.4598 0.037 Uiso 1 1 calc R . . H44C H 0.7206 0.4048 0.4256 0.037 Uiso 1 1 calc R . . C45 C 0.5510(3) 0.2461(2) 0.41354(17) 0.0149(6) Uani 1 1 d . . . C46 C 0.5604(3) 0.2279(2) 0.49333(18) 0.0170(7) Uani 1 1 d . . . C47 C 0.6442(3) 0.1786(2) 0.52313(19) 0.0226(7) Uani 1 1 d . . . H47 H 0.6519 0.1654 0.5768 0.027 Uiso 1 1 calc R . . C48 C 0.7158(3) 0.1490(2) 0.4752(2) 0.0251(8) Uani 1 1 d . . . H48 H 0.7713 0.1150 0.4958 0.030 Uiso 1 1 calc R . . C49 C 0.7065(3) 0.1690(2) 0.3969(2) 0.0229(7) Uani 1 1 d . . . H49 H 0.7566 0.1489 0.3646 0.027 Uiso 1 1 calc R . . C50 C 0.6247(3) 0.2182(2) 0.36498(18) 0.0168(7) Uani 1 1 d . . . C51 C 0.4827(3) 0.2615(2) 0.54521(18) 0.0246(8) Uani 1 1 d . . . H51A H 0.5087 0.3276 0.5557 0.037 Uiso 1 1 calc R . . H51B H 0.4976 0.2403 0.5975 0.037 Uiso 1 1 calc R . . H51C H 0.3912 0.2384 0.5161 0.037 Uiso 1 1 calc R . . C52 C 0.6188(3) 0.2442(2) 0.28166(19) 0.0245(8) Uani 1 1 d . . . H52A H 0.5290 0.2282 0.2495 0.037 Uiso 1 1 calc R . . H52B H 0.6654 0.2118 0.2529 0.037 Uiso 1 1 calc R . . H52C H 0.6581 0.3094 0.2886 0.037 Uiso 1 1 calc R . . C53 C 0.1450(3) 0.1248(2) 0.34974(17) 0.0157(6) Uani 1 1 d . . . C54 C 0.2536(3) 0.0921(2) 0.34682(18) 0.0177(7) Uani 1 1 d . . . C55 C 0.2676(3) 0.0897(2) 0.26585(19) 0.0203(7) Uani 1 1 d . . . C56 C 0.1632(3) 0.1156(2) 0.21682(18) 0.0181(7) Uani 1 1 d . . . C57 C 0.0856(3) 0.1342(2) 0.26841(18) 0.0166(7) Uani 1 1 d . . . C58 C 0.0902(3) 0.1333(2) 0.42247(19) 0.0244(7) Uani 1 1 d . . . H58A H 0.0519 0.1832 0.4217 0.037 Uiso 1 1 calc R . . H58B H 0.1589 0.1452 0.4733 0.037 Uiso 1 1 calc R . . H58C H 0.0243 0.0770 0.4196 0.037 Uiso 1 1 calc R . . C59 C 0.3258(3) 0.0523(2) 0.4120(2) 0.0268(8) Uani 1 1 d . . . H59A H 0.2833 -0.0126 0.4039 0.040 Uiso 1 1 calc R . . H59B H 0.3268 0.0817 0.4663 0.040 Uiso 1 1 calc R . . H59C H 0.4141 0.0619 0.4080 0.040 Uiso 1 1 calc R . . C60 C 0.3617(3) 0.0517(2) 0.2333(2) 0.0309(8) Uani 1 1 d . . . H60A H 0.4444 0.0697 0.2750 0.046 Uiso 1 1 calc R . . H60B H 0.3732 0.0750 0.1837 0.046 Uiso 1 1 calc R . . H60C H 0.3287 -0.0143 0.2200 0.046 Uiso 1 1 calc R . . C61 C 0.1337(3) 0.1099(2) 0.12535(18) 0.0270(8) Uani 1 1 d . . . H61A H 0.0901 0.0471 0.0978 0.041 Uiso 1 1 calc R . . H61B H 0.2139 0.1313 0.1099 0.041 Uiso 1 1 calc R . . H61C H 0.0780 0.1476 0.1087 0.041 Uiso 1 1 calc R . . C62 C -0.0454(3) 0.1476(2) 0.2412(2) 0.0226(7) Uani 1 1 d . . . H62A H -0.0511 0.1750 0.1920 0.034 Uiso 1 1 calc R . . H62B H -0.0588 0.1875 0.2852 0.034 Uiso 1 1 calc R . . H62C H -0.1113 0.0892 0.2286 0.034 Uiso 1 1 calc R . . N1 N 0.5285(2) 0.70785(17) 0.11606(14) 0.0140(6) Uani 1 1 d . . . N2 N 0.7311(2) 0.65367(17) 0.21156(14) 0.0136(5) Uani 1 1 d . . . N3 N 0.2581(2) 0.35013(17) 0.29125(14) 0.0138(6) Uani 1 1 d . . . N4 N 0.4676(2) 0.29875(17) 0.38203(14) 0.0138(5) Uani 1 1 d . . . Ru1 Ru 0.70999(2) 0.777128(16) 0.190830(13) 0.01051(7) Uani 1 1 d . . . Ru2 Ru 0.28178(2) 0.228317(16) 0.315865(13) 0.01129(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0114(15) 0.0104(17) 0.0193(15) -0.0009(13) -0.0027(12) 0.0012(13) C2 0.0108(15) 0.0176(19) 0.0302(18) -0.0033(14) 0.0025(13) 0.0001(14) C3 0.0143(17) 0.025(2) 0.051(2) -0.0072(18) -0.0016(16) 0.0099(16) C4 0.032(2) 0.022(2) 0.043(2) -0.0003(17) -0.0171(18) 0.0150(18) C5 0.037(2) 0.023(2) 0.0234(18) 0.0033(15) -0.0102(16) 0.0033(18) C6 0.0209(17) 0.0134(18) 0.0185(16) 0.0007(13) -0.0025(13) 0.0001(14) C7 0.0244(19) 0.035(2) 0.044(2) 0.0042(18) 0.0181(17) 0.0055(18) C8 0.035(2) 0.026(2) 0.0223(17) 0.0003(15) 0.0091(15) 0.0055(18) C9 0.0150(16) 0.0146(18) 0.0215(16) 0.0034(14) 0.0018(13) 0.0007(14) C10 0.0200(18) 0.0132(19) 0.0355(19) 0.0027(15) -0.0069(15) -0.0008(15) C11 0.0191(17) 0.0056(17) 0.0287(17) 0.0033(14) 0.0009(14) -0.0025(14) C12 0.0171(16) 0.0093(17) 0.0205(16) 0.0019(13) 0.0051(13) 0.0025(14) C13 0.0221(18) 0.0129(18) 0.0265(17) 0.0051(14) -0.0015(14) 0.0046(15) C14 0.0126(15) 0.0071(16) 0.0186(15) 0.0021(12) 0.0011(12) 0.0031(13) C15 0.0210(17) 0.0103(17) 0.0257(17) 0.0065(14) 0.0069(14) 0.0073(15) C16 0.0184(17) 0.0168(19) 0.043(2) 0.0097(16) 0.0110(15) 0.0092(15) C17 0.0200(18) 0.021(2) 0.038(2) 0.0081(16) -0.0055(15) 0.0076(16) C18 0.0275(19) 0.0157(18) 0.0225(17) 0.0061(14) -0.0032(14) 0.0048(15) C19 0.0215(17) 0.0092(17) 0.0199(16) 0.0054(13) 0.0029(13) 0.0037(14) C20 0.0292(19) 0.023(2) 0.0277(18) 0.0038(15) 0.0136(15) 0.0107(17) C21 0.034(2) 0.020(2) 0.0203(17) 0.0068(14) 0.0103(15) 0.0104(17) C22 0.0180(16) 0.0087(16) 0.0184(15) -0.0008(12) 0.0047(13) -0.0012(13) C23 0.0136(15) 0.0096(16) 0.0241(16) 0.0008(13) 0.0022(13) 0.0023(13) C24 0.0172(16) 0.0080(16) 0.0186(15) 0.0031(12) 0.0026(13) -0.0005(13) C25 0.0128(15) 0.0087(16) 0.0273(17) 0.0031(13) 0.0085(13) -0.0004(13) C26 0.0157(16) 0.0071(16) 0.0174(15) 0.0015(12) -0.0001(12) 0.0001(13) C27 0.0283(18) 0.0173(18) 0.0212(16) 0.0019(14) 0.0082(14) 0.0057(15) C28 0.0197(16) 0.0121(17) 0.0306(17) 0.0047(14) 0.0052(14) 0.0072(14) C29 0.0276(18) 0.0196(18) 0.0220(16) 0.0082(14) 0.0081(14) 0.0040(15) C30 0.0187(17) 0.0203(19) 0.0366(19) 0.0090(15) 0.0133(15) 0.0044(15) C31 0.0209(17) 0.0117(17) 0.0248(17) 0.0020(13) -0.0019(13) 0.0012(14) C32 0.0146(16) 0.0093(17) 0.0218(16) 0.0054(13) -0.0001(13) 0.0026(14) C33 0.0213(17) 0.0154(18) 0.0222(16) 0.0050(14) 0.0038(14) 0.0046(15) C34 0.033(2) 0.026(2) 0.0217(17) 0.0056(15) -0.0073(15) 0.0056(17) C35 0.0179(18) 0.023(2) 0.044(2) 0.0118(17) -0.0093(16) 0.0048(16) C36 0.0167(17) 0.019(2) 0.046(2) 0.0105(17) 0.0080(16) 0.0061(16) C37 0.0145(16) 0.0126(18) 0.0308(18) 0.0059(14) 0.0062(14) 0.0031(14) C38 0.036(2) 0.029(2) 0.0238(18) 0.0084(16) 0.0107(16) 0.0072(18) C39 0.031(2) 0.025(2) 0.0309(19) 0.0087(16) 0.0162(16) 0.0134(17) C40 0.0178(16) 0.0163(19) 0.0203(16) 0.0042(14) 0.0031(13) 0.0071(15) C41 0.0198(17) 0.0118(18) 0.0325(18) 0.0055(15) -0.0011(14) 0.0028(15) C42 0.0169(17) 0.0115(18) 0.0260(17) 0.0009(14) 0.0012(14) 0.0021(15) C43 0.0143(16) 0.0153(18) 0.0202(16) 0.0034(14) 0.0025(13) 0.0016(14) C44 0.0168(17) 0.0164(19) 0.0345(19) 0.0081(15) -0.0029(14) 0.0026(15) C45 0.0127(15) 0.0086(16) 0.0185(15) 0.0034(13) -0.0011(12) -0.0012(13) C46 0.0160(16) 0.0109(17) 0.0189(15) 0.0013(13) 0.0000(13) -0.0003(14) C47 0.0261(18) 0.0153(18) 0.0192(16) 0.0062(14) -0.0050(14) 0.0022(15) C48 0.0205(17) 0.0195(19) 0.0325(19) 0.0059(15) -0.0025(15) 0.0090(15) C49 0.0168(16) 0.0177(19) 0.0337(18) 0.0020(15) 0.0061(14) 0.0059(15) C50 0.0147(15) 0.0136(17) 0.0204(16) 0.0026(13) 0.0042(13) 0.0019(14) C51 0.0314(19) 0.022(2) 0.0173(16) 0.0024(14) 0.0042(14) 0.0055(16) C52 0.0224(18) 0.027(2) 0.0265(17) 0.0069(15) 0.0113(14) 0.0066(16) C53 0.0188(16) 0.0073(15) 0.0192(15) 0.0020(12) 0.0071(13) -0.0009(13) C54 0.0191(16) 0.0061(16) 0.0231(16) 0.0008(13) 0.0024(13) -0.0010(13) C55 0.0154(16) 0.0093(17) 0.0321(18) -0.0071(14) 0.0102(14) -0.0020(13) C56 0.0214(17) 0.0103(17) 0.0180(15) -0.0015(13) 0.0056(13) -0.0018(14) C57 0.0138(15) 0.0065(16) 0.0260(17) 0.0001(13) 0.0055(13) -0.0017(13) C58 0.0295(18) 0.0185(18) 0.0245(17) 0.0030(14) 0.0127(14) 0.0016(15) C59 0.0233(18) 0.0135(18) 0.040(2) 0.0090(15) 0.0017(15) 0.0032(15) C60 0.0222(18) 0.022(2) 0.045(2) -0.0070(16) 0.0117(16) 0.0047(16) C61 0.0287(19) 0.024(2) 0.0206(17) -0.0014(14) 0.0057(14) -0.0026(16) C62 0.0158(16) 0.0160(18) 0.0320(18) 0.0034(14) 0.0047(14) -0.0002(14) N1 0.0134(13) 0.0117(15) 0.0173(13) 0.0041(11) 0.0029(10) 0.0045(12) N2 0.0120(13) 0.0122(15) 0.0152(12) 0.0023(11) 0.0015(10) 0.0031(12) N3 0.0114(13) 0.0142(15) 0.0153(12) 0.0036(11) 0.0020(10) 0.0038(12) N4 0.0117(13) 0.0133(15) 0.0162(13) 0.0040(11) 0.0024(10) 0.0040(12) Ru1 0.00992(13) 0.00851(14) 0.01293(12) 0.00274(10) 0.00240(10) 0.00266(11) Ru2 0.01016(13) 0.00876(14) 0.01387(13) 0.00200(10) 0.00245(10) 0.00164(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.407(4) . ? C1 C6 1.407(4) . ? C1 N1 1.447(4) . ? C2 C3 1.407(5) . ? C2 C7 1.511(5) . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.402(4) . ? C5 H5 0.9500 . ? C6 C8 1.513(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.348(4) . ? C9 C11 1.394(4) . ? C9 C10 1.525(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.395(4) . ? C11 H11 0.9500 . ? C12 N2 1.349(4) . ? C12 C13 1.521(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.398(4) . ? C14 C19 1.415(4) . ? C14 N2 1.452(3) . ? C15 C16 1.402(4) . ? C15 C20 1.519(4) . ? C16 C17 1.392(5) . ? C16 H16 0.9500 . ? C17 C18 1.381(5) . ? C17 H17 0.9500 . ? C18 C19 1.399(4) . ? C18 H18 0.9500 . ? C19 C21 1.500(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C26 1.436(4) . ? C22 C23 1.440(4) . ? C22 C27 1.509(4) . ? C22 Ru1 2.160(3) . ? C23 C24 1.423(4) . ? C23 C28 1.507(4) . ? C23 Ru1 2.209(3) . ? C24 C25 1.446(4) . ? C24 C29 1.507(4) . ? C24 Ru1 2.181(3) . ? C25 C26 1.424(4) . ? C25 C30 1.505(4) . ? C25 Ru1 2.184(3) . ? C26 C31 1.513(4) . ? C26 Ru1 2.214(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.402(4) . ? C32 C33 1.408(4) . ? C32 N3 1.448(4) . ? C33 C34 1.405(4) . ? C33 C38 1.510(4) . ? C34 C35 1.376(5) . ? C34 H34 0.9500 . ? C35 C36 1.389(5) . ? C35 H35 0.9500 . ? C36 C37 1.391(4) . ? C36 H36 0.9500 . ? C37 C39 1.518(4) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 N3 1.346(4) . ? C40 C42 1.401(4) . ? C40 C41 1.522(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.396(4) . ? C42 H42 0.9500 . ? C43 N4 1.344(4) . ? C43 C44 1.526(4) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.401(4) . ? C45 C46 1.407(4) . ? C45 N4 1.449(4) . ? C46 C47 1.404(4) . ? C46 C51 1.512(4) . ? C47 C48 1.386(4) . ? C47 H47 0.9500 . ? C48 C49 1.393(5) . ? C48 H48 0.9500 . ? C49 C50 1.398(4) . ? C49 H49 0.9500 . ? C50 C52 1.513(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C57 1.435(4) . ? C53 C54 1.441(4) . ? C53 C58 1.509(4) . ? C53 Ru2 2.155(3) . ? C54 C55 1.420(4) . ? C54 C59 1.510(4) . ? C54 Ru2 2.211(3) . ? C55 C56 1.450(4) . ? C55 C60 1.508(4) . ? C55 Ru2 2.181(3) . ? C56 C57 1.423(4) . ? C56 C61 1.504(4) . ? C56 Ru2 2.188(3) . ? C57 C62 1.509(4) . ? C57 Ru2 2.211(3) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? N1 Ru1 2.070(2) . ? N2 Ru1 2.060(2) . ? N3 Ru2 2.062(3) . ? N4 Ru2 2.067(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 121.5(3) . . ? C2 C1 N1 119.0(3) . . ? C6 C1 N1 119.4(3) . . ? C1 C2 C3 117.6(3) . . ? C1 C2 C7 120.7(3) . . ? C3 C2 C7 121.7(3) . . ? C4 C3 C2 121.4(3) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 121.0(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 118.3(3) . . ? C5 C6 C8 121.3(3) . . ? C1 C6 C8 120.4(3) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C11 123.3(3) . . ? N1 C9 C10 120.3(3) . . ? C11 C9 C10 116.4(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C12 128.1(3) . . ? C9 C11 H11 115.9 . . ? C12 C11 H11 115.9 . . ? N2 C12 C11 123.1(3) . . ? N2 C12 C13 120.5(3) . . ? C11 C12 C13 116.4(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 121.7(3) . . ? C15 C14 N2 119.7(3) . . ? C19 C14 N2 118.5(3) . . ? C14 C15 C16 118.1(3) . . ? C14 C15 C20 121.2(3) . . ? C16 C15 C20 120.6(3) . . ? C17 C16 C15 121.0(3) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C18 C17 C16 120.1(3) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 121.2(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C14 117.9(3) . . ? C18 C19 C21 121.7(3) . . ? C14 C19 C21 120.4(3) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C26 C22 C23 108.3(2) . . ? C26 C22 C27 125.2(3) . . ? C23 C22 C27 125.7(3) . . ? C26 C22 Ru1 72.85(17) . . ? C23 C22 Ru1 72.60(17) . . ? C27 C22 Ru1 128.4(2) . . ? C24 C23 C22 107.5(2) . . ? C24 C23 C28 126.4(3) . . ? C22 C23 C28 125.6(3) . . ? C24 C23 Ru1 70.02(17) . . ? C22 C23 Ru1 68.93(17) . . ? C28 C23 Ru1 132.7(2) . . ? C23 C24 C25 108.3(2) . . ? C23 C24 C29 126.3(3) . . ? C25 C24 C29 124.7(3) . . ? C23 C24 Ru1 72.17(17) . . ? C25 C24 Ru1 70.78(17) . . ? C29 C24 Ru1 130.9(2) . . ? C26 C25 C24 108.0(2) . . ? C26 C25 C30 125.8(3) . . ? C24 C25 C30 125.4(3) . . ? C26 C25 Ru1 72.22(17) . . ? C24 C25 Ru1 70.53(17) . . ? C30 C25 Ru1 130.4(2) . . ? C25 C26 C22 107.7(2) . . ? C25 C26 C31 125.4(3) . . ? C22 C26 C31 126.2(3) . . ? C25 C26 Ru1 69.99(17) . . ? C22 C26 Ru1 68.83(16) . . ? C31 C26 Ru1 134.0(2) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 121.4(3) . . ? C37 C32 N3 119.4(3) . . ? C33 C32 N3 119.2(3) . . ? C34 C33 C32 118.1(3) . . ? C34 C33 C38 121.2(3) . . ? C32 C33 C38 120.7(3) . . ? C35 C34 C33 121.0(3) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 120.0(3) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C37 121.3(3) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C36 C37 C32 118.3(3) . . ? C36 C37 C39 120.5(3) . . ? C32 C37 C39 121.2(3) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N3 C40 C42 123.6(3) . . ? N3 C40 C41 120.0(3) . . ? C42 C40 C41 116.4(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C40 127.5(3) . . ? C43 C42 H42 116.2 . . ? C40 C42 H42 116.2 . . ? N4 C43 C42 123.4(3) . . ? N4 C43 C44 120.9(3) . . ? C42 C43 C44 115.7(3) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 121.7(3) . . ? C50 C45 N4 118.9(3) . . ? C46 C45 N4 119.3(3) . . ? C47 C46 C45 118.2(3) . . ? C47 C46 C51 121.4(3) . . ? C45 C46 C51 120.4(3) . . ? C48 C47 C46 120.8(3) . . ? C48 C47 H47 119.6 . . ? C46 C47 H47 119.6 . . ? C47 C48 C49 120.1(3) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C48 C49 C50 121.0(3) . . ? C48 C49 H49 119.5 . . ? C50 C49 H49 119.5 . . ? C49 C50 C45 118.3(3) . . ? C49 C50 C52 121.3(3) . . ? C45 C50 C52 120.4(3) . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C57 C53 C54 108.3(2) . . ? C57 C53 C58 125.2(3) . . ? C54 C53 C58 125.8(3) . . ? C57 C53 Ru2 72.95(17) . . ? C54 C53 Ru2 72.85(17) . . ? C58 C53 Ru2 127.4(2) . . ? C55 C54 C53 107.4(3) . . ? C55 C54 C59 125.0(3) . . ? C53 C54 C59 126.8(3) . . ? C55 C54 Ru2 70.01(18) . . ? C53 C54 Ru2 68.62(17) . . ? C59 C54 Ru2 134.5(2) . . ? C54 C55 C56 108.4(3) . . ? C54 C55 C60 125.3(3) . . ? C56 C55 C60 125.6(3) . . ? C54 C55 Ru2 72.27(17) . . ? C56 C55 Ru2 70.86(17) . . ? C60 C55 Ru2 130.3(2) . . ? C57 C56 C55 107.8(3) . . ? C57 C56 C61 126.9(3) . . ? C55 C56 C61 124.8(3) . . ? C57 C56 Ru2 72.01(17) . . ? C55 C56 Ru2 70.37(17) . . ? C61 C56 Ru2 129.8(2) . . ? C56 C57 C53 107.8(3) . . ? C56 C57 C62 126.4(3) . . ? C53 C57 C62 125.1(3) . . ? C56 C57 Ru2 70.24(17) . . ? C53 C57 Ru2 68.68(17) . . ? C62 C57 Ru2 133.3(2) . . ? C53 C58 H58A 109.5 . . ? C53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C53 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C54 C59 H59A 109.5 . . ? C54 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C54 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C55 C60 H60A 109.5 . . ? C55 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C56 C61 H61A 109.5 . . ? C56 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C56 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C9 N1 C1 114.3(2) . . ? C9 N1 Ru1 128.9(2) . . ? C1 N1 Ru1 116.77(19) . . ? C12 N2 C14 113.7(2) . . ? C12 N2 Ru1 129.31(19) . . ? C14 N2 Ru1 116.97(19) . . ? C40 N3 C32 113.6(2) . . ? C40 N3 Ru2 128.89(19) . . ? C32 N3 Ru2 117.49(19) . . ? C43 N4 C45 114.0(2) . . ? C43 N4 Ru2 129.0(2) . . ? C45 N4 Ru2 117.02(19) . . ? N2 Ru1 N1 87.22(10) . . ? N2 Ru1 C22 127.18(10) . . ? N1 Ru1 C22 127.01(10) . . ? N2 Ru1 C24 145.14(10) . . ? N1 Ru1 C24 112.16(10) . . ? C22 Ru1 C24 64.25(11) . . ? N2 Ru1 C25 111.17(10) . . ? N1 Ru1 C25 146.28(10) . . ? C22 Ru1 C25 64.22(11) . . ? C24 Ru1 C25 38.69(11) . . ? N2 Ru1 C23 165.55(10) . . ? N1 Ru1 C23 104.07(10) . . ? C22 Ru1 C23 38.47(11) . . ? C24 Ru1 C23 37.81(11) . . ? C25 Ru1 C23 63.89(11) . . ? N2 Ru1 C26 103.76(10) . . ? N1 Ru1 C26 165.30(10) . . ? C22 Ru1 C26 38.31(11) . . ? C24 Ru1 C26 63.80(11) . . ? C25 Ru1 C26 37.79(11) . . ? C23 Ru1 C26 63.65(11) . . ? N3 Ru2 N4 87.34(10) . . ? N3 Ru2 C53 125.69(10) . . ? N4 Ru2 C53 128.27(10) . . ? N3 Ru2 C55 146.79(11) . . ? N4 Ru2 C55 111.20(11) . . ? C53 Ru2 C55 64.26(11) . . ? N3 Ru2 C56 112.07(11) . . ? N4 Ru2 C56 144.74(10) . . ? C53 Ru2 C56 64.28(11) . . ? C55 Ru2 C56 38.77(11) . . ? N3 Ru2 C54 164.21(11) . . ? N4 Ru2 C54 104.35(10) . . ? C53 Ru2 C54 38.53(11) . . ? C55 Ru2 C54 37.73(11) . . ? C56 Ru2 C54 63.91(11) . . ? N3 Ru2 C57 103.36(10) . . ? N4 Ru2 C57 166.48(10) . . ? C53 Ru2 C57 38.36(11) . . ? C55 Ru2 C57 63.79(11) . . ? C56 Ru2 C57 37.75(11) . . ? C54 Ru2 C57 63.66(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.1(5) . . . . ? N1 C1 C2 C3 -178.3(3) . . . . ? C6 C1 C2 C7 178.7(3) . . . . ? N1 C1 C2 C7 1.5(5) . . . . ? C1 C2 C3 C4 -1.7(5) . . . . ? C7 C2 C3 C4 178.5(3) . . . . ? C2 C3 C4 C5 2.0(6) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C4 C5 C6 C1 -3.2(5) . . . . ? C4 C5 C6 C8 174.3(3) . . . . ? C2 C1 C6 C5 3.5(5) . . . . ? N1 C1 C6 C5 -179.2(3) . . . . ? C2 C1 C6 C8 -174.0(3) . . . . ? N1 C1 C6 C8 3.2(5) . . . . ? N1 C9 C11 C12 -1.8(5) . . . . ? C10 C9 C11 C12 178.9(3) . . . . ? C9 C11 C12 N2 -1.1(5) . . . . ? C9 C11 C12 C13 178.9(3) . . . . ? C19 C14 C15 C16 -2.8(5) . . . . ? N2 C14 C15 C16 -178.8(3) . . . . ? C19 C14 C15 C20 174.5(3) . . . . ? N2 C14 C15 C20 -1.6(5) . . . . ? C14 C15 C16 C17 2.2(5) . . . . ? C20 C15 C16 C17 -175.0(3) . . . . ? C15 C16 C17 C18 -0.5(5) . . . . ? C16 C17 C18 C19 -0.8(5) . . . . ? C17 C18 C19 C14 0.2(5) . . . . ? C17 C18 C19 C21 -179.9(3) . . . . ? C15 C14 C19 C18 1.6(5) . . . . ? N2 C14 C19 C18 177.7(3) . . . . ? C15 C14 C19 C21 -178.3(3) . . . . ? N2 C14 C19 C21 -2.3(4) . . . . ? C26 C22 C23 C24 4.9(3) . . . . ? C27 C22 C23 C24 175.1(3) . . . . ? Ru1 C22 C23 C24 -59.7(2) . . . . ? C26 C22 C23 C28 -167.2(3) . . . . ? C27 C22 C23 C28 3.0(5) . . . . ? Ru1 C22 C23 C28 128.2(3) . . . . ? C26 C22 C23 Ru1 64.6(2) . . . . ? C27 C22 C23 Ru1 -125.2(3) . . . . ? C22 C23 C24 C25 -3.0(3) . . . . ? C28 C23 C24 C25 169.1(3) . . . . ? Ru1 C23 C24 C25 -62.0(2) . . . . ? C22 C23 C24 C29 -173.0(3) . . . . ? C28 C23 C24 C29 -0.9(5) . . . . ? Ru1 C23 C24 C29 128.1(3) . . . . ? C22 C23 C24 Ru1 59.0(2) . . . . ? C28 C23 C24 Ru1 -129.0(3) . . . . ? C23 C24 C25 C26 -0.1(3) . . . . ? C29 C24 C25 C26 170.1(3) . . . . ? Ru1 C24 C25 C26 -62.9(2) . . . . ? C23 C24 C25 C30 -170.8(3) . . . . ? C29 C24 C25 C30 -0.7(5) . . . . ? Ru1 C24 C25 C30 126.3(3) . . . . ? C23 C24 C25 Ru1 62.8(2) . . . . ? C29 C24 C25 Ru1 -127.0(3) . . . . ? C24 C25 C26 C22 3.1(3) . . . . ? C30 C25 C26 C22 173.8(3) . . . . ? Ru1 C25 C26 C22 -58.7(2) . . . . ? C24 C25 C26 C31 -167.8(3) . . . . ? C30 C25 C26 C31 3.0(5) . . . . ? Ru1 C25 C26 C31 130.4(3) . . . . ? C24 C25 C26 Ru1 61.8(2) . . . . ? C30 C25 C26 Ru1 -127.5(3) . . . . ? C23 C22 C26 C25 -5.0(3) . . . . ? C27 C22 C26 C25 -175.2(3) . . . . ? Ru1 C22 C26 C25 59.4(2) . . . . ? C23 C22 C26 C31 165.8(3) . . . . ? C27 C22 C26 C31 -4.5(5) . . . . ? Ru1 C22 C26 C31 -129.8(3) . . . . ? C23 C22 C26 Ru1 -64.4(2) . . . . ? C27 C22 C26 Ru1 125.3(3) . . . . ? C37 C32 C33 C34 -2.3(5) . . . . ? N3 C32 C33 C34 179.6(3) . . . . ? C37 C32 C33 C38 174.4(3) . . . . ? N3 C32 C33 C38 -3.7(5) . . . . ? C32 C33 C34 C35 1.8(5) . . . . ? C38 C33 C34 C35 -174.9(3) . . . . ? C33 C34 C35 C36 0.0(6) . . . . ? C34 C35 C36 C37 -1.3(5) . . . . ? C35 C36 C37 C32 0.7(5) . . . . ? C35 C36 C37 C39 -179.9(3) . . . . ? C33 C32 C37 C36 1.1(5) . . . . ? N3 C32 C37 C36 179.2(3) . . . . ? C33 C32 C37 C39 -178.3(3) . . . . ? N3 C32 C37 C39 -0.2(5) . . . . ? N3 C40 C42 C43 4.5(5) . . . . ? C41 C40 C42 C43 -175.6(3) . . . . ? C40 C42 C43 N4 -2.1(5) . . . . ? C40 C42 C43 C44 177.3(3) . . . . ? C50 C45 C46 C47 -1.5(5) . . . . ? N4 C45 C46 C47 -178.5(3) . . . . ? C50 C45 C46 C51 178.1(3) . . . . ? N4 C45 C46 C51 1.1(5) . . . . ? C45 C46 C47 C48 0.2(5) . . . . ? C51 C46 C47 C48 -179.4(3) . . . . ? C46 C47 C48 C49 0.9(5) . . . . ? C47 C48 C49 C50 -0.6(5) . . . . ? C48 C49 C50 C45 -0.7(5) . . . . ? C48 C49 C50 C52 177.0(3) . . . . ? C46 C45 C50 C49 1.7(5) . . . . ? N4 C45 C50 C49 178.7(3) . . . . ? C46 C45 C50 C52 -175.9(3) . . . . ? N4 C45 C50 C52 1.1(4) . . . . ? C57 C53 C54 C55 5.3(3) . . . . ? C58 C53 C54 C55 176.3(3) . . . . ? Ru2 C53 C54 C55 -59.5(2) . . . . ? C57 C53 C54 C59 -164.9(3) . . . . ? C58 C53 C54 C59 6.1(5) . . . . ? Ru2 C53 C54 C59 130.3(3) . . . . ? C57 C53 C54 Ru2 64.8(2) . . . . ? C58 C53 C54 Ru2 -124.2(3) . . . . ? C53 C54 C55 C56 -3.4(4) . . . . ? C59 C54 C55 C56 167.1(3) . . . . ? Ru2 C54 C55 C56 -62.0(2) . . . . ? C53 C54 C55 C60 -174.0(3) . . . . ? C59 C54 C55 C60 -3.6(5) . . . . ? Ru2 C54 C55 C60 127.3(3) . . . . ? C53 C54 C55 Ru2 58.6(2) . . . . ? C59 C54 C55 Ru2 -130.9(3) . . . . ? C54 C55 C56 C57 0.2(4) . . . . ? C60 C55 C56 C57 170.8(3) . . . . ? Ru2 C55 C56 C57 -62.7(2) . . . . ? C54 C55 C56 C61 -171.7(3) . . . . ? C60 C55 C56 C61 -1.0(5) . . . . ? Ru2 C55 C56 C61 125.4(3) . . . . ? C54 C55 C56 Ru2 62.9(2) . . . . ? C60 C55 C56 Ru2 -126.5(3) . . . . ? C55 C56 C57 C53 3.1(3) . . . . ? C61 C56 C57 C53 174.7(3) . . . . ? Ru2 C56 C57 C53 -58.6(2) . . . . ? C55 C56 C57 C62 -168.5(3) . . . . ? C61 C56 C57 C62 3.1(5) . . . . ? Ru2 C56 C57 C62 129.8(3) . . . . ? C55 C56 C57 Ru2 61.7(2) . . . . ? C61 C56 C57 Ru2 -126.7(3) . . . . ? C54 C53 C57 C56 -5.2(3) . . . . ? C58 C53 C57 C56 -176.3(3) . . . . ? Ru2 C53 C57 C56 59.6(2) . . . . ? C54 C53 C57 C62 166.5(3) . . . . ? C58 C53 C57 C62 -4.5(5) . . . . ? Ru2 C53 C57 C62 -128.7(3) . . . . ? C54 C53 C57 Ru2 -64.8(2) . . . . ? C58 C53 C57 Ru2 124.2(3) . . . . ? C11 C9 N1 C1 -178.2(3) . . . . ? C10 C9 N1 C1 1.1(4) . . . . ? C11 C9 N1 Ru1 3.0(4) . . . . ? C10 C9 N1 Ru1 -177.7(2) . . . . ? C2 C1 N1 C9 87.6(3) . . . . ? C6 C1 N1 C9 -89.7(3) . . . . ? C2 C1 N1 Ru1 -93.4(3) . . . . ? C6 C1 N1 Ru1 89.3(3) . . . . ? C11 C12 N2 C14 -177.3(3) . . . . ? C13 C12 N2 C14 2.6(4) . . . . ? C11 C12 N2 Ru1 2.7(4) . . . . ? C13 C12 N2 Ru1 -177.3(2) . . . . ? C15 C14 N2 C12 87.6(3) . . . . ? C19 C14 N2 C12 -88.5(3) . . . . ? C15 C14 N2 Ru1 -92.4(3) . . . . ? C19 C14 N2 Ru1 91.4(3) . . . . ? C42 C40 N3 C32 178.4(3) . . . . ? C41 C40 N3 C32 -1.5(4) . . . . ? C42 C40 N3 Ru2 -1.5(4) . . . . ? C41 C40 N3 Ru2 178.7(2) . . . . ? C37 C32 N3 C40 -87.0(3) . . . . ? C33 C32 N3 C40 91.2(3) . . . . ? C37 C32 N3 Ru2 92.9(3) . . . . ? C33 C32 N3 Ru2 -89.0(3) . . . . ? C42 C43 N4 C45 175.2(3) . . . . ? C44 C43 N4 C45 -4.1(4) . . . . ? C42 C43 N4 Ru2 -3.1(4) . . . . ? C44 C43 N4 Ru2 177.5(2) . . . . ? C50 C45 N4 C43 -88.3(3) . . . . ? C46 C45 N4 C43 88.8(3) . . . . ? C50 C45 N4 Ru2 90.3(3) . . . . ? C46 C45 N4 Ru2 -92.6(3) . . . . ? C12 N2 Ru1 N1 -1.4(2) . . . . ? C14 N2 Ru1 N1 178.6(2) . . . . ? C12 N2 Ru1 C22 134.6(2) . . . . ? C14 N2 Ru1 C22 -45.3(2) . . . . ? C12 N2 Ru1 C24 -127.6(3) . . . . ? C14 N2 Ru1 C24 52.4(3) . . . . ? C12 N2 Ru1 C25 -152.3(2) . . . . ? C14 N2 Ru1 C25 27.7(2) . . . . ? C12 N2 Ru1 C23 140.5(4) . . . . ? C14 N2 Ru1 C23 -39.4(5) . . . . ? C12 N2 Ru1 C26 168.7(2) . . . . ? C14 N2 Ru1 C26 -11.3(2) . . . . ? C9 N1 Ru1 N2 -1.4(3) . . . . ? C1 N1 Ru1 N2 179.8(2) . . . . ? C9 N1 Ru1 C22 -137.6(2) . . . . ? C1 N1 Ru1 C22 43.7(2) . . . . ? C9 N1 Ru1 C24 148.7(2) . . . . ? C1 N1 Ru1 C24 -30.0(2) . . . . ? C9 N1 Ru1 C25 123.9(3) . . . . ? C1 N1 Ru1 C25 -54.8(3) . . . . ? C9 N1 Ru1 C23 -172.3(2) . . . . ? C1 N1 Ru1 C23 9.0(2) . . . . ? C9 N1 Ru1 C26 -140.3(4) . . . . ? C1 N1 Ru1 C26 41.0(5) . . . . ? C26 C22 Ru1 N2 61.4(2) . . . . ? C23 C22 Ru1 N2 177.64(15) . . . . ? C27 C22 Ru1 N2 -60.3(3) . . . . ? C26 C22 Ru1 N1 -178.88(15) . . . . ? C23 C22 Ru1 N1 -62.7(2) . . . . ? C27 C22 Ru1 N1 59.4(3) . . . . ? C26 C22 Ru1 C24 -79.62(18) . . . . ? C23 C22 Ru1 C24 36.60(17) . . . . ? C27 C22 Ru1 C24 158.7(3) . . . . ? C26 C22 Ru1 C25 -36.46(17) . . . . ? C23 C22 Ru1 C25 79.76(18) . . . . ? C27 C22 Ru1 C25 -158.1(3) . . . . ? C26 C22 Ru1 C23 -116.2(2) . . . . ? C27 C22 Ru1 C23 122.1(3) . . . . ? C23 C22 Ru1 C26 116.2(2) . . . . ? C27 C22 Ru1 C26 -121.7(3) . . . . ? C23 C24 Ru1 N2 -156.00(17) . . . . ? C25 C24 Ru1 N2 -38.6(3) . . . . ? C29 C24 Ru1 N2 81.1(3) . . . . ? C23 C24 Ru1 N1 84.45(18) . . . . ? C25 C24 Ru1 N1 -158.12(16) . . . . ? C29 C24 Ru1 N1 -38.5(3) . . . . ? C23 C24 Ru1 C22 -37.23(17) . . . . ? C25 C24 Ru1 C22 80.20(18) . . . . ? C29 C24 Ru1 C22 -160.2(3) . . . . ? C23 C24 Ru1 C25 -117.4(2) . . . . ? C29 C24 Ru1 C25 119.6(3) . . . . ? C25 C24 Ru1 C23 117.4(2) . . . . ? C29 C24 Ru1 C23 -122.9(4) . . . . ? C23 C24 Ru1 C26 -80.04(18) . . . . ? C25 C24 Ru1 C26 37.38(16) . . . . ? C29 C24 Ru1 C26 157.0(3) . . . . ? C26 C25 Ru1 N2 -85.22(18) . . . . ? C24 C25 Ru1 N2 157.53(16) . . . . ? C30 C25 Ru1 N2 37.1(3) . . . . ? C26 C25 Ru1 N1 155.67(18) . . . . ? C24 C25 Ru1 N1 38.4(3) . . . . ? C30 C25 Ru1 N1 -82.0(3) . . . . ? C26 C25 Ru1 C22 36.96(17) . . . . ? C24 C25 Ru1 C22 -80.28(18) . . . . ? C30 C25 Ru1 C22 159.3(3) . . . . ? C26 C25 Ru1 C24 117.2(2) . . . . ? C30 C25 Ru1 C24 -120.5(3) . . . . ? C26 C25 Ru1 C23 79.94(18) . . . . ? C24 C25 Ru1 C23 -37.30(16) . . . . ? C30 C25 Ru1 C23 -157.8(3) . . . . ? C24 C25 Ru1 C26 -117.2(2) . . . . ? C30 C25 Ru1 C26 122.3(4) . . . . ? C24 C23 Ru1 N2 111.3(4) . . . . ? C22 C23 Ru1 N2 -7.6(5) . . . . ? C28 C23 Ru1 N2 -127.1(4) . . . . ? C24 C23 Ru1 N1 -108.14(17) . . . . ? C22 C23 Ru1 N1 133.00(17) . . . . ? C28 C23 Ru1 N1 13.5(3) . . . . ? C24 C23 Ru1 C22 118.9(2) . . . . ? C28 C23 Ru1 C22 -119.5(4) . . . . ? C22 C23 Ru1 C24 -118.9(2) . . . . ? C28 C23 Ru1 C24 121.6(4) . . . . ? C24 C23 Ru1 C25 38.17(17) . . . . ? C22 C23 Ru1 C25 -80.69(18) . . . . ? C28 C23 Ru1 C25 159.8(3) . . . . ? C24 C23 Ru1 C26 80.49(18) . . . . ? C22 C23 Ru1 C26 -38.37(17) . . . . ? C28 C23 Ru1 C26 -157.9(3) . . . . ? C25 C26 Ru1 N2 106.92(17) . . . . ? C22 C26 Ru1 N2 -133.92(17) . . . . ? C31 C26 Ru1 N2 -13.4(3) . . . . ? C25 C26 Ru1 N1 -115.6(4) . . . . ? C22 C26 Ru1 N1 3.5(5) . . . . ? C31 C26 Ru1 N1 124.0(4) . . . . ? C25 C26 Ru1 C22 -119.2(2) . . . . ? C31 C26 Ru1 C22 120.5(4) . . . . ? C25 C26 Ru1 C24 -38.27(17) . . . . ? C22 C26 Ru1 C24 80.89(18) . . . . ? C31 C26 Ru1 C24 -158.6(3) . . . . ? C22 C26 Ru1 C25 119.2(2) . . . . ? C31 C26 Ru1 C25 -120.3(4) . . . . ? C25 C26 Ru1 C23 -80.64(18) . . . . ? C22 C26 Ru1 C23 38.52(17) . . . . ? C31 C26 Ru1 C23 159.0(3) . . . . ? C40 N3 Ru2 N4 -2.0(2) . . . . ? C32 N3 Ru2 N4 178.1(2) . . . . ? C40 N3 Ru2 C53 134.9(2) . . . . ? C32 N3 Ru2 C53 -45.0(2) . . . . ? C40 N3 Ru2 C55 -128.2(3) . . . . ? C32 N3 Ru2 C55 52.0(3) . . . . ? C40 N3 Ru2 C56 -151.7(2) . . . . ? C32 N3 Ru2 C56 28.4(2) . . . . ? C40 N3 Ru2 C54 136.4(4) . . . . ? C32 N3 Ru2 C54 -43.5(5) . . . . ? C40 N3 Ru2 C57 169.6(2) . . . . ? C32 N3 Ru2 C57 -10.2(2) . . . . ? C43 N4 Ru2 N3 4.3(2) . . . . ? C45 N4 Ru2 N3 -174.0(2) . . . . ? C43 N4 Ru2 C53 -130.7(2) . . . . ? C45 N4 Ru2 C53 51.0(2) . . . . ? C43 N4 Ru2 C55 156.0(2) . . . . ? C45 N4 Ru2 C55 -22.3(2) . . . . ? C43 N4 Ru2 C56 130.2(3) . . . . ? C45 N4 Ru2 C56 -48.1(3) . . . . ? C43 N4 Ru2 C54 -164.9(2) . . . . ? C45 N4 Ru2 C54 16.7(2) . . . . ? C43 N4 Ru2 C57 -138.5(4) . . . . ? C45 N4 Ru2 C57 43.2(5) . . . . ? C57 C53 Ru2 N3 63.31(19) . . . . ? C54 C53 Ru2 N3 179.35(15) . . . . ? C58 C53 Ru2 N3 -58.4(3) . . . . ? C57 C53 Ru2 N4 -177.09(15) . . . . ? C54 C53 Ru2 N4 -61.0(2) . . . . ? C58 C53 Ru2 N4 61.2(3) . . . . ? C57 C53 Ru2 C55 -79.57(18) . . . . ? C54 C53 Ru2 C55 36.47(17) . . . . ? C58 C53 Ru2 C55 158.7(3) . . . . ? C57 C53 Ru2 C56 -36.34(16) . . . . ? C54 C53 Ru2 C56 79.71(18) . . . . ? C58 C53 Ru2 C56 -158.0(3) . . . . ? C57 C53 Ru2 C54 -116.0(2) . . . . ? C58 C53 Ru2 C54 122.3(3) . . . . ? C54 C53 Ru2 C57 116.0(2) . . . . ? C58 C53 Ru2 C57 -121.7(3) . . . . ? C54 C55 Ru2 N3 -153.72(19) . . . . ? C56 C55 Ru2 N3 -36.2(3) . . . . ? C60 C55 Ru2 N3 84.6(4) . . . . ? C54 C55 Ru2 N4 86.17(18) . . . . ? C56 C55 Ru2 N4 -156.33(16) . . . . ? C60 C55 Ru2 N4 -35.5(3) . . . . ? C54 C55 Ru2 C53 -37.23(17) . . . . ? C56 C55 Ru2 C53 80.26(18) . . . . ? C60 C55 Ru2 C53 -158.9(3) . . . . ? C54 C55 Ru2 C56 -117.5(2) . . . . ? C60 C55 Ru2 C56 120.9(4) . . . . ? C56 C55 Ru2 C54 117.5(2) . . . . ? C60 C55 Ru2 C54 -121.7(4) . . . . ? C54 C55 Ru2 C57 -80.11(19) . . . . ? C56 C55 Ru2 C57 37.39(17) . . . . ? C60 C55 Ru2 C57 158.2(3) . . . . ? C57 C56 Ru2 N3 -83.31(18) . . . . ? C55 C56 Ru2 N3 159.56(16) . . . . ? C61 C56 Ru2 N3 40.1(3) . . . . ? C57 C56 Ru2 N4 157.56(18) . . . . ? C55 C56 Ru2 N4 40.4(3) . . . . ? C61 C56 Ru2 N4 -79.0(3) . . . . ? C57 C56 Ru2 C53 36.92(17) . . . . ? C55 C56 Ru2 C53 -80.21(19) . . . . ? C61 C56 Ru2 C53 160.4(3) . . . . ? C57 C56 Ru2 C55 117.1(3) . . . . ? C61 C56 Ru2 C55 -119.4(4) . . . . ? C57 C56 Ru2 C54 79.95(19) . . . . ? C55 C56 Ru2 C54 -37.18(17) . . . . ? C61 C56 Ru2 C54 -156.6(3) . . . . ? C55 C56 Ru2 C57 -117.1(3) . . . . ? C61 C56 Ru2 C57 123.4(4) . . . . ? C55 C54 Ru2 N3 117.0(4) . . . . ? C53 C54 Ru2 N3 -1.9(5) . . . . ? C59 C54 Ru2 N3 -123.2(4) . . . . ? C55 C54 Ru2 N4 -106.21(18) . . . . ? C53 C54 Ru2 N4 134.84(16) . . . . ? C59 C54 Ru2 N4 13.6(3) . . . . ? C55 C54 Ru2 C53 119.0(3) . . . . ? C59 C54 Ru2 C53 -121.2(4) . . . . ? C53 C54 Ru2 C55 -119.0(3) . . . . ? C59 C54 Ru2 C55 119.8(4) . . . . ? C55 C54 Ru2 C56 38.20(17) . . . . ? C53 C54 Ru2 C56 -80.75(18) . . . . ? C59 C54 Ru2 C56 158.0(3) . . . . ? C55 C54 Ru2 C57 80.47(19) . . . . ? C53 C54 Ru2 C57 -38.48(16) . . . . ? C59 C54 Ru2 C57 -159.7(3) . . . . ? C56 C57 Ru2 N3 108.92(18) . . . . ? C53 C57 Ru2 N3 -131.77(16) . . . . ? C62 C57 Ru2 N3 -13.0(3) . . . . ? C56 C57 Ru2 N4 -109.5(4) . . . . ? C53 C57 Ru2 N4 9.8(5) . . . . ? C62 C57 Ru2 N4 128.6(4) . . . . ? C56 C57 Ru2 C53 -119.3(2) . . . . ? C62 C57 Ru2 C53 118.8(4) . . . . ? C56 C57 Ru2 C55 -38.40(18) . . . . ? C53 C57 Ru2 C55 80.91(18) . . . . ? C62 C57 Ru2 C55 -160.3(3) . . . . ? C53 C57 Ru2 C56 119.3(2) . . . . ? C62 C57 Ru2 C56 -121.9(4) . . . . ? C56 C57 Ru2 C54 -80.67(19) . . . . ? C53 C57 Ru2 C54 38.64(16) . . . . ? C62 C57 Ru2 C54 157.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.361 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.072 data_adp481 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*Ru((3,5-Me2C6H3NCMe)2CH)' _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 N2 Ru' _chemical_formula_sum 'C31 H40 N2 Ru' _chemical_formula_weight 541.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6289(14) _cell_length_b 11.0346(18) _cell_length_c 13.8160(15) _cell_angle_alpha 79.105(11) _cell_angle_beta 76.564(9) _cell_angle_gamma 73.919(10) _cell_volume 1359.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 53 _cell_measurement_theta_min 3.567 _cell_measurement_theta_max 21.828 _exptl_crystal_description prisim _exptl_crystal_colour red _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_min 0.166 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 0.597 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.862128 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; Bruker Nonius Area Dector Scaling and Absorption Correction SADABS 2.10 (Bruker, 2003) based on an algorithm described by R.H. Blessing, Acta Cryst. (1995), a51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonus KappaCCD with \k-goniostat' _diffrn_detector 'Bruker Apex II CCD' _diffrn_measurement_method '\f & \w scans' _diffrn_source 'Enraf Nonius FR590' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26496 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4772 _reflns_number_gt 4521 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'Collect (Hooft, R.W.W., 1998. Nonius B.V., 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg A.J.M., Nonius B.V., 1989-2000)' _computing_data_reduction 'EvalCCD (Hooft R.W.W., Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick G.M., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick G.M., 2008)' _computing_molecular_graphics 'ORTEP-3 for windows 2.02 (Farrugia, 2008)' _computing_publication_material 'WinGX 1.80.05 (Farrugia, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A number of CF3 substituents are positioned disordered over multiple sites. A split refinement method used employed where the occupancy was allowed to refine. Some of the fluorine atoms are prolate due diffuse electron density. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+1.2717P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4772 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0191 _refine_ls_wR_factor_ref 0.0482 _refine_ls_wR_factor_gt 0.0467 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.76307(19) 0.45289(16) 0.20435(13) 0.0131(3) Uani 1 1 d . . . C2 C 0.79848(19) 0.50336(16) 0.10382(13) 0.0150(4) Uani 1 1 d . . . H2 H 0.8989 0.4912 0.0714 0.018 Uiso 1 1 calc R . . C3 C 0.6881(2) 0.57160(17) 0.05020(14) 0.0179(4) Uani 1 1 d . . . C4 C 0.5411(2) 0.58933(17) 0.09989(15) 0.0185(4) Uani 1 1 d . . . H4 H 0.4652 0.6351 0.0641 0.022 Uiso 1 1 calc R . . C5 C 0.5035(2) 0.54131(16) 0.20085(15) 0.0172(4) Uani 1 1 d . . . C6 C 0.61591(19) 0.47309(16) 0.25283(14) 0.0149(4) Uani 1 1 d . . . H6 H 0.5918 0.4403 0.3216 0.018 Uiso 1 1 calc R . . C7 C 0.7280(2) 0.6229(2) -0.05977(15) 0.0260(4) Uani 1 1 d . . . H7A H 0.7689 0.6965 -0.0657 0.039 Uiso 1 1 calc R . . H7B H 0.6396 0.6487 -0.0896 0.039 Uiso 1 1 calc R . . H7C H 0.8012 0.5565 -0.0951 0.039 Uiso 1 1 calc R . . C8 C 0.3438(2) 0.55811(19) 0.25276(16) 0.0244(4) Uani 1 1 d . . . H8A H 0.2810 0.6198 0.2102 0.037 Uiso 1 1 calc R . . H8B H 0.3297 0.5892 0.3171 0.037 Uiso 1 1 calc R . . H8C H 0.3174 0.4762 0.2645 0.037 Uiso 1 1 calc R . . C9 C 0.92374(19) 0.44350(16) 0.31301(13) 0.0134(4) Uani 1 1 d . . . C10 C 0.8465(2) 0.58200(17) 0.32260(16) 0.0216(4) Uani 1 1 d . . . H10A H 0.8467 0.6309 0.2555 0.032 Uiso 1 1 calc R . . H10B H 0.8983 0.6164 0.3601 0.032 Uiso 1 1 calc R . . H10C H 0.7447 0.5880 0.3583 0.032 Uiso 1 1 calc R . . C11 C 1.04010(19) 0.38972(17) 0.36442(13) 0.0144(4) Uani 1 1 d . . . H11 H 1.0587 0.4431 0.4039 0.017 Uiso 1 1 calc R . . C12 C 1.13245(18) 0.26710(16) 0.36494(13) 0.0129(3) Uani 1 1 d . . . C13 C 1.2598(2) 0.23851(18) 0.42037(15) 0.0199(4) Uani 1 1 d . . . H13A H 1.2491 0.1699 0.4760 0.030 Uiso 1 1 calc R . . H13B H 1.2592 0.3151 0.4468 0.030 Uiso 1 1 calc R . . H13C H 1.3531 0.2122 0.3739 0.030 Uiso 1 1 calc R . . C14 C 1.22453(18) 0.05782(16) 0.32393(13) 0.0119(3) Uani 1 1 d . . . C15 C 1.21039(18) -0.03509(16) 0.40737(13) 0.0134(4) Uani 1 1 d . . . H15 H 1.1299 -0.0182 0.4618 0.016 Uiso 1 1 calc R . . C16 C 1.31363(19) -0.15262(17) 0.41151(13) 0.0147(4) Uani 1 1 d . . . C17 C 1.43178(19) -0.17481(17) 0.33092(13) 0.0151(4) Uani 1 1 d . . . H17 H 1.5021 -0.2545 0.3329 0.018 Uiso 1 1 calc R . . C18 C 1.44906(18) -0.08280(17) 0.24762(13) 0.0141(4) Uani 1 1 d . . . C19 C 1.34453(18) 0.03428(16) 0.24557(13) 0.0129(3) Uani 1 1 d . . . H19 H 1.3558 0.0985 0.1899 0.015 Uiso 1 1 calc R . . C20 C 1.2939(2) -0.25608(18) 0.49906(15) 0.0244(4) Uani 1 1 d . . . H20A H 1.2509 -0.2175 0.5610 0.037 Uiso 1 1 calc R . . H20B H 1.3898 -0.3143 0.5054 0.037 Uiso 1 1 calc R . . H20C H 1.2282 -0.3034 0.4875 0.037 Uiso 1 1 calc R . . C21 C 1.5763(2) -0.10844(18) 0.16021(14) 0.0195(4) Uani 1 1 d . . . H21A H 1.6465 -0.0588 0.1600 0.029 Uiso 1 1 calc R . . H21B H 1.5392 -0.0839 0.0972 0.029 Uiso 1 1 calc R . . H21C H 1.6256 -0.1993 0.1668 0.029 Uiso 1 1 calc R . . C22 C 0.82533(19) 0.06305(16) 0.24155(13) 0.0129(3) Uani 1 1 d . . . C23 C 0.97733(19) -0.00773(16) 0.21833(13) 0.0132(3) Uani 1 1 d . . . C24 C 1.04337(19) 0.05354(16) 0.12568(13) 0.0139(4) Uani 1 1 d . . . C25 C 0.93154(19) 0.15883(16) 0.08931(13) 0.0142(4) Uani 1 1 d . . . C26 C 0.79538(19) 0.16052(16) 0.15831(13) 0.0129(3) Uani 1 1 d . . . C27 C 0.7154(2) 0.02801(18) 0.33180(14) 0.0188(4) Uani 1 1 d . . . H27A H 0.6287 0.0997 0.3405 0.028 Uiso 1 1 calc R . . H27B H 0.7600 0.0077 0.3917 0.028 Uiso 1 1 calc R . . H27C H 0.6857 -0.0463 0.3221 0.028 Uiso 1 1 calc R . . C28 C 1.0440(2) -0.13160(17) 0.27572(14) 0.0184(4) Uani 1 1 d . . . H28A H 1.0172 -0.2012 0.2554 0.028 Uiso 1 1 calc R . . H28B H 1.0070 -0.1289 0.3478 0.028 Uiso 1 1 calc R . . H28C H 1.1514 -0.1457 0.2615 0.028 Uiso 1 1 calc R . . C29 C 1.1954(2) 0.00975(19) 0.06555(14) 0.0201(4) Uani 1 1 d . . . H29A H 1.2541 -0.0588 0.1064 0.030 Uiso 1 1 calc R . . H29B H 1.2425 0.0811 0.0456 0.030 Uiso 1 1 calc R . . H29C H 1.1887 -0.0216 0.0054 0.030 Uiso 1 1 calc R . . C30 C 0.9547(2) 0.23745(18) -0.01225(13) 0.0207(4) Uani 1 1 d . . . H30A H 0.9629 0.1858 -0.0647 0.031 Uiso 1 1 calc R . . H30B H 1.0453 0.2661 -0.0222 0.031 Uiso 1 1 calc R . . H30C H 0.8709 0.3116 -0.0159 0.031 Uiso 1 1 calc R . . C31 C 0.64510(19) 0.23619(17) 0.14131(14) 0.0176(4) Uani 1 1 d . . . H31A H 0.6524 0.3185 0.1016 0.026 Uiso 1 1 calc R . . H31B H 0.5795 0.2501 0.2062 0.026 Uiso 1 1 calc R . . H31C H 0.6054 0.1893 0.1051 0.026 Uiso 1 1 calc R . . N1 N 0.88019(15) 0.37960(13) 0.25618(11) 0.0117(3) Uani 1 1 d . . . N2 N 1.11545(15) 0.17784(13) 0.31748(10) 0.0111(3) Uani 1 1 d . . . Ru1 Ru 0.959838(14) 0.191882(12) 0.232755(10) 0.00910(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0161(9) 0.0081(8) 0.0171(9) -0.0027(7) -0.0064(7) -0.0031(7) C2 0.0156(9) 0.0126(8) 0.0181(9) -0.0011(7) -0.0042(7) -0.0051(7) C3 0.0239(10) 0.0126(9) 0.0205(10) 0.0013(7) -0.0104(8) -0.0073(7) C4 0.0196(9) 0.0112(8) 0.0271(10) 0.0001(8) -0.0137(8) -0.0014(7) C5 0.0159(9) 0.0104(8) 0.0270(10) -0.0061(7) -0.0061(8) -0.0020(7) C6 0.0173(9) 0.0120(8) 0.0158(9) -0.0027(7) -0.0035(7) -0.0033(7) C7 0.0310(11) 0.0254(11) 0.0243(11) 0.0079(9) -0.0145(9) -0.0112(9) C8 0.0150(9) 0.0238(10) 0.0345(12) -0.0087(9) -0.0057(8) -0.0012(8) C9 0.0138(8) 0.0121(8) 0.0140(9) -0.0017(7) -0.0012(7) -0.0037(7) C10 0.0235(10) 0.0143(9) 0.0304(11) -0.0073(8) -0.0123(8) -0.0015(8) C11 0.0165(9) 0.0148(9) 0.0146(9) -0.0041(7) -0.0037(7) -0.0060(7) C12 0.0133(8) 0.0155(9) 0.0106(8) -0.0005(7) -0.0026(7) -0.0055(7) C13 0.0209(9) 0.0179(9) 0.0245(10) -0.0049(8) -0.0117(8) -0.0033(8) C14 0.0118(8) 0.0125(8) 0.0137(9) -0.0034(7) -0.0056(7) -0.0029(7) C15 0.0120(8) 0.0167(9) 0.0116(8) -0.0037(7) -0.0011(7) -0.0033(7) C16 0.0160(9) 0.0154(9) 0.0137(9) -0.0005(7) -0.0053(7) -0.0045(7) C17 0.0131(8) 0.0127(8) 0.0192(9) -0.0029(7) -0.0062(7) 0.0002(7) C18 0.0117(8) 0.0178(9) 0.0147(9) -0.0053(7) -0.0017(7) -0.0052(7) C19 0.0145(8) 0.0141(9) 0.0122(9) -0.0004(7) -0.0041(7) -0.0064(7) C20 0.0297(11) 0.0182(10) 0.0188(10) 0.0034(8) -0.0027(8) -0.0009(8) C21 0.0162(9) 0.0210(10) 0.0196(10) -0.0055(8) 0.0012(8) -0.0034(7) C22 0.0143(8) 0.0128(8) 0.0139(9) -0.0023(7) -0.0038(7) -0.0059(7) C23 0.0147(8) 0.0120(8) 0.0156(9) -0.0045(7) -0.0049(7) -0.0045(7) C24 0.0153(9) 0.0155(9) 0.0138(9) -0.0073(7) -0.0019(7) -0.0057(7) C25 0.0198(9) 0.0154(9) 0.0115(9) -0.0037(7) -0.0052(7) -0.0081(7) C26 0.0165(9) 0.0116(8) 0.0133(9) -0.0026(7) -0.0065(7) -0.0044(7) C27 0.0166(9) 0.0252(10) 0.0161(9) 0.0001(8) -0.0024(7) -0.0101(8) C28 0.0207(9) 0.0119(9) 0.0250(10) -0.0018(7) -0.0099(8) -0.0033(7) C29 0.0168(9) 0.0269(10) 0.0196(10) -0.0127(8) 0.0013(8) -0.0075(8) C30 0.0324(11) 0.0221(10) 0.0118(9) -0.0007(8) -0.0047(8) -0.0138(8) C31 0.0171(9) 0.0153(9) 0.0235(10) -0.0024(8) -0.0107(8) -0.0037(7) N1 0.0121(7) 0.0110(7) 0.0120(7) -0.0002(6) -0.0039(6) -0.0027(6) N2 0.0106(7) 0.0111(7) 0.0108(7) -0.0013(6) -0.0017(6) -0.0017(6) Ru1 0.00956(7) 0.00915(7) 0.00904(8) -0.00147(5) -0.00242(5) -0.00230(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.396(3) . ? C1 C6 1.395(2) . ? C1 N1 1.446(2) . ? C2 C3 1.399(3) . ? C2 H2 0.9500 . ? C3 C4 1.400(3) . ? C3 C7 1.517(3) . ? C4 C5 1.396(3) . ? C4 H4 0.9500 . ? C5 C6 1.400(3) . ? C5 C8 1.514(3) . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.347(2) . ? C9 C11 1.398(2) . ? C9 C10 1.519(2) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.398(2) . ? C11 H11 0.9500 . ? C12 N2 1.345(2) . ? C12 C13 1.524(2) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.390(2) . ? C14 C15 1.399(2) . ? C14 N2 1.447(2) . ? C15 C16 1.399(2) . ? C15 H15 0.9500 . ? C16 C17 1.398(2) . ? C16 C20 1.515(3) . ? C17 C18 1.395(3) . ? C17 H17 0.9500 . ? C18 C19 1.401(2) . ? C18 C21 1.513(2) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C26 1.441(2) . ? C22 C23 1.449(2) . ? C22 C27 1.502(2) . ? C22 Ru1 2.1436(17) . ? C23 C24 1.426(2) . ? C23 C28 1.500(2) . ? C23 Ru1 2.2055(17) . ? C24 C25 1.449(3) . ? C24 C29 1.504(2) . ? C24 Ru1 2.1877(17) . ? C25 C26 1.428(2) . ? C25 C30 1.508(2) . ? C25 Ru1 2.1711(17) . ? C26 C31 1.504(2) . ? C26 Ru1 2.2092(17) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N1 Ru1 2.0595(14) . ? N2 Ru1 2.0632(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.68(16) . . ? C2 C1 N1 119.14(15) . . ? C6 C1 N1 121.18(16) . . ? C1 C2 C3 120.86(17) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C4 C3 C2 118.52(17) . . ? C4 C3 C7 121.17(17) . . ? C2 C3 C7 120.30(17) . . ? C5 C4 C3 121.48(17) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 118.93(17) . . ? C4 C5 C8 120.85(17) . . ? C6 C5 C8 120.18(17) . . ? C1 C6 C5 120.50(17) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C11 123.48(15) . . ? N1 C9 C10 120.01(15) . . ? C11 C9 C10 116.50(15) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C12 128.06(16) . . ? C9 C11 H11 116.0 . . ? C12 C11 H11 116.0 . . ? N2 C12 C11 123.26(15) . . ? N2 C12 C13 120.23(15) . . ? C11 C12 C13 116.48(15) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 119.59(15) . . ? C19 C14 N2 119.42(15) . . ? C15 C14 N2 120.99(15) . . ? C16 C15 C14 120.65(16) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 118.62(16) . . ? C17 C16 C20 120.58(16) . . ? C15 C16 C20 120.73(16) . . ? C18 C17 C16 121.65(16) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 118.59(16) . . ? C17 C18 C21 121.20(16) . . ? C19 C18 C21 120.20(16) . . ? C14 C19 C18 120.87(16) . . ? C14 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C26 C22 C23 108.42(15) . . ? C26 C22 C27 126.65(16) . . ? C23 C22 C27 124.52(16) . . ? C26 C22 Ru1 73.14(10) . . ? C23 C22 Ru1 72.87(10) . . ? C27 C22 Ru1 125.70(12) . . ? C24 C23 C22 107.33(15) . . ? C24 C23 C28 127.20(16) . . ? C22 C23 C28 125.04(16) . . ? C24 C23 Ru1 70.39(9) . . ? C22 C23 Ru1 68.25(9) . . ? C28 C23 Ru1 132.34(12) . . ? C23 C24 C25 108.27(15) . . ? C23 C24 C29 127.64(17) . . ? C25 C24 C29 123.57(16) . . ? C23 C24 Ru1 71.74(10) . . ? C25 C24 Ru1 69.97(9) . . ? C29 C24 Ru1 130.43(12) . . ? C26 C25 C24 108.28(15) . . ? C26 C25 C30 127.12(16) . . ? C24 C25 C30 123.96(16) . . ? C26 C25 Ru1 72.42(10) . . ? C24 C25 Ru1 71.20(9) . . ? C30 C25 Ru1 129.31(12) . . ? C25 C26 C22 107.35(15) . . ? C25 C26 C31 126.54(16) . . ? C22 C26 C31 125.58(16) . . ? C25 C26 Ru1 69.53(9) . . ? C22 C26 Ru1 68.22(9) . . ? C31 C26 Ru1 133.86(12) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C9 N1 C1 115.61(14) . . ? C9 N1 Ru1 128.46(11) . . ? C1 N1 Ru1 115.92(10) . . ? C12 N2 C14 115.29(14) . . ? C12 N2 Ru1 128.64(11) . . ? C14 N2 Ru1 116.02(10) . . ? N1 Ru1 N2 87.92(6) . . ? N1 Ru1 C22 124.68(6) . . ? N2 Ru1 C22 128.29(6) . . ? N1 Ru1 C25 112.79(6) . . ? N2 Ru1 C25 143.43(6) . . ? C22 Ru1 C25 64.80(7) . . ? N1 Ru1 C24 147.99(6) . . ? N2 Ru1 C24 110.06(6) . . ? C22 Ru1 C24 64.62(6) . . ? C25 Ru1 C24 38.83(7) . . ? N1 Ru1 C23 163.54(6) . . ? N2 Ru1 C23 103.55(6) . . ? C22 Ru1 C23 38.88(6) . . ? C25 Ru1 C23 64.32(7) . . ? C24 Ru1 C23 37.87(6) . . ? N1 Ru1 C26 103.09(6) . . ? N2 Ru1 C26 166.60(6) . . ? C22 Ru1 C26 38.64(6) . . ? C25 Ru1 C26 38.05(6) . . ? C24 Ru1 C26 64.06(6) . . ? C23 Ru1 C26 64.15(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.5(3) . . . . ? N1 C1 C2 C3 178.09(15) . . . . ? C1 C2 C3 C4 0.6(3) . . . . ? C1 C2 C3 C7 -178.36(16) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? C7 C3 C4 C5 179.36(17) . . . . ? C3 C4 C5 C6 -0.5(3) . . . . ? C3 C4 C5 C8 -178.29(17) . . . . ? C2 C1 C6 C5 1.3(2) . . . . ? N1 C1 C6 C5 -178.24(15) . . . . ? C4 C5 C6 C1 -0.3(3) . . . . ? C8 C5 C6 C1 177.45(16) . . . . ? N1 C9 C11 C12 2.0(3) . . . . ? C10 C9 C11 C12 -177.20(17) . . . . ? C9 C11 C12 N2 -3.8(3) . . . . ? C9 C11 C12 C13 174.42(17) . . . . ? C19 C14 C15 C16 -1.7(2) . . . . ? N2 C14 C15 C16 177.78(15) . . . . ? C14 C15 C16 C17 0.5(3) . . . . ? C14 C15 C16 C20 -176.52(16) . . . . ? C15 C16 C17 C18 0.4(3) . . . . ? C20 C16 C17 C18 177.42(17) . . . . ? C16 C17 C18 C19 -0.1(3) . . . . ? C16 C17 C18 C21 -179.21(16) . . . . ? C15 C14 C19 C18 2.0(2) . . . . ? N2 C14 C19 C18 -177.48(15) . . . . ? C17 C18 C19 C14 -1.1(2) . . . . ? C21 C18 C19 C14 178.01(16) . . . . ? C26 C22 C23 C24 5.21(18) . . . . ? C27 C22 C23 C24 178.25(16) . . . . ? Ru1 C22 C23 C24 -59.80(11) . . . . ? C26 C22 C23 C28 -167.70(16) . . . . ? C27 C22 C23 C28 5.4(3) . . . . ? Ru1 C22 C23 C28 127.30(16) . . . . ? C26 C22 C23 Ru1 65.01(11) . . . . ? C27 C22 C23 Ru1 -121.95(17) . . . . ? C22 C23 C24 C25 -2.28(18) . . . . ? C28 C23 C24 C25 170.42(16) . . . . ? Ru1 C23 C24 C25 -60.74(11) . . . . ? C22 C23 C24 C29 -174.10(16) . . . . ? C28 C23 C24 C29 -1.4(3) . . . . ? Ru1 C23 C24 C29 127.44(18) . . . . ? C22 C23 C24 Ru1 58.45(11) . . . . ? C28 C23 C24 Ru1 -128.85(17) . . . . ? C23 C24 C25 C26 -1.49(19) . . . . ? C29 C24 C25 C26 170.73(15) . . . . ? Ru1 C24 C25 C26 -63.36(11) . . . . ? C23 C24 C25 C30 -172.86(15) . . . . ? C29 C24 C25 C30 -0.6(3) . . . . ? Ru1 C24 C25 C30 125.28(16) . . . . ? C23 C24 C25 Ru1 61.86(11) . . . . ? C29 C24 C25 Ru1 -125.91(16) . . . . ? C24 C25 C26 C22 4.69(18) . . . . ? C30 C25 C26 C22 175.70(16) . . . . ? Ru1 C25 C26 C22 -57.89(11) . . . . ? C24 C25 C26 C31 -167.34(16) . . . . ? C30 C25 C26 C31 3.7(3) . . . . ? Ru1 C25 C26 C31 130.09(17) . . . . ? C24 C25 C26 Ru1 62.57(11) . . . . ? C30 C25 C26 Ru1 -126.41(17) . . . . ? C23 C22 C26 C25 -6.12(19) . . . . ? C27 C22 C26 C25 -178.98(16) . . . . ? Ru1 C22 C26 C25 58.71(11) . . . . ? C23 C22 C26 C31 166.00(15) . . . . ? C27 C22 C26 C31 -6.9(3) . . . . ? Ru1 C22 C26 C31 -129.17(16) . . . . ? C23 C22 C26 Ru1 -64.83(11) . . . . ? C27 C22 C26 Ru1 122.31(17) . . . . ? C11 C9 N1 C1 -176.78(16) . . . . ? C10 C9 N1 C1 2.4(2) . . . . ? C11 C9 N1 Ru1 2.7(2) . . . . ? C10 C9 N1 Ru1 -178.16(12) . . . . ? C2 C1 N1 C9 97.89(19) . . . . ? C6 C1 N1 C9 -82.6(2) . . . . ? C2 C1 N1 Ru1 -81.63(17) . . . . ? C6 C1 N1 Ru1 97.91(16) . . . . ? C11 C12 N2 C14 178.17(16) . . . . ? C13 C12 N2 C14 0.0(2) . . . . ? C11 C12 N2 Ru1 0.7(2) . . . . ? C13 C12 N2 Ru1 -177.40(12) . . . . ? C19 C14 N2 C12 -96.99(18) . . . . ? C15 C14 N2 C12 83.5(2) . . . . ? C19 C14 N2 Ru1 80.79(17) . . . . ? C15 C14 N2 Ru1 -98.71(16) . . . . ? C9 N1 Ru1 N2 -3.92(15) . . . . ? C1 N1 Ru1 N2 175.53(12) . . . . ? C9 N1 Ru1 C22 132.87(14) . . . . ? C1 N1 Ru1 C22 -47.68(14) . . . . ? C9 N1 Ru1 C25 -152.84(14) . . . . ? C1 N1 Ru1 C25 26.60(13) . . . . ? C9 N1 Ru1 C24 -130.04(15) . . . . ? C1 N1 Ru1 C24 49.41(17) . . . . ? C9 N1 Ru1 C23 130.9(2) . . . . ? C1 N1 Ru1 C23 -49.7(3) . . . . ? C9 N1 Ru1 C26 168.35(14) . . . . ? C1 N1 Ru1 C26 -12.20(13) . . . . ? C12 N2 Ru1 N1 2.26(15) . . . . ? C14 N2 Ru1 N1 -175.17(12) . . . . ? C12 N2 Ru1 C22 -131.90(14) . . . . ? C14 N2 Ru1 C22 50.67(14) . . . . ? C12 N2 Ru1 C25 129.25(15) . . . . ? C14 N2 Ru1 C25 -48.18(16) . . . . ? C12 N2 Ru1 C24 155.14(14) . . . . ? C14 N2 Ru1 C24 -22.29(13) . . . . ? C12 N2 Ru1 C23 -165.80(14) . . . . ? C14 N2 Ru1 C23 16.77(13) . . . . ? C12 N2 Ru1 C26 -143.3(2) . . . . ? C14 N2 Ru1 C26 39.3(3) . . . . ? C26 C22 Ru1 N1 64.88(11) . . . . ? C23 C22 Ru1 N1 -179.09(9) . . . . ? C27 C22 Ru1 N1 -58.51(17) . . . . ? C26 C22 Ru1 N2 -175.79(9) . . . . ? C23 C22 Ru1 N2 -59.75(12) . . . . ? C27 C22 Ru1 N2 60.83(17) . . . . ? C26 C22 Ru1 C25 -36.37(10) . . . . ? C23 C22 Ru1 C25 79.66(11) . . . . ? C27 C22 Ru1 C25 -159.76(17) . . . . ? C26 C22 Ru1 C24 -79.51(11) . . . . ? C23 C22 Ru1 C24 36.52(10) . . . . ? C27 C22 Ru1 C24 157.10(17) . . . . ? C26 C22 Ru1 C23 -116.04(14) . . . . ? C27 C22 Ru1 C23 120.58(19) . . . . ? C23 C22 Ru1 C26 116.04(14) . . . . ? C27 C22 Ru1 C26 -123.39(19) . . . . ? C26 C25 Ru1 N1 -82.04(11) . . . . ? C24 C25 Ru1 N1 160.87(9) . . . . ? C30 C25 Ru1 N1 41.93(18) . . . . ? C26 C25 Ru1 N2 157.93(10) . . . . ? C24 C25 Ru1 N2 40.84(15) . . . . ? C30 C25 Ru1 N2 -78.1(2) . . . . ? C26 C25 Ru1 C22 36.92(10) . . . . ? C24 C25 Ru1 C22 -80.16(11) . . . . ? C30 C25 Ru1 C22 160.89(19) . . . . ? C26 C25 Ru1 C24 117.09(14) . . . . ? C30 C25 Ru1 C24 -118.9(2) . . . . ? C26 C25 Ru1 C23 80.17(11) . . . . ? C24 C25 Ru1 C23 -36.92(10) . . . . ? C30 C25 Ru1 C23 -155.86(19) . . . . ? C24 C25 Ru1 C26 -117.09(14) . . . . ? C30 C25 Ru1 C26 124.0(2) . . . . ? C23 C24 Ru1 N1 -152.89(11) . . . . ? C25 C24 Ru1 N1 -34.74(16) . . . . ? C29 C24 Ru1 N1 82.8(2) . . . . ? C23 C24 Ru1 N2 86.36(10) . . . . ? C25 C24 Ru1 N2 -155.49(9) . . . . ? C29 C24 Ru1 N2 -37.95(18) . . . . ? C23 C24 Ru1 C22 -37.48(10) . . . . ? C25 C24 Ru1 C22 80.67(11) . . . . ? C29 C24 Ru1 C22 -161.79(19) . . . . ? C23 C24 Ru1 C25 -118.15(14) . . . . ? C29 C24 Ru1 C25 117.5(2) . . . . ? C25 C24 Ru1 C23 118.15(14) . . . . ? C29 C24 Ru1 C23 -124.3(2) . . . . ? C23 C24 Ru1 C26 -80.54(11) . . . . ? C25 C24 Ru1 C26 37.61(10) . . . . ? C29 C24 Ru1 C26 155.15(19) . . . . ? C24 C23 Ru1 N1 121.5(2) . . . . ? C22 C23 Ru1 N1 2.6(3) . . . . ? C28 C23 Ru1 N1 -115.6(2) . . . . ? C24 C23 Ru1 N2 -105.37(10) . . . . ? C22 C23 Ru1 N2 135.78(10) . . . . ? C28 C23 Ru1 N2 17.57(18) . . . . ? C24 C23 Ru1 C22 118.85(14) . . . . ? C28 C23 Ru1 C22 -118.2(2) . . . . ? C24 C23 Ru1 C25 37.84(10) . . . . ? C22 C23 Ru1 C25 -81.01(11) . . . . ? C28 C23 Ru1 C25 160.78(19) . . . . ? C22 C23 Ru1 C24 -118.85(14) . . . . ? C28 C23 Ru1 C24 122.9(2) . . . . ? C24 C23 Ru1 C26 80.28(11) . . . . ? C22 C23 Ru1 C26 -38.57(10) . . . . ? C28 C23 Ru1 C26 -156.78(19) . . . . ? C25 C26 Ru1 N1 110.38(10) . . . . ? C22 C26 Ru1 N1 -130.14(10) . . . . ? C31 C26 Ru1 N1 -11.13(18) . . . . ? C25 C26 Ru1 N2 -105.1(3) . . . . ? C22 C26 Ru1 N2 14.4(3) . . . . ? C31 C26 Ru1 N2 133.4(2) . . . . ? C25 C26 Ru1 C22 -119.47(14) . . . . ? C31 C26 Ru1 C22 119.0(2) . . . . ? C22 C26 Ru1 C25 119.47(14) . . . . ? C31 C26 Ru1 C25 -121.5(2) . . . . ? C25 C26 Ru1 C24 -38.37(10) . . . . ? C22 C26 Ru1 C24 81.10(11) . . . . ? C31 C26 Ru1 C24 -159.9(2) . . . . ? C25 C26 Ru1 C23 -80.66(11) . . . . ? C22 C26 Ru1 C23 38.81(10) . . . . ? C31 C26 Ru1 C23 157.82(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.347 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.052 data_adp489 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*Ru((3,5-Me2C6H3NC(CF3))2CH)' _chemical_melting_point ? _chemical_formula_moiety 'C31 H28 F12 N2 Ru, C6 H6' _chemical_formula_sum 'C37 H34 F12 N2 Ru' _chemical_formula_weight 835.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8692(7) _cell_length_b 9.2206(8) _cell_length_c 21.5339(17) _cell_angle_alpha 86.320(7) _cell_angle_beta 87.252(7) _cell_angle_gamma 85.375(7) _cell_volume 1750.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 4121 _cell_measurement_theta_min 2.8235 _cell_measurement_theta_max 26.8616 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.542 _exptl_absorpt_correction_T_min 0.98016 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ? _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Xcalibur, Sapphire2, large Be window' _diffrn_detector_area_resol_mean 8.2812 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11896 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_sigmaI/netI 0.1224 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5696 _reflns_number_gt 3848 _reflns_threshold_expression I>2/s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick G.M., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick G.M., 2008)' _computing_molecular_graphics 'ORTEP-3 for windows 2.02 (Farrugia, 2008)' _computing_publication_material 'WinGX 1.80.05 (Farrugia, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5696 _refine_ls_number_parameters 495 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6677(6) 0.1660(6) 0.6298(2) 0.0163(12) Uani 1 1 d . . . C2 C 0.7745(6) 0.1979(6) 0.5834(3) 0.0194(13) Uani 1 1 d . . . H2 H 0.8786 0.1914 0.5927 0.023 Uiso 1 1 calc R . . C3 C 0.7311(6) 0.2398(6) 0.5228(3) 0.0212(14) Uani 1 1 d . . . C4 C 0.5795(6) 0.2468(6) 0.5091(3) 0.0232(14) Uani 1 1 d . . . H4 H 0.5492 0.2738 0.4680 0.028 Uiso 1 1 calc R . . C5 C 0.4732(6) 0.2145(6) 0.5553(3) 0.0214(14) Uani 1 1 d . . . C6 C 0.5166(6) 0.1738(6) 0.6151(3) 0.0189(13) Uani 1 1 d . . . H6 H 0.4420 0.1509 0.6466 0.023 Uiso 1 1 calc R . . C7 C 0.8498(7) 0.2734(8) 0.4738(3) 0.0344(18) Uani 1 1 d . . . C8 C 0.3107(7) 0.2212(8) 0.5404(3) 0.0311(16) Uani 1 1 d . . . C9 C 0.7378(6) -0.0243(6) 0.7025(3) 0.0202(13) Uani 1 1 d . . . C10 C 0.7167(7) -0.1237(6) 0.6511(3) 0.0301(15) Uani 1 1 d . . . H10A H 0.6139 -0.1050 0.6361 0.045 Uiso 1 1 calc R . . H10B H 0.7320 -0.2255 0.6671 0.045 Uiso 1 1 calc R . . H10C H 0.7904 -0.1052 0.6167 0.045 Uiso 1 1 calc R . . C11 C 0.7846(6) -0.0886(6) 0.7583(3) 0.0219(14) Uani 1 1 d . . . H11 H 0.7990 -0.1919 0.7605 0.026 Uiso 1 1 calc R . . C12 C 0.8135(6) -0.0217(6) 0.8119(3) 0.0208(14) Uani 1 1 d . . . C13 C 0.8740(8) -0.1187(6) 0.8664(3) 0.0393(18) Uani 1 1 d . . . H13A H 0.9755 -0.0926 0.8751 0.059 Uiso 1 1 calc R . . H13B H 0.8791 -0.2209 0.8559 0.059 Uiso 1 1 calc R . . H13C H 0.8065 -0.1051 0.9033 0.059 Uiso 1 1 calc R . . C14 C 0.8246(6) 0.1705(6) 0.8770(2) 0.0178(13) Uani 1 1 d . . . C15 C 0.9683(6) 0.2094(6) 0.8881(3) 0.0219(14) Uani 1 1 d . . . H15 H 1.0449 0.2062 0.8558 0.026 Uiso 1 1 calc R . . C16 C 1.0014(7) 0.2529(7) 0.9464(3) 0.0278(15) Uani 1 1 d . A . C17 C 0.8914(7) 0.2586(6) 0.9936(3) 0.0274(15) Uani 1 1 d . . . H17 H 0.9132 0.2899 1.0332 0.033 Uiso 1 1 calc R . . C18 C 0.7489(7) 0.2184(7) 0.9827(3) 0.0281(15) Uani 1 1 d . . . C19 C 0.7144(6) 0.1759(6) 0.9248(3) 0.0237(14) Uani 1 1 d . . . H19 H 0.6152 0.1503 0.9179 0.028 Uiso 1 1 calc R . . C20 C 1.1571(8) 0.2944(9) 0.9555(3) 0.0420(19) Uani 1 1 d D . . C21 C 0.6273(9) 0.2281(10) 1.0334(3) 0.049(2) Uani 1 1 d . . . C22 C 0.5835(6) 0.4728(5) 0.7627(3) 0.0175(13) Uani 1 1 d . . . C23 C 0.6392(7) 0.4801(6) 0.6985(3) 0.0190(14) Uani 1 1 d U . . C24 C 0.7962(6) 0.4801(6) 0.6991(3) 0.0187(13) Uani 1 1 d . . . C25 C 0.8398(6) 0.4826(6) 0.7634(3) 0.0206(14) Uani 1 1 d . . . C26 C 0.7085(7) 0.4830(6) 0.8018(3) 0.0204(14) Uani 1 1 d . . . C27 C 0.4198(7) 0.4717(6) 0.7842(3) 0.0314(16) Uani 1 1 d . . . H27A H 0.4115 0.4124 0.8235 0.047 Uiso 1 1 calc R . . H27B H 0.3629 0.4304 0.7526 0.047 Uiso 1 1 calc R . . H27C H 0.3783 0.5717 0.7906 0.047 Uiso 1 1 calc R . . C28 C 0.5418(7) 0.5046(6) 0.6431(3) 0.0292(15) Uani 1 1 d . . . H28A H 0.5083 0.6083 0.6375 0.044 Uiso 1 1 calc R . . H28B H 0.4532 0.4475 0.6498 0.044 Uiso 1 1 calc R . . H28C H 0.6002 0.4738 0.6058 0.044 Uiso 1 1 calc R . . C29 C 0.9066(7) 0.4944(6) 0.6442(3) 0.0326(16) Uani 1 1 d . . . H29A H 0.8579 0.4732 0.6063 0.049 Uiso 1 1 calc R . . H29B H 0.9951 0.4253 0.6507 0.049 Uiso 1 1 calc R . . H29C H 0.9386 0.5939 0.6400 0.049 Uiso 1 1 calc R . . C30 C 0.9987(7) 0.4995(6) 0.7814(3) 0.0316(16) Uani 1 1 d . . . H30A H 1.0061 0.4787 0.8264 0.047 Uiso 1 1 calc R . . H30B H 1.0245 0.5995 0.7704 0.047 Uiso 1 1 calc R . . H30C H 1.0690 0.4312 0.7592 0.047 Uiso 1 1 calc R . . C31 C 0.6898(7) 0.5104(7) 0.8701(3) 0.0316(16) Uani 1 1 d . . . H31A H 0.7856 0.4827 0.8902 0.047 Uiso 1 1 calc R . . H31B H 0.6106 0.4522 0.8895 0.047 Uiso 1 1 calc R . . H31C H 0.6611 0.6140 0.8750 0.047 Uiso 1 1 calc R . . C32 C 0.2650(8) 0.1094(8) 0.7647(3) 0.047(2) Uani 1 1 d . . . H32 H 0.2615 0.1999 0.7837 0.056 Uiso 1 1 calc R . . C33 C 0.3812(8) 0.0026(9) 0.7768(3) 0.0446(19) Uani 1 1 d . . . H33 H 0.4573 0.0200 0.8043 0.054 Uiso 1 1 calc R . . C34 C 0.3869(8) -0.1258(8) 0.7497(4) 0.0444(19) Uani 1 1 d . . . H34 H 0.4674 -0.1978 0.7578 0.053 Uiso 1 1 calc R . . C35 C 0.2759(8) -0.1524(8) 0.7102(4) 0.0463(19) Uani 1 1 d . . . H35 H 0.2790 -0.2434 0.6917 0.056 Uiso 1 1 calc R . . C36 C 0.1606(8) -0.0471(9) 0.6975(3) 0.048(2) Uani 1 1 d . . . H36 H 0.0854 -0.0653 0.6697 0.058 Uiso 1 1 calc R . . C37 C 0.1538(8) 0.0818(8) 0.7244(4) 0.048(2) Uani 1 1 d . . . H37 H 0.0732 0.1535 0.7159 0.057 Uiso 1 1 calc R . . N1 N 0.7147(5) 0.1219(5) 0.6915(2) 0.0183(11) Uani 1 1 d . . . N2 N 0.7914(5) 0.1239(5) 0.8171(2) 0.0173(11) Uani 1 1 d . . . F1 F 0.9426(5) 0.3649(5) 0.49057(17) 0.0611(13) Uani 1 1 d . . . F2 F 0.7936(5) 0.3276(6) 0.42157(19) 0.0867(19) Uani 1 1 d . . . F3 F 0.9377(6) 0.1582(5) 0.4588(2) 0.0816(17) Uani 1 1 d . . . F4 F 0.2209(4) 0.2755(6) 0.58408(19) 0.0709(15) Uani 1 1 d . . . F5 F 0.2796(4) 0.2978(6) 0.4884(2) 0.0774(16) Uani 1 1 d . . . F6 F 0.2636(5) 0.0931(5) 0.5329(3) 0.103(2) Uani 1 1 d . . . F7A F 1.2468(14) 0.1693(15) 0.9652(13) 0.075(6) Uani 0.62(4) 1 d PD A 1 F8A F 1.210(2) 0.368(3) 0.9132(6) 0.087(9) Uani 0.62(4) 1 d PD A 1 F7B F 1.2724(14) 0.228(3) 0.9264(14) 0.056(9) Uani 0.38(4) 1 d PD A 2 F8B F 1.175(3) 0.441(3) 0.9202(13) 0.054(6) Uani 0.38(4) 1 d PD A 2 F9 F 1.1709(5) 0.3469(5) 1.01013(18) 0.0638(14) Uani 1 1 d D A . F10 F 0.6731(5) 0.2541(8) 1.0871(2) 0.108(2) Uani 1 1 d . . . F11 F 0.5508(6) 0.1129(6) 1.0406(2) 0.097(2) Uani 1 1 d . . . F12 F 0.5217(6) 0.3339(6) 1.0200(2) 0.0922(19) Uani 1 1 d . . . Ru1 Ru 0.73336(6) 0.28381(5) 0.75031(2) 0.01518(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(3) 0.012(3) 0.015(3) -0.005(3) -0.005(2) -0.002(2) C2 0.012(3) 0.023(3) 0.023(3) -0.004(3) -0.002(2) -0.001(2) C3 0.025(4) 0.021(4) 0.019(3) -0.007(3) 0.000(3) -0.003(3) C4 0.023(4) 0.028(4) 0.019(3) -0.003(3) -0.002(3) 0.002(3) C5 0.020(3) 0.022(3) 0.023(3) -0.003(3) 0.002(3) -0.007(3) C6 0.018(3) 0.018(3) 0.020(3) -0.002(3) 0.006(2) -0.005(2) C7 0.020(4) 0.061(5) 0.023(4) 0.006(4) -0.001(3) -0.012(3) C8 0.026(4) 0.039(4) 0.027(4) 0.000(4) 0.000(3) 0.002(3) C9 0.020(3) 0.016(3) 0.025(3) -0.010(3) 0.000(3) 0.001(2) C10 0.048(4) 0.014(3) 0.029(4) -0.007(3) -0.006(3) -0.001(3) C11 0.028(4) 0.013(3) 0.025(3) -0.003(3) -0.003(3) 0.002(2) C12 0.021(3) 0.016(3) 0.025(3) 0.000(3) -0.005(3) -0.002(2) C13 0.069(5) 0.019(4) 0.030(4) 0.002(3) -0.014(3) 0.006(3) C14 0.028(4) 0.011(3) 0.014(3) 0.000(3) -0.002(2) 0.002(2) C15 0.025(4) 0.023(4) 0.017(3) 0.002(3) 0.000(3) 0.000(3) C16 0.034(4) 0.029(4) 0.021(3) 0.000(3) -0.003(3) -0.005(3) C17 0.040(4) 0.028(4) 0.015(3) -0.003(3) -0.006(3) 0.000(3) C18 0.029(4) 0.030(4) 0.024(4) 0.000(3) -0.003(3) 0.002(3) C19 0.019(3) 0.028(4) 0.024(3) 0.002(3) -0.001(3) -0.005(3) C20 0.031(4) 0.066(6) 0.031(4) -0.010(4) -0.011(3) -0.005(4) C21 0.048(5) 0.071(6) 0.025(4) -0.002(4) 0.010(4) -0.002(5) C22 0.021(3) 0.009(3) 0.022(3) -0.002(3) 0.002(2) -0.001(2) C23 0.034(4) 0.003(3) 0.021(3) -0.002(3) -0.009(3) -0.001(2) C24 0.022(3) 0.008(3) 0.025(3) -0.001(3) 0.008(3) 0.000(2) C25 0.028(4) 0.005(3) 0.029(3) -0.003(3) -0.003(3) 0.000(2) C26 0.034(4) 0.004(3) 0.023(3) -0.001(3) 0.006(3) -0.001(2) C27 0.029(4) 0.019(4) 0.044(4) 0.001(3) 0.010(3) 0.000(3) C28 0.040(4) 0.020(3) 0.027(4) -0.002(3) -0.008(3) 0.006(3) C29 0.046(4) 0.020(4) 0.031(4) -0.004(3) 0.015(3) -0.003(3) C30 0.030(4) 0.021(4) 0.043(4) -0.001(3) -0.006(3) 0.000(3) C31 0.047(4) 0.025(4) 0.022(4) -0.004(3) 0.000(3) 0.001(3) C32 0.047(5) 0.046(5) 0.049(5) -0.019(4) 0.030(4) -0.023(4) C33 0.038(5) 0.065(6) 0.034(4) -0.004(4) 0.001(3) -0.021(4) C34 0.044(5) 0.030(4) 0.059(5) 0.006(4) -0.001(4) -0.005(3) C35 0.045(5) 0.033(4) 0.062(5) -0.020(4) 0.007(4) -0.002(3) C36 0.038(5) 0.071(6) 0.038(5) -0.014(4) 0.007(3) -0.010(4) C37 0.041(5) 0.045(5) 0.052(5) 0.001(4) 0.019(4) 0.011(4) N1 0.014(3) 0.019(3) 0.022(3) -0.002(2) -0.002(2) -0.0023(19) N2 0.020(3) 0.017(3) 0.016(3) -0.003(2) -0.004(2) 0.000(2) F1 0.057(3) 0.099(4) 0.034(2) -0.013(2) 0.014(2) -0.051(3) F2 0.044(3) 0.187(6) 0.026(3) 0.043(3) 0.001(2) -0.028(3) F3 0.075(4) 0.075(4) 0.089(4) -0.007(3) 0.061(3) -0.001(3) F4 0.020(2) 0.148(5) 0.043(3) -0.030(3) -0.0017(18) 0.023(3) F5 0.027(2) 0.146(5) 0.053(3) 0.048(3) -0.013(2) -0.004(3) F6 0.048(3) 0.065(4) 0.205(7) -0.017(4) -0.058(4) -0.017(2) F7A 0.027(6) 0.069(7) 0.132(15) -0.019(9) -0.028(7) 0.007(4) F8A 0.043(10) 0.18(2) 0.041(7) 0.056(12) -0.015(6) -0.069(14) F7B 0.022(7) 0.072(17) 0.080(19) -0.048(14) -0.001(8) 0.002(8) F8B 0.053(12) 0.053(13) 0.057(10) 0.015(9) -0.022(8) -0.018(8) F9 0.065(3) 0.105(4) 0.029(2) -0.017(2) -0.011(2) -0.040(3) F10 0.061(3) 0.247(7) 0.024(3) -0.042(3) 0.009(2) -0.046(4) F11 0.118(5) 0.088(4) 0.086(4) -0.030(3) 0.071(4) -0.051(3) F12 0.085(4) 0.113(5) 0.067(4) 0.006(3) 0.040(3) 0.031(3) Ru1 0.0185(3) 0.0130(3) 0.0139(2) -0.00081(19) -0.00005(17) -0.00059(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.378(7) . ? C1 C6 1.386(7) . ? C1 N1 1.436(7) . ? C2 C3 1.402(7) . ? C2 H2 0.9500 . ? C3 C4 1.385(7) . ? C3 C7 1.490(8) . ? C4 C5 1.373(8) . ? C4 H4 0.9500 . ? C5 C6 1.382(7) . ? C5 C8 1.487(8) . ? C6 H6 0.9500 . ? C7 F1 1.304(7) . ? C7 F2 1.306(7) . ? C7 F3 1.314(8) . ? C8 F4 1.302(7) . ? C8 F6 1.307(8) . ? C8 F5 1.313(7) . ? C9 N1 1.354(7) . ? C9 C11 1.373(7) . ? C9 C10 1.510(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.387(8) . ? C11 H11 0.9500 . ? C12 N2 1.352(7) . ? C12 C13 1.521(7) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.386(7) . ? C14 C15 1.387(7) . ? C14 N2 1.436(7) . ? C15 C16 1.393(8) . ? C15 H15 0.9500 . ? C16 C17 1.376(8) . ? C16 C20 1.487(9) . ? C17 C18 1.381(8) . ? C17 H17 0.9500 . ? C18 C19 1.386(8) . ? C18 C21 1.498(9) . ? C19 H19 0.9500 . ? C20 F8A 1.203(14) . ? C20 F7B 1.305(13) . ? C20 F9 1.315(8) . ? C20 F7A 1.358(11) . ? C20 F8B 1.53(2) . ? C21 F10 1.287(8) . ? C21 F11 1.303(9) . ? C21 F12 1.324(9) . ? C22 C26 1.437(8) . ? C22 C23 1.445(8) . ? C22 C27 1.503(8) . ? C22 Ru1 2.128(5) . ? C23 C24 1.393(7) . ? C23 C28 1.501(7) . ? C23 Ru1 2.192(5) . ? C24 C25 1.457(8) . ? C24 C29 1.504(7) . ? C24 Ru1 2.157(5) . ? C25 C26 1.396(8) . ? C25 C30 1.501(8) . ? C25 Ru1 2.169(5) . ? C26 C31 1.507(8) . ? C26 Ru1 2.196(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.388(10) . ? C32 C37 1.394(10) . ? C32 H32 0.9500 . ? C33 C34 1.349(9) . ? C33 H33 0.9500 . ? C34 C35 1.377(10) . ? C34 H34 0.9500 . ? C35 C36 1.376(10) . ? C35 H35 0.9500 . ? C36 C37 1.351(10) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? N1 Ru1 2.040(5) . ? N2 Ru1 2.045(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.8(5) . . ? C2 C1 N1 119.7(5) . . ? C6 C1 N1 121.4(5) . . ? C1 C2 C3 120.6(5) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 119.6(5) . . ? C4 C3 C7 121.3(5) . . ? C2 C3 C7 119.1(5) . . ? C5 C4 C3 119.7(5) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.4(5) . . ? C4 C5 C8 119.5(5) . . ? C6 C5 C8 120.0(5) . . ? C5 C6 C1 120.8(5) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? F1 C7 F2 107.0(6) . . ? F1 C7 F3 104.5(6) . . ? F2 C7 F3 105.2(6) . . ? F1 C7 C3 113.2(6) . . ? F2 C7 C3 112.9(5) . . ? F3 C7 C3 113.2(6) . . ? F4 C8 F6 105.0(6) . . ? F4 C8 F5 107.0(6) . . ? F6 C8 F5 104.7(6) . . ? F4 C8 C5 113.0(6) . . ? F6 C8 C5 112.9(5) . . ? F5 C8 C5 113.6(5) . . ? N1 C9 C11 123.1(5) . . ? N1 C9 C10 119.6(5) . . ? C11 C9 C10 117.2(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C12 128.2(5) . . ? C9 C11 H11 115.9 . . ? C12 C11 H11 115.9 . . ? N2 C12 C11 122.9(5) . . ? N2 C12 C13 119.6(5) . . ? C11 C12 C13 117.4(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 118.8(5) . . ? C19 C14 N2 120.7(5) . . ? C15 C14 N2 120.5(5) . . ? C14 C15 C16 120.6(5) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 120.3(6) . . ? C17 C16 C20 121.5(6) . . ? C15 C16 C20 118.2(6) . . ? C16 C17 C18 119.1(6) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C17 C18 C19 121.1(6) . . ? C17 C18 C21 119.4(6) . . ? C19 C18 C21 119.4(6) . . ? C14 C19 C18 120.1(5) . . ? C14 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? F8A C20 F7B 66.9(10) . . ? F8A C20 F9 112.8(13) . . ? F7B C20 F9 121.1(10) . . ? F8A C20 F7A 109.9(10) . . ? F7B C20 F7A 43.7(9) . . ? F9 C20 F7A 97.4(9) . . ? F8A C20 C16 114.9(9) . . ? F7B C20 C16 119.7(9) . . ? F9 C20 C16 112.8(6) . . ? F7A C20 C16 107.4(8) . . ? F8A C20 F8B 28.4(15) . . ? F7B C20 F8B 94.5(14) . . ? F9 C20 F8B 93.3(13) . . ? F7A C20 F8B 135.4(12) . . ? C16 C20 F8B 107.8(12) . . ? F10 C21 F11 107.6(7) . . ? F10 C21 F12 105.5(8) . . ? F11 C21 F12 103.0(7) . . ? F10 C21 C18 114.9(7) . . ? F11 C21 C18 113.5(7) . . ? F12 C21 C18 111.4(6) . . ? C26 C22 C23 108.5(5) . . ? C26 C22 C27 125.8(5) . . ? C23 C22 C27 125.4(5) . . ? C26 C22 Ru1 73.2(3) . . ? C23 C22 Ru1 72.9(3) . . ? C27 C22 Ru1 125.0(4) . . ? C24 C23 C22 107.0(5) . . ? C24 C23 C28 127.5(5) . . ? C22 C23 C28 125.0(5) . . ? C24 C23 Ru1 70.0(3) . . ? C22 C23 Ru1 68.1(3) . . ? C28 C23 Ru1 133.3(4) . . ? C23 C24 C25 108.7(5) . . ? C23 C24 C29 127.8(5) . . ? C25 C24 C29 123.0(5) . . ? C23 C24 Ru1 72.7(3) . . ? C25 C24 Ru1 70.8(3) . . ? C29 C24 Ru1 128.2(4) . . ? C26 C25 C24 108.1(5) . . ? C26 C25 C30 128.0(6) . . ? C24 C25 C30 123.5(5) . . ? C26 C25 Ru1 72.4(3) . . ? C24 C25 Ru1 69.9(3) . . ? C30 C25 Ru1 128.5(4) . . ? C25 C26 C22 107.4(5) . . ? C25 C26 C31 128.5(6) . . ? C22 C26 C31 123.5(5) . . ? C25 C26 Ru1 70.3(3) . . ? C22 C26 Ru1 68.0(3) . . ? C31 C26 Ru1 133.3(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 119.0(7) . . ? C33 C32 H32 120.5 . . ? C37 C32 H32 120.5 . . ? C34 C33 C32 120.6(7) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 120.0(7) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.0(8) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C35 120.5(8) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C32 119.9(7) . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C9 N1 C1 114.1(5) . . ? C9 N1 Ru1 129.2(4) . . ? C1 N1 Ru1 116.8(3) . . ? C12 N2 C14 114.1(4) . . ? C12 N2 Ru1 128.9(4) . . ? C14 N2 Ru1 116.8(3) . . ? N1 Ru1 N2 87.36(18) . . ? N1 Ru1 C22 127.96(19) . . ? N2 Ru1 C22 126.5(2) . . ? N1 Ru1 C24 110.7(2) . . ? N2 Ru1 C24 146.5(2) . . ? C22 Ru1 C24 64.3(2) . . ? N1 Ru1 C25 145.0(2) . . ? N2 Ru1 C25 111.6(2) . . ? C22 Ru1 C25 64.2(2) . . ? C24 Ru1 C25 39.4(2) . . ? N1 Ru1 C23 103.65(19) . . ? N2 Ru1 C23 165.54(19) . . ? C22 Ru1 C23 39.0(2) . . ? C24 Ru1 C23 37.3(2) . . ? C25 Ru1 C23 64.2(2) . . ? N1 Ru1 C26 166.56(19) . . ? N2 Ru1 C26 103.50(19) . . ? C22 Ru1 C26 38.8(2) . . ? C24 Ru1 C26 64.1(2) . . ? C25 Ru1 C26 37.3(2) . . ? C23 Ru1 C26 64.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.1(8) . . . . ? N1 C1 C2 C3 179.4(5) . . . . ? C1 C2 C3 C4 -1.1(8) . . . . ? C1 C2 C3 C7 -180.0(6) . . . . ? C2 C3 C4 C5 0.9(8) . . . . ? C7 C3 C4 C5 179.7(6) . . . . ? C3 C4 C5 C6 -0.6(9) . . . . ? C3 C4 C5 C8 -179.6(5) . . . . ? C4 C5 C6 C1 0.6(9) . . . . ? C8 C5 C6 C1 179.6(5) . . . . ? C2 C1 C6 C5 -0.8(8) . . . . ? N1 C1 C6 C5 -179.1(5) . . . . ? C4 C3 C7 F1 130.7(6) . . . . ? C2 C3 C7 F1 -50.5(8) . . . . ? C4 C3 C7 F2 8.9(9) . . . . ? C2 C3 C7 F2 -172.2(6) . . . . ? C4 C3 C7 F3 -110.5(7) . . . . ? C2 C3 C7 F3 68.3(8) . . . . ? C4 C5 C8 F4 -140.7(6) . . . . ? C6 C5 C8 F4 40.2(8) . . . . ? C4 C5 C8 F6 100.3(7) . . . . ? C6 C5 C8 F6 -78.8(8) . . . . ? C4 C5 C8 F5 -18.7(9) . . . . ? C6 C5 C8 F5 162.3(6) . . . . ? N1 C9 C11 C12 1.1(10) . . . . ? C10 C9 C11 C12 179.2(6) . . . . ? C9 C11 C12 N2 3.2(10) . . . . ? C9 C11 C12 C13 -176.2(6) . . . . ? C19 C14 C15 C16 0.0(8) . . . . ? N2 C14 C15 C16 -179.2(5) . . . . ? C14 C15 C16 C17 -0.3(9) . . . . ? C14 C15 C16 C20 -179.5(5) . . . . ? C15 C16 C17 C18 1.1(9) . . . . ? C20 C16 C17 C18 -179.8(6) . . . . ? C16 C17 C18 C19 -1.6(9) . . . . ? C16 C17 C18 C21 -178.4(6) . . . . ? C15 C14 C19 C18 -0.5(8) . . . . ? N2 C14 C19 C18 178.7(5) . . . . ? C17 C18 C19 C14 1.2(9) . . . . ? C21 C18 C19 C14 178.1(6) . . . . ? C17 C16 C20 F8A -136.6(18) . . . . ? C15 C16 C20 F8A 42.6(19) . . . . ? C17 C16 C20 F7B 147(2) . . . . ? C15 C16 C20 F7B -34(2) . . . . ? C17 C16 C20 F9 -5.4(10) . . . . ? C15 C16 C20 F9 173.8(6) . . . . ? C17 C16 C20 F7A 100.8(14) . . . . ? C15 C16 C20 F7A -80.1(13) . . . . ? C17 C16 C20 F8B -106.9(13) . . . . ? C15 C16 C20 F8B 72.2(13) . . . . ? C17 C18 C21 F10 -9.8(11) . . . . ? C19 C18 C21 F10 173.3(7) . . . . ? C17 C18 C21 F11 -134.2(7) . . . . ? C19 C18 C21 F11 48.9(9) . . . . ? C17 C18 C21 F12 110.1(8) . . . . ? C19 C18 C21 F12 -66.7(9) . . . . ? C26 C22 C23 C24 5.6(6) . . . . ? C27 C22 C23 C24 179.4(5) . . . . ? Ru1 C22 C23 C24 -59.4(4) . . . . ? C26 C22 C23 C28 -166.5(5) . . . . ? C27 C22 C23 C28 7.2(9) . . . . ? Ru1 C22 C23 C28 128.4(5) . . . . ? C26 C22 C23 Ru1 65.0(4) . . . . ? C27 C22 C23 Ru1 -121.2(5) . . . . ? C22 C23 C24 C25 -3.7(6) . . . . ? C28 C23 C24 C25 168.2(5) . . . . ? Ru1 C23 C24 C25 -61.9(4) . . . . ? C22 C23 C24 C29 -176.5(5) . . . . ? C28 C23 C24 C29 -4.6(9) . . . . ? Ru1 C23 C24 C29 125.3(6) . . . . ? C22 C23 C24 Ru1 58.2(3) . . . . ? C28 C23 C24 Ru1 -129.9(6) . . . . ? C23 C24 C25 C26 0.4(6) . . . . ? C29 C24 C25 C26 173.6(5) . . . . ? Ru1 C24 C25 C26 -62.7(4) . . . . ? C23 C24 C25 C30 -173.2(5) . . . . ? C29 C24 C25 C30 -0.1(8) . . . . ? Ru1 C24 C25 C30 123.6(5) . . . . ? C23 C24 C25 Ru1 63.2(4) . . . . ? C29 C24 C25 Ru1 -123.6(5) . . . . ? C24 C25 C26 C22 3.1(6) . . . . ? C30 C25 C26 C22 176.4(5) . . . . ? Ru1 C25 C26 C22 -58.0(4) . . . . ? C24 C25 C26 C31 -168.7(5) . . . . ? C30 C25 C26 C31 4.6(9) . . . . ? Ru1 C25 C26 C31 130.2(6) . . . . ? C24 C25 C26 Ru1 61.1(4) . . . . ? C30 C25 C26 Ru1 -125.6(5) . . . . ? C23 C22 C26 C25 -5.4(6) . . . . ? C27 C22 C26 C25 -179.1(5) . . . . ? Ru1 C22 C26 C25 59.4(4) . . . . ? C23 C22 C26 C31 166.9(5) . . . . ? C27 C22 C26 C31 -6.8(8) . . . . ? Ru1 C22 C26 C31 -128.3(5) . . . . ? C23 C22 C26 Ru1 -64.8(4) . . . . ? C27 C22 C26 Ru1 121.5(5) . . . . ? C37 C32 C33 C34 0.3(10) . . . . ? C32 C33 C34 C35 -0.7(10) . . . . ? C33 C34 C35 C36 1.1(11) . . . . ? C34 C35 C36 C37 -1.2(11) . . . . ? C35 C36 C37 C32 0.8(10) . . . . ? C33 C32 C37 C36 -0.4(10) . . . . ? C11 C9 N1 C1 179.3(5) . . . . ? C10 C9 N1 C1 1.3(7) . . . . ? C11 C9 N1 Ru1 -2.0(8) . . . . ? C10 C9 N1 Ru1 180.0(4) . . . . ? C2 C1 N1 C9 -92.6(6) . . . . ? C6 C1 N1 C9 85.7(6) . . . . ? C2 C1 N1 Ru1 88.6(5) . . . . ? C6 C1 N1 Ru1 -93.2(5) . . . . ? C11 C12 N2 C14 178.5(5) . . . . ? C13 C12 N2 C14 -2.1(7) . . . . ? C11 C12 N2 Ru1 -6.4(8) . . . . ? C13 C12 N2 Ru1 173.0(4) . . . . ? C19 C14 N2 C12 -88.0(6) . . . . ? C15 C14 N2 C12 91.2(6) . . . . ? C19 C14 N2 Ru1 96.3(5) . . . . ? C15 C14 N2 Ru1 -84.6(5) . . . . ? C9 N1 Ru1 N2 -0.3(5) . . . . ? C1 N1 Ru1 N2 178.3(4) . . . . ? C9 N1 Ru1 C22 -136.4(4) . . . . ? C1 N1 Ru1 C22 42.3(4) . . . . ? C9 N1 Ru1 C24 150.6(5) . . . . ? C1 N1 Ru1 C24 -30.7(4) . . . . ? C9 N1 Ru1 C25 124.9(5) . . . . ? C1 N1 Ru1 C25 -56.5(5) . . . . ? C9 N1 Ru1 C23 -170.9(5) . . . . ? C1 N1 Ru1 C23 7.8(4) . . . . ? C9 N1 Ru1 C26 -144.6(7) . . . . ? C1 N1 Ru1 C26 34.0(10) . . . . ? C12 N2 Ru1 N1 4.4(5) . . . . ? C14 N2 Ru1 N1 179.4(4) . . . . ? C12 N2 Ru1 C22 141.5(4) . . . . ? C14 N2 Ru1 C22 -43.5(5) . . . . ? C12 N2 Ru1 C24 -120.4(5) . . . . ? C14 N2 Ru1 C24 54.6(5) . . . . ? C12 N2 Ru1 C25 -145.3(5) . . . . ? C14 N2 Ru1 C25 29.7(4) . . . . ? C12 N2 Ru1 C23 144.6(7) . . . . ? C14 N2 Ru1 C23 -40.4(10) . . . . ? C12 N2 Ru1 C26 176.4(5) . . . . ? C14 N2 Ru1 C26 -8.6(4) . . . . ? C26 C22 Ru1 N1 -176.9(3) . . . . ? C23 C22 Ru1 N1 -60.9(4) . . . . ? C27 C22 Ru1 N1 60.8(6) . . . . ? C26 C22 Ru1 N2 62.7(4) . . . . ? C23 C22 Ru1 N2 178.8(3) . . . . ? C27 C22 Ru1 N2 -59.6(6) . . . . ? C26 C22 Ru1 C24 -79.9(3) . . . . ? C23 C22 Ru1 C24 36.2(3) . . . . ? C27 C22 Ru1 C24 157.8(6) . . . . ? C26 C22 Ru1 C25 -36.0(3) . . . . ? C23 C22 Ru1 C25 80.1(3) . . . . ? C27 C22 Ru1 C25 -158.3(6) . . . . ? C26 C22 Ru1 C23 -116.1(4) . . . . ? C27 C22 Ru1 C23 121.6(6) . . . . ? C23 C22 Ru1 C26 116.1(4) . . . . ? C27 C22 Ru1 C26 -122.3(6) . . . . ? C23 C24 Ru1 N1 85.4(3) . . . . ? C25 C24 Ru1 N1 -156.8(3) . . . . ? C29 C24 Ru1 N1 -39.5(6) . . . . ? C23 C24 Ru1 N2 -155.8(3) . . . . ? C25 C24 Ru1 N2 -38.1(5) . . . . ? C29 C24 Ru1 N2 79.3(7) . . . . ? C23 C24 Ru1 C22 -37.8(3) . . . . ? C25 C24 Ru1 C22 79.9(3) . . . . ? C29 C24 Ru1 C22 -162.7(6) . . . . ? C23 C24 Ru1 C25 -117.7(5) . . . . ? C29 C24 Ru1 C25 117.4(7) . . . . ? C25 C24 Ru1 C23 117.7(5) . . . . ? C29 C24 Ru1 C23 -124.9(7) . . . . ? C23 C24 Ru1 C26 -81.0(4) . . . . ? C25 C24 Ru1 C26 36.7(3) . . . . ? C29 C24 Ru1 C26 154.1(6) . . . . ? C26 C25 Ru1 N1 157.4(3) . . . . ? C24 C25 Ru1 N1 39.9(5) . . . . ? C30 C25 Ru1 N1 -77.5(6) . . . . ? C26 C25 Ru1 N2 -83.9(3) . . . . ? C24 C25 Ru1 N2 158.5(3) . . . . ? C30 C25 Ru1 N2 41.1(6) . . . . ? C26 C25 Ru1 C22 37.4(3) . . . . ? C24 C25 Ru1 C22 -80.2(3) . . . . ? C30 C25 Ru1 C22 162.4(6) . . . . ? C26 C25 Ru1 C24 117.6(5) . . . . ? C30 C25 Ru1 C24 -117.4(7) . . . . ? C26 C25 Ru1 C23 80.9(4) . . . . ? C24 C25 Ru1 C23 -36.6(3) . . . . ? C30 C25 Ru1 C23 -154.0(6) . . . . ? C24 C25 Ru1 C26 -117.6(5) . . . . ? C30 C25 Ru1 C26 125.0(7) . . . . ? C24 C23 Ru1 N1 -106.4(3) . . . . ? C22 C23 Ru1 N1 134.9(3) . . . . ? C28 C23 Ru1 N1 16.8(6) . . . . ? C24 C23 Ru1 N2 114.9(8) . . . . ? C22 C23 Ru1 N2 -3.9(9) . . . . ? C28 C23 Ru1 N2 -122.0(8) . . . . ? C24 C23 Ru1 C22 118.8(5) . . . . ? C28 C23 Ru1 C22 -118.1(7) . . . . ? C22 C23 Ru1 C24 -118.8(5) . . . . ? C28 C23 Ru1 C24 123.1(7) . . . . ? C24 C23 Ru1 C25 38.6(3) . . . . ? C22 C23 Ru1 C25 -80.2(3) . . . . ? C28 C23 Ru1 C25 161.7(7) . . . . ? C24 C23 Ru1 C26 80.2(4) . . . . ? C22 C23 Ru1 C26 -38.6(3) . . . . ? C28 C23 Ru1 C26 -156.7(7) . . . . ? C25 C26 Ru1 N1 -108.8(8) . . . . ? C22 C26 Ru1 N1 10.4(10) . . . . ? C31 C26 Ru1 N1 126.4(8) . . . . ? C25 C26 Ru1 N2 108.1(3) . . . . ? C22 C26 Ru1 N2 -132.7(3) . . . . ? C31 C26 Ru1 N2 -16.8(6) . . . . ? C25 C26 Ru1 C22 -119.2(5) . . . . ? C31 C26 Ru1 C22 115.9(7) . . . . ? C25 C26 Ru1 C24 -38.7(3) . . . . ? C22 C26 Ru1 C24 80.5(3) . . . . ? C31 C26 Ru1 C24 -163.6(7) . . . . ? C22 C26 Ru1 C25 119.2(5) . . . . ? C31 C26 Ru1 C25 -124.9(7) . . . . ? C25 C26 Ru1 C23 -80.3(3) . . . . ? C22 C26 Ru1 C23 38.9(3) . . . . ? C31 C26 Ru1 C23 154.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 0.992 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.109 data_adp492 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'CpRu((3,5-(CH3)2C6H3NC(CF3))2CH)' _chemical_melting_point ? _chemical_formula_moiety 'C31 H34 F6 N2 Ru, C6 H6' _chemical_formula_sum 'C37 H40 F6 N2 Ru' _chemical_formula_weight 727.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8077(10) _cell_length_b 11.4136(8) _cell_length_c 16.3247(15) _cell_angle_alpha 105.494(6) _cell_angle_beta 97.740(7) _cell_angle_gamma 105.622(9) _cell_volume 1653.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 172 _cell_measurement_theta_min 4.504 _cell_measurement_theta_max 22.567 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.568 _exptl_crystal_size_mid 0.225 _exptl_crystal_size_min 0.160 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.537 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.870118 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Bruker Nonius Area Dector Scaling and Absorption Correction SADABS 2.10 (Bruker, 2003) based on an algorithm described by R.H. Blessing, Acta Cryst. (1995), a51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonus KappaCCD with \k-goniostat' _diffrn_detector 'Apex II 95mm CCD camera' _diffrn_measurement_method 'sequential \f and \w scans' _diffrn_source 'Enraf Nonius FR590' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31566 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5820 _reflns_number_gt 5429 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'Collect (Hooft, R.W.W., 1998. Nonius B.V., 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg A.J.M., Nonius B.V., 1989-2000)' _computing_data_reduction 'EvalCCD (Hooft R.W.W., Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick G.M., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick G.M., 2008)' _computing_molecular_graphics 'ORTEP-3 for windows 2.02 (Farrugia, 2008)' _computing_publication_material 'WinGX 1.80.05 (Farrugia, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+1.9262P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5820 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0551 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3824(2) 0.59752(18) 0.67206(13) 0.0132(4) Uani 1 1 d . . . C2 C 0.3577(2) 0.52582(19) 0.58447(14) 0.0165(4) Uani 1 1 d . . . H2 H 0.4360 0.5324 0.5556 0.020 Uiso 1 1 calc R . . C3 C 0.2185(2) 0.44439(19) 0.53891(14) 0.0195(5) Uani 1 1 d . . . C4 C 0.1054(2) 0.43674(19) 0.58300(15) 0.0210(5) Uani 1 1 d . . . H4 H 0.0104 0.3817 0.5525 0.025 Uiso 1 1 calc R . . C5 C 0.1282(2) 0.50795(19) 0.67075(15) 0.0187(4) Uani 1 1 d . . . C6 C 0.2687(2) 0.58936(19) 0.71484(14) 0.0159(4) Uani 1 1 d . . . H6 H 0.2862 0.6392 0.7743 0.019 Uiso 1 1 calc R . . C7 C 0.1927(3) 0.3661(2) 0.44380(15) 0.0286(5) Uani 1 1 d . . . H7A H 0.0883 0.3330 0.4178 0.043 Uiso 1 1 calc R . . H7C H 0.2309 0.2943 0.4397 0.043 Uiso 1 1 calc R . . H7B H 0.2424 0.4207 0.4124 0.043 Uiso 1 1 calc R . . C8 C 0.0038(2) 0.4994(2) 0.71716(17) 0.0270(5) Uani 1 1 d . . . H8A H -0.0714 0.4158 0.6891 0.040 Uiso 1 1 calc R . . H8B H -0.0373 0.5678 0.7140 0.040 Uiso 1 1 calc R . . H8C H 0.0396 0.5090 0.7784 0.040 Uiso 1 1 calc R . . C9 C 0.6106(2) 0.63423(18) 0.76450(12) 0.0125(4) Uani 1 1 d . . . C10 C 0.5472(2) 0.50113(19) 0.77400(13) 0.0168(4) Uani 1 1 d . . . C11 C 0.7548(2) 0.69733(18) 0.80832(13) 0.0132(4) Uani 1 1 d . . . H11 H 0.7991 0.6536 0.8401 0.016 Uiso 1 1 calc R . . C12 C 0.8416(2) 0.81761(18) 0.81076(13) 0.0128(4) Uani 1 1 d . . . C13 C 0.9997(2) 0.8551(2) 0.85952(15) 0.0220(5) Uani 1 1 d . . . C14 C 0.9042(2) 1.01596(18) 0.77939(13) 0.0129(4) Uani 1 1 d . . . C15 C 0.9799(2) 1.02303(19) 0.71355(13) 0.0150(4) Uani 1 1 d . . . H15 H 0.9633 0.9484 0.6654 0.018 Uiso 1 1 calc R . . C16 C 1.0802(2) 1.1390(2) 0.71772(14) 0.0176(4) Uani 1 1 d . . . C17 C 1.1035(2) 1.2468(2) 0.78939(14) 0.0185(4) Uani 1 1 d . . . H17 H 1.1715 1.3259 0.7928 0.022 Uiso 1 1 calc R . . C18 C 1.0292(2) 1.24142(19) 0.85641(14) 0.0179(4) Uani 1 1 d . . . C19 C 0.9291(2) 1.12447(19) 0.85090(13) 0.0153(4) Uani 1 1 d . . . H19 H 0.8780 1.1190 0.8959 0.018 Uiso 1 1 calc R . . C20 C 1.1584(2) 1.1464(2) 0.64435(15) 0.0245(5) Uani 1 1 d . . . H20C H 1.2224 1.2344 0.6569 0.037 Uiso 1 1 calc R . . H20A H 1.0871 1.1214 0.5895 0.037 Uiso 1 1 calc R . . H20B H 1.2165 1.0881 0.6392 0.037 Uiso 1 1 calc R . . C21 C 1.0517(3) 1.3606(2) 0.93182(15) 0.0267(5) Uani 1 1 d . . . H21B H 1.0826 1.3458 0.9868 0.040 Uiso 1 1 calc R . . H21A H 0.9605 1.3805 0.9314 0.040 Uiso 1 1 calc R . . H21C H 1.1266 1.4328 0.9261 0.040 Uiso 1 1 calc R . . C22 C 0.4674(2) 0.98357(18) 0.70548(13) 0.0123(4) Uani 1 1 d . . . C23 C 0.3874(2) 0.86898(18) 0.63360(13) 0.0138(4) Uani 1 1 d . . . C24 C 0.4777(2) 0.85323(19) 0.57286(13) 0.0155(4) Uani 1 1 d . . . C25 C 0.6088(2) 0.96334(19) 0.60352(13) 0.0147(4) Uani 1 1 d . . . C26 C 0.6000(2) 1.04572(18) 0.68383(13) 0.0134(4) Uani 1 1 d . . . C27 C 0.4151(2) 1.0389(2) 0.78490(14) 0.0190(4) Uani 1 1 d . . . H27B H 0.3710 1.1030 0.7752 0.028 Uiso 1 1 calc R . . H27C H 0.4973 1.0796 0.8354 0.028 Uiso 1 1 calc R . . H27A H 0.3427 0.9701 0.7959 0.028 Uiso 1 1 calc R . . C28 C 0.2303(2) 0.7932(2) 0.61999(15) 0.0204(5) Uani 1 1 d . . . H28B H 0.1692 0.8313 0.5902 0.031 Uiso 1 1 calc R . . H28C H 0.2066 0.7945 0.6766 0.031 Uiso 1 1 calc R . . H28A H 0.2127 0.7043 0.5843 0.031 Uiso 1 1 calc R . . C29 C 0.4396(3) 0.7525(2) 0.48493(14) 0.0236(5) Uani 1 1 d . . . H29B H 0.4174 0.7899 0.4393 0.035 Uiso 1 1 calc R . . H29A H 0.3546 0.6811 0.4817 0.035 Uiso 1 1 calc R . . H29C H 0.5219 0.7209 0.4766 0.035 Uiso 1 1 calc R . . C30 C 0.7209(2) 0.9897(2) 0.55041(14) 0.0218(5) Uani 1 1 d . . . H30A H 0.6785 1.0079 0.4992 0.033 Uiso 1 1 calc R . . H30B H 0.7529 0.9145 0.5314 0.033 Uiso 1 1 calc R . . H30C H 0.8043 1.0639 0.5860 0.033 Uiso 1 1 calc R . . C31 C 0.6965(2) 1.18061(19) 0.73142(14) 0.0187(4) Uani 1 1 d . . . H31A H 0.6556 1.2406 0.7119 0.028 Uiso 1 1 calc R . . H31C H 0.7935 1.1912 0.7193 0.028 Uiso 1 1 calc R . . H31B H 0.7034 1.1982 0.7942 0.028 Uiso 1 1 calc R . . C32 C 0.4293(3) 0.1523(2) 0.03792(16) 0.0311(6) Uani 1 1 d . . . H32 H 0.3739 0.0885 0.0584 0.037 Uiso 1 1 calc R . . C33 C 0.3607(3) 0.2174(2) -0.00551(15) 0.0281(5) Uani 1 1 d . . . H33 H 0.2581 0.1974 -0.0155 0.034 Uiso 1 1 calc R . . C34 C 0.4419(3) 0.3112(2) -0.03424(15) 0.0247(5) Uani 1 1 d . . . H34 H 0.3949 0.3560 -0.0637 0.030 Uiso 1 1 calc R . . C35 C 0.5913(3) 0.3402(2) -0.02031(14) 0.0245(5) Uani 1 1 d . . . H35 H 0.6468 0.4049 -0.0400 0.029 Uiso 1 1 calc R . . C36 C 0.6598(3) 0.2747(2) 0.02244(15) 0.0271(5) Uani 1 1 d . . . H36 H 0.7623 0.2943 0.0319 0.033 Uiso 1 1 calc R . . C37 C 0.5790(3) 0.1805(2) 0.05132(15) 0.0295(5) Uani 1 1 d . . . H37 H 0.6259 0.1353 0.0803 0.035 Uiso 1 1 calc R . . N1 N 0.52941(17) 0.68086(15) 0.71665(10) 0.0123(3) Uani 1 1 d . . . N2 N 0.79730(17) 0.89506(15) 0.77185(10) 0.0115(3) Uani 1 1 d . . . F1 F 0.64819(13) 0.46665(11) 0.81811(8) 0.0230(3) Uani 1 1 d . . . F2 F 0.44051(13) 0.49495(12) 0.81800(9) 0.0248(3) Uani 1 1 d . . . F3 F 0.49361(15) 0.40705(11) 0.69685(8) 0.0263(3) Uani 1 1 d . . . F4 F 1.02314(13) 0.76954(12) 0.89792(9) 0.0287(3) Uani 1 1 d . . . F5 F 1.04589(18) 0.96628(14) 0.92304(12) 0.0565(5) Uani 1 1 d . . . F6 F 1.09060(15) 0.8611(2) 0.80558(12) 0.0581(5) Uani 1 1 d . . . Ru1 Ru 0.594415(17) 0.856395(14) 0.698014(10) 0.00971(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0132(10) 0.0083(9) 0.0175(10) 0.0052(8) 0.0004(8) 0.0029(8) C2 0.0166(10) 0.0144(10) 0.0184(11) 0.0040(8) 0.0025(8) 0.0067(8) C3 0.0202(11) 0.0128(10) 0.0213(11) 0.0023(9) -0.0028(9) 0.0054(8) C4 0.0139(10) 0.0135(10) 0.0301(13) 0.0055(9) -0.0039(9) 0.0012(8) C5 0.0156(10) 0.0137(10) 0.0290(12) 0.0109(9) 0.0045(9) 0.0043(8) C6 0.0170(10) 0.0128(10) 0.0179(11) 0.0059(8) 0.0035(8) 0.0038(8) C7 0.0277(13) 0.0235(12) 0.0229(12) -0.0049(10) -0.0063(10) 0.0074(10) C8 0.0163(11) 0.0276(12) 0.0393(14) 0.0166(11) 0.0084(10) 0.0036(9) C9 0.0159(10) 0.0109(9) 0.0117(10) 0.0031(8) 0.0057(8) 0.0050(8) C10 0.0189(11) 0.0136(10) 0.0166(11) 0.0057(8) 0.0009(8) 0.0035(8) C11 0.0152(10) 0.0149(10) 0.0127(10) 0.0068(8) 0.0040(8) 0.0072(8) C12 0.0116(10) 0.0162(10) 0.0111(10) 0.0044(8) 0.0030(8) 0.0049(8) C13 0.0151(11) 0.0227(11) 0.0310(13) 0.0168(10) 0.0021(9) 0.0040(9) C14 0.0093(9) 0.0132(10) 0.0164(10) 0.0070(8) 0.0005(8) 0.0029(8) C15 0.0139(10) 0.0158(10) 0.0163(10) 0.0060(8) 0.0030(8) 0.0058(8) C16 0.0129(10) 0.0219(11) 0.0224(11) 0.0126(9) 0.0053(8) 0.0064(8) C17 0.0122(10) 0.0150(10) 0.0276(12) 0.0112(9) 0.0019(9) 0.0003(8) C18 0.0152(10) 0.0150(10) 0.0206(11) 0.0050(9) -0.0007(8) 0.0030(8) C19 0.0145(10) 0.0171(10) 0.0137(10) 0.0058(8) 0.0025(8) 0.0036(8) C20 0.0222(11) 0.0267(12) 0.0300(13) 0.0155(10) 0.0132(10) 0.0063(10) C21 0.0291(13) 0.0171(11) 0.0263(13) 0.0016(10) 0.0045(10) 0.0015(9) C22 0.0122(9) 0.0135(9) 0.0135(10) 0.0059(8) 0.0016(8) 0.0067(8) C23 0.0139(10) 0.0139(10) 0.0143(10) 0.0052(8) -0.0007(8) 0.0063(8) C24 0.0214(11) 0.0158(10) 0.0116(10) 0.0060(8) 0.0002(8) 0.0100(9) C25 0.0184(10) 0.0165(10) 0.0158(10) 0.0102(8) 0.0056(8) 0.0101(8) C26 0.0147(10) 0.0134(10) 0.0143(10) 0.0065(8) 0.0011(8) 0.0071(8) C27 0.0181(11) 0.0218(11) 0.0180(11) 0.0039(9) 0.0056(9) 0.0096(9) C28 0.0147(10) 0.0180(10) 0.0266(12) 0.0076(9) -0.0020(9) 0.0052(9) C29 0.0372(13) 0.0210(11) 0.0130(11) 0.0039(9) 0.0013(9) 0.0134(10) C30 0.0259(12) 0.0296(12) 0.0208(12) 0.0161(10) 0.0106(9) 0.0157(10) C31 0.0193(11) 0.0129(10) 0.0238(12) 0.0070(9) 0.0015(9) 0.0054(8) C32 0.0454(15) 0.0205(12) 0.0246(13) 0.0060(10) 0.0146(11) 0.0036(11) C33 0.0241(12) 0.0268(12) 0.0271(13) -0.0014(10) 0.0078(10) 0.0068(10) C34 0.0296(12) 0.0208(11) 0.0199(12) 0.0020(9) -0.0023(10) 0.0101(10) C35 0.0278(12) 0.0206(11) 0.0196(12) 0.0058(9) 0.0021(10) 0.0011(9) C36 0.0235(12) 0.0302(13) 0.0218(12) 0.0025(10) -0.0016(10) 0.0084(10) C37 0.0452(15) 0.0248(12) 0.0196(12) 0.0067(10) 0.0009(11) 0.0166(11) N1 0.0123(8) 0.0116(8) 0.0115(8) 0.0024(7) 0.0020(7) 0.0031(7) N2 0.0113(8) 0.0120(8) 0.0109(8) 0.0038(7) 0.0029(6) 0.0025(7) F1 0.0241(7) 0.0164(6) 0.0292(7) 0.0126(5) -0.0016(5) 0.0060(5) F2 0.0230(7) 0.0250(7) 0.0318(7) 0.0181(6) 0.0112(6) 0.0046(5) F3 0.0388(8) 0.0106(6) 0.0217(7) 0.0014(5) -0.0041(6) 0.0045(5) F4 0.0173(6) 0.0310(7) 0.0422(8) 0.0252(7) -0.0030(6) 0.0057(6) F5 0.0492(10) 0.0243(8) 0.0665(12) 0.0002(8) -0.0425(9) 0.0060(7) F6 0.0177(7) 0.1176(16) 0.0756(13) 0.0747(12) 0.0242(8) 0.0297(9) Ru1 0.01006(8) 0.00938(8) 0.00972(8) 0.00345(6) 0.00165(6) 0.00303(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.389(3) . ? C1 C2 1.396(3) . ? C1 N1 1.456(2) . ? C2 C3 1.399(3) . ? C3 C4 1.397(3) . ? C3 C7 1.518(3) . ? C4 C5 1.399(3) . ? C5 C6 1.402(3) . ? C5 C8 1.515(3) . ? C9 N1 1.345(3) . ? C9 C11 1.391(3) . ? C9 C10 1.537(3) . ? C10 F2 1.344(2) . ? C10 F3 1.346(2) . ? C10 F1 1.350(2) . ? C11 C12 1.394(3) . ? C12 N2 1.344(3) . ? C12 C13 1.533(3) . ? C13 F5 1.324(3) . ? C13 F6 1.336(3) . ? C13 F4 1.345(2) . ? C14 C15 1.393(3) . ? C14 C19 1.394(3) . ? C14 N2 1.454(2) . ? C15 C16 1.399(3) . ? C16 C17 1.393(3) . ? C16 C20 1.516(3) . ? C17 C18 1.399(3) . ? C18 C19 1.400(3) . ? C18 C21 1.512(3) . ? C22 C26 1.442(3) . ? C22 C23 1.443(3) . ? C22 C27 1.503(3) . ? C22 Ru1 2.1434(19) . ? C23 C24 1.424(3) . ? C23 C28 1.503(3) . ? C23 Ru1 2.2161(19) . ? C24 C25 1.450(3) . ? C24 C29 1.505(3) . ? C24 Ru1 2.190(2) . ? C25 C26 1.423(3) . ? C25 C30 1.507(3) . ? C25 Ru1 2.2048(19) . ? C26 C31 1.499(3) . ? C26 Ru1 2.2210(19) . ? C32 C37 1.389(4) . ? C32 C33 1.389(4) . ? C33 C34 1.382(3) . ? C34 C35 1.385(3) . ? C35 C36 1.386(3) . ? C36 C37 1.385(3) . ? N1 Ru1 2.0502(16) . ? N2 Ru1 2.0504(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 120.33(18) . . ? C6 C1 N1 121.32(18) . . ? C2 C1 N1 118.35(17) . . ? C1 C2 C3 120.42(19) . . ? C4 C3 C2 118.6(2) . . ? C4 C3 C7 121.38(19) . . ? C2 C3 C7 120.1(2) . . ? C3 C4 C5 121.80(19) . . ? C4 C5 C6 118.5(2) . . ? C4 C5 C8 121.0(2) . . ? C6 C5 C8 120.5(2) . . ? C1 C6 C5 120.4(2) . . ? N1 C9 C11 125.09(18) . . ? N1 C9 C10 120.83(17) . . ? C11 C9 C10 114.08(17) . . ? F2 C10 F3 107.23(16) . . ? F2 C10 F1 105.63(16) . . ? F3 C10 F1 105.36(16) . . ? F2 C10 C9 112.95(16) . . ? F3 C10 C9 112.96(16) . . ? F1 C10 C9 112.12(16) . . ? C9 C11 C12 127.25(18) . . ? N2 C12 C11 125.03(18) . . ? N2 C12 C13 120.85(17) . . ? C11 C12 C13 114.07(17) . . ? F5 C13 F6 107.3(2) . . ? F5 C13 F4 104.87(18) . . ? F6 C13 F4 105.27(18) . . ? F5 C13 C12 114.30(18) . . ? F6 C13 C12 111.60(18) . . ? F4 C13 C12 112.81(17) . . ? C15 C14 C19 120.22(18) . . ? C15 C14 N2 119.31(17) . . ? C19 C14 N2 120.45(17) . . ? C14 C15 C16 120.58(19) . . ? C17 C16 C15 118.58(19) . . ? C17 C16 C20 121.34(19) . . ? C15 C16 C20 120.07(19) . . ? C16 C17 C18 121.67(19) . . ? C17 C18 C19 118.86(19) . . ? C17 C18 C21 120.83(19) . . ? C19 C18 C21 120.26(19) . . ? C14 C19 C18 120.09(19) . . ? C26 C22 C23 108.43(17) . . ? C26 C22 C27 124.84(18) . . ? C23 C22 C27 126.33(18) . . ? C26 C22 Ru1 73.64(11) . . ? C23 C22 Ru1 73.42(11) . . ? C27 C22 Ru1 124.59(14) . . ? C24 C23 C22 107.28(17) . . ? C24 C23 C28 126.61(18) . . ? C22 C23 C28 125.50(18) . . ? C24 C23 Ru1 70.14(11) . . ? C22 C23 Ru1 67.97(11) . . ? C28 C23 Ru1 133.92(14) . . ? C23 C24 C25 108.28(17) . . ? C23 C24 C29 127.45(19) . . ? C25 C24 C29 123.68(19) . . ? C23 C24 Ru1 72.16(11) . . ? C25 C24 Ru1 71.30(11) . . ? C29 C24 Ru1 129.12(14) . . ? C26 C25 C24 108.17(17) . . ? C26 C25 C30 127.72(19) . . ? C24 C25 C30 123.58(19) . . ? C26 C25 Ru1 71.86(11) . . ? C24 C25 Ru1 70.16(11) . . ? C30 C25 Ru1 130.08(14) . . ? C25 C26 C22 107.43(17) . . ? C25 C26 C31 127.13(18) . . ? C22 C26 C31 124.84(18) . . ? C25 C26 Ru1 70.62(11) . . ? C22 C26 Ru1 67.82(10) . . ? C31 C26 Ru1 133.59(14) . . ? C37 C32 C33 119.9(2) . . ? C34 C33 C32 119.9(2) . . ? C33 C34 C35 120.3(2) . . ? C34 C35 C36 119.9(2) . . ? C37 C36 C35 120.1(2) . . ? C36 C37 C32 120.0(2) . . ? C9 N1 C1 116.94(16) . . ? C9 N1 Ru1 126.24(13) . . ? C1 N1 Ru1 116.80(12) . . ? C12 N2 C14 117.42(16) . . ? C12 N2 Ru1 126.29(13) . . ? C14 N2 Ru1 116.24(12) . . ? N1 Ru1 N2 90.07(6) . . ? N1 Ru1 C22 124.53(7) . . ? N2 Ru1 C22 126.81(7) . . ? N1 Ru1 C24 111.74(7) . . ? N2 Ru1 C24 143.63(7) . . ? C22 Ru1 C24 64.38(7) . . ? N1 Ru1 C25 146.80(7) . . ? N2 Ru1 C25 109.81(7) . . ? C22 Ru1 C25 64.16(7) . . ? C24 Ru1 C25 38.54(8) . . ? N1 Ru1 C23 102.27(7) . . ? N2 Ru1 C23 165.08(7) . . ? C22 Ru1 C23 38.62(7) . . ? C24 Ru1 C23 37.70(7) . . ? C25 Ru1 C23 63.58(7) . . ? N1 Ru1 C26 163.06(7) . . ? N2 Ru1 C26 102.64(7) . . ? C22 Ru1 C26 38.54(7) . . ? C24 Ru1 C26 63.69(7) . . ? C25 Ru1 C26 37.52(7) . . ? C23 Ru1 C26 63.68(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.4(3) . . . . ? N1 C1 C2 C3 179.97(18) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C1 C2 C3 C7 -179.64(19) . . . . ? C2 C3 C4 C5 0.0(3) . . . . ? C7 C3 C4 C5 179.7(2) . . . . ? C3 C4 C5 C6 0.3(3) . . . . ? C3 C4 C5 C8 179.3(2) . . . . ? C2 C1 C6 C5 0.7(3) . . . . ? N1 C1 C6 C5 -179.65(17) . . . . ? C4 C5 C6 C1 -0.7(3) . . . . ? C8 C5 C6 C1 -179.69(19) . . . . ? N1 C9 C10 F2 -66.0(2) . . . . ? C11 C9 C10 F2 114.48(19) . . . . ? N1 C9 C10 F3 55.9(2) . . . . ? C11 C9 C10 F3 -123.60(19) . . . . ? N1 C9 C10 F1 174.76(17) . . . . ? C11 C9 C10 F1 -4.7(2) . . . . ? N1 C9 C11 C12 -0.4(3) . . . . ? C10 C9 C11 C12 179.03(19) . . . . ? C9 C11 C12 N2 1.8(3) . . . . ? C9 C11 C12 C13 -175.59(19) . . . . ? N2 C12 C13 F5 57.3(3) . . . . ? C11 C12 C13 F5 -125.2(2) . . . . ? N2 C12 C13 F6 -64.7(3) . . . . ? C11 C12 C13 F6 112.7(2) . . . . ? N2 C12 C13 F4 176.98(18) . . . . ? C11 C12 C13 F4 -5.5(3) . . . . ? C19 C14 C15 C16 -0.8(3) . . . . ? N2 C14 C15 C16 178.02(18) . . . . ? C14 C15 C16 C17 0.5(3) . . . . ? C14 C15 C16 C20 -178.16(19) . . . . ? C15 C16 C17 C18 -0.1(3) . . . . ? C20 C16 C17 C18 178.5(2) . . . . ? C16 C17 C18 C19 0.0(3) . . . . ? C16 C17 C18 C21 -177.6(2) . . . . ? C15 C14 C19 C18 0.6(3) . . . . ? N2 C14 C19 C18 -178.16(18) . . . . ? C17 C18 C19 C14 -0.2(3) . . . . ? C21 C18 C19 C14 177.32(19) . . . . ? C26 C22 C23 C24 6.5(2) . . . . ? C27 C22 C23 C24 179.56(18) . . . . ? Ru1 C22 C23 C24 -59.35(13) . . . . ? C26 C22 C23 C28 -165.05(18) . . . . ? C27 C22 C23 C28 8.0(3) . . . . ? Ru1 C22 C23 C28 129.09(19) . . . . ? C26 C22 C23 Ru1 65.86(13) . . . . ? C27 C22 C23 Ru1 -121.1(2) . . . . ? C22 C23 C24 C25 -4.6(2) . . . . ? C28 C23 C24 C25 166.88(18) . . . . ? Ru1 C23 C24 C25 -62.55(13) . . . . ? C22 C23 C24 C29 -175.97(19) . . . . ? C28 C23 C24 C29 -4.5(3) . . . . ? Ru1 C23 C24 C29 126.0(2) . . . . ? C22 C23 C24 Ru1 57.98(13) . . . . ? C28 C23 C24 Ru1 -130.6(2) . . . . ? C23 C24 C25 C26 0.9(2) . . . . ? C29 C24 C25 C26 172.73(18) . . . . ? Ru1 C24 C25 C26 -62.18(13) . . . . ? C23 C24 C25 C30 -171.30(18) . . . . ? C29 C24 C25 C30 0.5(3) . . . . ? Ru1 C24 C25 C30 125.59(19) . . . . ? C23 C24 C25 Ru1 63.10(13) . . . . ? C29 C24 C25 Ru1 -125.09(19) . . . . ? C24 C25 C26 C22 3.1(2) . . . . ? C30 C25 C26 C22 174.90(19) . . . . ? Ru1 C25 C26 C22 -58.00(13) . . . . ? C24 C25 C26 C31 -168.33(18) . . . . ? C30 C25 C26 C31 3.5(3) . . . . ? Ru1 C25 C26 C31 130.6(2) . . . . ? C24 C25 C26 Ru1 61.10(13) . . . . ? C30 C25 C26 Ru1 -127.1(2) . . . . ? C23 C22 C26 C25 -5.9(2) . . . . ? C27 C22 C26 C25 -179.13(18) . . . . ? Ru1 C22 C26 C25 59.77(13) . . . . ? C23 C22 C26 C31 165.73(18) . . . . ? C27 C22 C26 C31 -7.5(3) . . . . ? Ru1 C22 C26 C31 -128.56(19) . . . . ? C23 C22 C26 Ru1 -65.71(13) . . . . ? C27 C22 C26 Ru1 121.10(19) . . . . ? C37 C32 C33 C34 -0.8(3) . . . . ? C32 C33 C34 C35 0.3(3) . . . . ? C33 C34 C35 C36 0.2(3) . . . . ? C34 C35 C36 C37 -0.1(3) . . . . ? C35 C36 C37 C32 -0.4(3) . . . . ? C33 C32 C37 C36 0.9(4) . . . . ? C11 C9 N1 C1 176.98(18) . . . . ? C10 C9 N1 C1 -2.5(3) . . . . ? C11 C9 N1 Ru1 -1.4(3) . . . . ? C10 C9 N1 Ru1 179.16(13) . . . . ? C6 C1 N1 C9 83.2(2) . . . . ? C2 C1 N1 C9 -97.1(2) . . . . ? C6 C1 N1 Ru1 -98.26(19) . . . . ? C2 C1 N1 Ru1 81.39(19) . . . . ? C11 C12 N2 C14 -178.33(18) . . . . ? C13 C12 N2 C14 -1.1(3) . . . . ? C11 C12 N2 Ru1 -1.1(3) . . . . ? C13 C12 N2 Ru1 176.14(14) . . . . ? C15 C14 N2 C12 94.4(2) . . . . ? C19 C14 N2 C12 -86.8(2) . . . . ? C15 C14 N2 Ru1 -83.19(19) . . . . ? C19 C14 N2 Ru1 95.61(19) . . . . ? C9 N1 Ru1 N2 1.52(16) . . . . ? C1 N1 Ru1 N2 -176.87(14) . . . . ? C9 N1 Ru1 C22 -135.22(15) . . . . ? C1 N1 Ru1 C22 46.39(16) . . . . ? C9 N1 Ru1 C24 151.68(15) . . . . ? C1 N1 Ru1 C24 -26.71(15) . . . . ? C9 N1 Ru1 C25 129.89(16) . . . . ? C1 N1 Ru1 C25 -48.5(2) . . . . ? C9 N1 Ru1 C23 -170.04(16) . . . . ? C1 N1 Ru1 C23 11.57(15) . . . . ? C9 N1 Ru1 C26 -137.5(2) . . . . ? C1 N1 Ru1 C26 44.1(3) . . . . ? C12 N2 Ru1 N1 -0.36(16) . . . . ? C14 N2 Ru1 N1 176.95(13) . . . . ? C12 N2 Ru1 C22 134.80(15) . . . . ? C14 N2 Ru1 C22 -47.89(16) . . . . ? C12 N2 Ru1 C24 -129.14(16) . . . . ? C14 N2 Ru1 C24 48.17(19) . . . . ? C12 N2 Ru1 C25 -153.21(15) . . . . ? C14 N2 Ru1 C25 24.10(15) . . . . ? C12 N2 Ru1 C23 145.8(2) . . . . ? C14 N2 Ru1 C23 -36.9(3) . . . . ? C12 N2 Ru1 C26 168.35(16) . . . . ? C14 N2 Ru1 C26 -14.34(14) . . . . ? C26 C22 Ru1 N1 -178.93(10) . . . . ? C23 C22 Ru1 N1 -63.38(13) . . . . ? C27 C22 Ru1 N1 59.68(19) . . . . ? C26 C22 Ru1 N2 59.94(13) . . . . ? C23 C22 Ru1 N2 175.49(10) . . . . ? C27 C22 Ru1 N2 -61.45(19) . . . . ? C26 C22 Ru1 C24 -79.22(12) . . . . ? C23 C22 Ru1 C24 36.32(11) . . . . ? C27 C22 Ru1 C24 159.39(19) . . . . ? C26 C22 Ru1 C25 -36.25(11) . . . . ? C23 C22 Ru1 C25 79.30(12) . . . . ? C27 C22 Ru1 C25 -157.64(19) . . . . ? C26 C22 Ru1 C23 -115.55(16) . . . . ? C27 C22 Ru1 C23 123.1(2) . . . . ? C23 C22 Ru1 C26 115.55(16) . . . . ? C27 C22 Ru1 C26 -121.4(2) . . . . ? C23 C24 Ru1 N1 81.86(12) . . . . ? C25 C24 Ru1 N1 -160.96(11) . . . . ? C29 C24 Ru1 N1 -42.3(2) . . . . ? C23 C24 Ru1 N2 -155.20(11) . . . . ? C25 C24 Ru1 N2 -38.02(17) . . . . ? C29 C24 Ru1 N2 80.6(2) . . . . ? C23 C24 Ru1 C22 -37.19(11) . . . . ? C25 C24 Ru1 C22 79.99(12) . . . . ? C29 C24 Ru1 C22 -161.4(2) . . . . ? C23 C24 Ru1 C25 -117.18(16) . . . . ? C29 C24 Ru1 C25 118.6(2) . . . . ? C25 C24 Ru1 C23 117.18(16) . . . . ? C29 C24 Ru1 C23 -124.2(2) . . . . ? C23 C24 Ru1 C26 -80.26(12) . . . . ? C25 C24 Ru1 C26 36.92(11) . . . . ? C29 C24 Ru1 C26 155.6(2) . . . . ? C26 C25 Ru1 N1 151.44(12) . . . . ? C24 C25 Ru1 N1 33.60(18) . . . . ? C30 C25 Ru1 N1 -84.1(2) . . . . ? C26 C25 Ru1 N2 -85.00(12) . . . . ? C24 C25 Ru1 N2 157.16(11) . . . . ? C30 C25 Ru1 N2 39.5(2) . . . . ? C26 C25 Ru1 C22 37.23(11) . . . . ? C24 C25 Ru1 C22 -80.62(12) . . . . ? C30 C25 Ru1 C22 161.7(2) . . . . ? C26 C25 Ru1 C24 117.85(16) . . . . ? C30 C25 Ru1 C24 -117.7(2) . . . . ? C26 C25 Ru1 C23 80.44(12) . . . . ? C24 C25 Ru1 C23 -37.41(11) . . . . ? C30 C25 Ru1 C23 -155.1(2) . . . . ? C24 C25 Ru1 C26 -117.85(16) . . . . ? C30 C25 Ru1 C26 124.5(2) . . . . ? C24 C23 Ru1 N1 -109.77(12) . . . . ? C22 C23 Ru1 N1 131.09(11) . . . . ? C28 C23 Ru1 N1 12.4(2) . . . . ? C24 C23 Ru1 N2 105.0(3) . . . . ? C22 C23 Ru1 N2 -14.2(3) . . . . ? C28 C23 Ru1 N2 -132.9(3) . . . . ? C24 C23 Ru1 C22 119.14(17) . . . . ? C28 C23 Ru1 C22 -118.7(2) . . . . ? C22 C23 Ru1 C24 -119.14(17) . . . . ? C28 C23 Ru1 C24 122.2(2) . . . . ? C24 C23 Ru1 C25 38.23(11) . . . . ? C22 C23 Ru1 C25 -80.91(12) . . . . ? C28 C23 Ru1 C25 160.4(2) . . . . ? C24 C23 Ru1 C26 80.30(12) . . . . ? C22 C23 Ru1 C26 -38.85(11) . . . . ? C28 C23 Ru1 C26 -157.5(2) . . . . ? C25 C26 Ru1 N1 -116.1(2) . . . . ? C22 C26 Ru1 N1 3.0(3) . . . . ? C31 C26 Ru1 N1 120.7(3) . . . . ? C25 C26 Ru1 N2 106.15(12) . . . . ? C22 C26 Ru1 N2 -134.75(11) . . . . ? C31 C26 Ru1 N2 -17.1(2) . . . . ? C25 C26 Ru1 C22 -119.09(16) . . . . ? C31 C26 Ru1 C22 117.6(2) . . . . ? C25 C26 Ru1 C24 -37.92(12) . . . . ? C22 C26 Ru1 C24 81.18(12) . . . . ? C31 C26 Ru1 C24 -161.2(2) . . . . ? C22 C26 Ru1 C25 119.09(16) . . . . ? C31 C26 Ru1 C25 -123.3(2) . . . . ? C25 C26 Ru1 C23 -80.18(12) . . . . ? C22 C26 Ru1 C23 38.92(11) . . . . ? C31 C26 Ru1 C23 156.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.359 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.055 data_adp479 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cp*Ru(3,5-(CF3)2C6H3(CF3))2CH' _chemical_melting_point ? _chemical_formula_moiety 'C31 H22 F18 N2 Ru, C6 H6' _chemical_formula_sum 'C37 H28 F18 N2 Ru' _chemical_formula_weight 943.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7701(14) _cell_length_b 39.424(4) _cell_length_c 23.119(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.995(14) _cell_angle_gamma 90.00 _cell_volume 7411.7(19) _cell_formula_units_Z 8 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 208 _cell_measurement_theta_min 3.505 _cell_measurement_theta_max 20.242 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.553 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.210 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3760 _exptl_absorpt_coefficient_mu 0.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.719776 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; Bruker Nonius Area Dector Scaling and Absorption Correction SADABS 2.10 (Bruker, 2003) based on an algorithm described by R.H. Blessing, Acta Cryst. (1995), a51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonus (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonus KappaCCD with \k-goniostat' _diffrn_detector 'Bruker Apex II CCD' _diffrn_measurement_method '\f & \w scans' _diffrn_source 'Enraf Nonius FR590' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88177 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12869 _reflns_number_gt 11255 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'Collect (Hooft, R.W.W., 1998. Nonius B.V., 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg A.J.M., Nonius B.V., 1989-2000)' _computing_data_reduction 'EvalCCD (Hooft R.W.W., Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick G.M., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick G.M., 2008)' _computing_molecular_graphics 'ORTEP-3 for windows 2.02 (Farrugia, 2008)' _computing_publication_material 'WinGX 1.80.05 (Farrugia, 2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A number of CF3 substituents are positioned disordered over multiple sites. A split refinement method used employed where the occupancy was allowed to refine. Some of the fluorine atoms are prolate due diffuse electron density. Similarly part of one benzene solvate was split over two positions, and the occupancy was allowed to refine. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+54.1019P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12869 _refine_ls_number_parameters 1095 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.235 _refine_ls_restrained_S_all 1.234 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3038(10) 0.79782(18) 0.1149(3) 0.0171(16) Uani 1 1 d . . . C2 C 0.1391(10) 0.7998(2) 0.1072(4) 0.0198(17) Uani 1 1 d . . . H2 H 0.1058 0.7942 0.1407 0.024 Uiso 1 1 calc R . . C3 C 0.0232(10) 0.8102(2) 0.0501(4) 0.0230(18) Uani 1 1 d . . . C4 C 0.0679(10) 0.8182(2) 0.0007(4) 0.0210(18) Uani 1 1 d . . . H4 H -0.0124 0.8251 -0.0382 0.025 Uiso 1 1 calc R . . C5 C 0.2347(12) 0.8159(2) 0.0088(4) 0.027(2) Uani 1 1 d . C . C6 C 0.3506(11) 0.8054(2) 0.0657(4) 0.0245(19) Uani 1 1 d . . . H6 H 0.4628 0.8034 0.0707 0.029 Uiso 1 1 calc R . . C7 C -0.1563(12) 0.8113(2) 0.0424(4) 0.034(2) Uani 1 1 d . . . C8 C 0.2875(13) 0.8255(3) -0.0443(5) 0.043(2) Uani 1 1 d . . . C9 C 0.4470(10) 0.75339(19) 0.1829(3) 0.0192(17) Uani 1 1 d . . . C10 C 0.3742(13) 0.7289(2) 0.1283(4) 0.034(2) Uani 1 1 d . . . C11 C 0.5436(10) 0.73740(18) 0.2389(4) 0.0260(18) Uani 1 1 d . . . H11 H 0.5502 0.7134 0.2377 0.031 Uiso 1 1 calc R . . C12 C 0.6307(11) 0.7527(2) 0.2958(4) 0.0245(19) Uani 1 1 d . . . C13 C 0.7228(15) 0.7292(2) 0.3495(5) 0.042(3) Uani 1 1 d . . . C14 C 0.7462(10) 0.79841(18) 0.3662(3) 0.0159(16) Uani 1 1 d . . . C15 C 0.9150(10) 0.8025(2) 0.3796(4) 0.0212(17) Uani 1 1 d . . . H15 H 0.9587 0.7982 0.3484 0.025 Uiso 1 1 calc R . . C16 C 1.0191(9) 0.8131(2) 0.4395(4) 0.0229(18) Uani 1 1 d . . . C17 C 0.9590(10) 0.8193(2) 0.4859(3) 0.0205(17) Uani 1 1 d . . . H17 H 1.0307 0.8263 0.5262 0.025 Uiso 1 1 calc R . . C18 C 0.7918(9) 0.8150(2) 0.4725(4) 0.0194(17) Uani 1 1 d . . . C19 C 0.6845(10) 0.8051(2) 0.4130(4) 0.0212(18) Uani 1 1 d . . . H19 H 0.5702 0.8029 0.4043 0.025 Uiso 1 1 calc R . . C20 C 1.2010(11) 0.8174(3) 0.4514(4) 0.034(2) Uani 1 1 d . . . C21 C 0.7221(11) 0.8218(3) 0.5206(4) 0.030(2) Uani 1 1 d . . . C22 C 0.6673(10) 0.86901(19) 0.2396(5) 0.029(2) Uani 1 1 d . . . C23 C 0.6244(11) 0.87132(19) 0.2937(4) 0.0194(18) Uani 1 1 d U . . C24 C 0.4546(11) 0.86957(17) 0.2735(4) 0.0203(19) Uani 1 1 d . . . C25 C 0.3866(10) 0.87072(19) 0.2058(4) 0.0221(19) Uani 1 1 d . . . C26 C 0.5201(13) 0.87062(19) 0.1860(4) 0.029(2) Uani 1 1 d . . . C27 C 0.8426(13) 0.8703(2) 0.2416(8) 0.069(4) Uani 1 1 d . . . H27A H 0.8499 0.8571 0.2068 0.104 Uiso 1 1 calc R . . H27B H 0.9176 0.8607 0.2811 0.104 Uiso 1 1 calc R . . H27C H 0.8731 0.8939 0.2382 0.104 Uiso 1 1 calc R . . C28 C 0.7432(16) 0.8798(2) 0.3581(5) 0.060(4) Uani 1 1 d . . . H28A H 0.7548 0.9045 0.3627 0.090 Uiso 1 1 calc R . . H28B H 0.8504 0.8696 0.3647 0.090 Uiso 1 1 calc R . . H28C H 0.7019 0.8708 0.3890 0.090 Uiso 1 1 calc R . . C29 C 0.3473(15) 0.8715(2) 0.3115(6) 0.051(3) Uani 1 1 d . . . H29A H 0.4063 0.8618 0.3530 0.077 Uiso 1 1 calc R . . H29B H 0.2458 0.8587 0.2905 0.077 Uiso 1 1 calc R . . H29C H 0.3201 0.8952 0.3157 0.077 Uiso 1 1 calc R . . C30 C 0.2057(13) 0.8751(3) 0.1644(6) 0.057(3) Uani 1 1 d . . . H30A H 0.1724 0.8986 0.1668 0.085 Uiso 1 1 calc R . . H30B H 0.1387 0.8598 0.1785 0.085 Uiso 1 1 calc R . . H30C H 0.1897 0.8697 0.1211 0.085 Uiso 1 1 calc R . . C31 C 0.516(2) 0.8755(2) 0.1201(5) 0.065(4) Uani 1 1 d . . . H31A H 0.5859 0.8583 0.1115 0.097 Uiso 1 1 calc R . . H31B H 0.5579 0.8982 0.1164 0.097 Uiso 1 1 calc R . . H31C H 0.4032 0.8732 0.0901 0.097 Uiso 1 1 calc R . . C32 C 0.4836(10) 0.94970(17) 0.6196(3) 0.0137(16) Uani 1 1 d . . . C33 C 0.3309(11) 0.9433(2) 0.5723(4) 0.0243(19) Uani 1 1 d . . . H33 H 0.2326 0.9468 0.5798 0.029 Uiso 1 1 calc R . . C34 C 0.3228(10) 0.9318(2) 0.5142(4) 0.0222(18) Uani 1 1 d . . . C35 C 0.4643(10) 0.9275(2) 0.5012(4) 0.0234(18) Uani 1 1 d . . . H35 H 0.4584 0.9202 0.4612 0.028 Uiso 1 1 calc R . . C36 C 0.6166(10) 0.9344(2) 0.5494(4) 0.0228(18) Uani 1 1 d . . . C37 C 0.6248(10) 0.94540(19) 0.6075(3) 0.0173(17) Uani 1 1 d . . . H37 H 0.7288 0.9500 0.6392 0.021 Uiso 1 1 calc R . . C38 C 0.1566(12) 0.9259(3) 0.4641(4) 0.037(2) Uani 1 1 d . . . C40 C 0.7775(13) 0.9299(3) 0.5392(4) 0.037(2) Uani 1 1 d . . . C41 C 0.5073(10) 0.9958(2) 0.6891(4) 0.0219(18) Uani 1 1 d . . . C42 C 0.4911(14) 1.0188(2) 0.6343(4) 0.041(3) Uani 1 1 d . . . C43 C 0.5293(11) 1.01177(17) 0.7447(4) 0.0268(18) Uani 1 1 d . . . H43 H 0.5338 1.0358 0.7440 0.032 Uiso 1 1 calc R . . C44 C 0.5458(10) 0.9975(2) 0.8009(4) 0.0231(18) Uani 1 1 d . . . C45 C 0.5846(15) 1.0225(2) 0.8557(5) 0.041(2) Uani 1 1 d . . . C46 C 0.5448(10) 0.95358(18) 0.8712(3) 0.0168(17) Uani 1 1 d . . . C47 C 0.6932(10) 0.9455(2) 0.9183(3) 0.0218(18) Uani 1 1 d . . . H47 H 0.7922 0.9461 0.9106 0.026 Uiso 1 1 calc R . . C48 C 0.6963(10) 0.9365(2) 0.9774(4) 0.0260(19) Uani 1 1 d . D . C49 C 0.5507(10) 0.9351(2) 0.9887(4) 0.0238(19) Uani 1 1 d . . . H49 H 0.5523 0.9287 1.0286 0.029 Uiso 1 1 calc R . . C50 C 0.4038(9) 0.9432(2) 0.9407(4) 0.0177(16) Uani 1 1 d . . . C51 C 0.3982(9) 0.9526(2) 0.8817(4) 0.0177(17) Uani 1 1 d . . . H51 H 0.2966 0.9583 0.8494 0.021 Uiso 1 1 calc R . . C52 C 0.8586(12) 0.9268(3) 1.0278(4) 0.040(3) Uani 1 1 d . . . C53 C 0.2414(12) 0.9431(2) 0.9519(4) 0.031(2) Uani 1 1 d . . . C54 C 0.6454(10) 0.8796(2) 0.7735(4) 0.0234(19) Uani 1 1 d . . . C55 C 0.5269(11) 0.88007(19) 0.8033(4) 0.0221(19) Uani 1 1 d . . . C56 C 0.3714(10) 0.88217(19) 0.7549(4) 0.0260(19) Uani 1 1 d . . . C57 C 0.3874(12) 0.8796(2) 0.6950(4) 0.0242(19) Uani 1 1 d . . . C58 C 0.5587(11) 0.87749(19) 0.7073(4) 0.0211(19) Uani 1 1 d . . . C59 C 0.8305(11) 0.8769(2) 0.8068(5) 0.042(3) Uani 1 1 d . . . H59A H 0.8847 0.8897 0.7834 0.064 Uiso 1 1 calc R . . H59B H 0.8635 0.8530 0.8094 0.064 Uiso 1 1 calc R . . H59C H 0.8629 0.8863 0.8489 0.064 Uiso 1 1 calc R . . C60 C 0.5633(17) 0.8727(2) 0.8706(5) 0.055(3) Uani 1 1 d . . . H60A H 0.4846 0.8848 0.8840 0.083 Uiso 1 1 calc R . . H60B H 0.6752 0.8802 0.8957 0.083 Uiso 1 1 calc R . . H60C H 0.5540 0.8483 0.8762 0.083 Uiso 1 1 calc R . . C61 C 0.2078(12) 0.8818(2) 0.7642(7) 0.054(3) Uani 1 1 d . . . H61A H 0.1736 0.8583 0.7660 0.082 Uiso 1 1 calc R . . H61B H 0.1241 0.8935 0.7293 0.082 Uiso 1 1 calc R . . H61C H 0.2210 0.8933 0.8033 0.082 Uiso 1 1 calc R . . C62 C 0.2457(14) 0.8754(3) 0.6334(5) 0.052(3) Uani 1 1 d . . . H62A H 0.2872 0.8753 0.5995 0.079 Uiso 1 1 calc R . . H62B H 0.1681 0.8942 0.6273 0.079 Uiso 1 1 calc R . . H62C H 0.1895 0.8539 0.6333 0.079 Uiso 1 1 calc R . . C63 C 0.6404(15) 0.8705(2) 0.6614(5) 0.047(3) Uani 1 1 d . . . H63A H 0.7357 0.8854 0.6704 0.070 Uiso 1 1 calc R . . H63B H 0.5619 0.8747 0.6189 0.070 Uiso 1 1 calc R . . H63C H 0.6765 0.8468 0.6652 0.070 Uiso 1 1 calc R . . C64 C 0.9211(15) 0.7695(3) 0.2136(5) 0.050(3) Uani 1 1 d . . . H64 H 0.8360 0.7858 0.1977 0.060 Uiso 1 1 calc R . . C65 C 1.0729(15) 0.7793(2) 0.2584(5) 0.049(3) Uani 1 1 d . . . H65 H 1.0930 0.8023 0.2712 0.059 Uiso 1 1 calc R . . C66 C 1.1911(14) 0.7554(3) 0.2832(5) 0.054(3) Uani 1 1 d . . . H66 H 1.2938 0.7619 0.3139 0.064 Uiso 1 1 calc R . . C67 C 1.1659(14) 0.7221(3) 0.2650(6) 0.059(3) Uani 1 1 d . . . H67 H 1.2481 0.7055 0.2837 0.071 Uiso 1 1 calc R . . C68 C 1.0150(15) 0.7132(3) 0.2178(6) 0.056(3) Uani 1 1 d . . . H68 H 0.9969 0.6904 0.2032 0.067 Uiso 1 1 calc R . . C69 C 0.8936(14) 0.7371(3) 0.1926(5) 0.051(3) Uani 1 1 d . . . H69 H 0.7918 0.7309 0.1610 0.061 Uiso 1 1 calc R . . C70 C 0.9823(16) 0.5278(3) 0.2628(7) 0.075(4) Uani 1 1 d . B . H70 H 0.9466 0.5488 0.2734 0.090 Uiso 1 1 calc R . . C71 C 0.9717(15) 0.4985(4) 0.2948(6) 0.072(4) Uani 1 1 d D . . H71 H 0.9118 0.4977 0.3215 0.086 Uiso 1 1 calc R A 1 C72A C 1.054(9) 0.4706(10) 0.285(3) 0.05(2) Uani 0.29(10) 1 d PD B 1 H72A H 1.0591 0.4502 0.3074 0.062 Uiso 0.29(10) 1 calc PR B 1 C73A C 1.130(8) 0.4727(12) 0.242(2) 0.050(17) Uani 0.29(10) 1 d PD B 1 H73A H 1.2112 0.4564 0.2429 0.060 Uiso 0.29(10) 1 calc PR B 1 C72B C 0.999(9) 0.4686(7) 0.270(2) 0.108(18) Uani 0.71(10) 1 d PD B 2 H72B H 0.9772 0.4477 0.2859 0.130 Uiso 0.71(10) 1 calc PR B 2 C73B C 1.057(8) 0.4684(5) 0.222(2) 0.087(14) Uani 0.71(10) 1 d PD B 2 H73B H 1.0764 0.4474 0.2063 0.104 Uiso 0.71(10) 1 calc PR B 2 C74 C 1.0887(17) 0.4981(4) 0.1982(6) 0.074(4) Uani 1 1 d D . . H74 H 1.0923 0.4953 0.1579 0.089 Uiso 1 1 calc R B 1 C75 C 1.0435(16) 0.5268(3) 0.2163(7) 0.070(4) Uani 1 1 d . B . H75 H 1.0536 0.5473 0.1966 0.084 Uiso 1 1 calc R . . F1 F -0.1753(7) 0.82730(19) 0.0901(3) 0.0607(19) Uani 1 1 d . . . F2 F -0.2520(7) 0.82676(16) -0.0102(3) 0.0476(15) Uani 1 1 d . . . F3 F -0.2202(7) 0.77989(15) 0.0400(3) 0.0502(15) Uani 1 1 d . . . F4 F 0.3910(10) 0.8515(2) -0.0293(3) 0.072(2) Uani 1 1 d . C . F5 F 0.3747(10) 0.80025(19) -0.0561(3) 0.074(2) Uani 1 1 d . C . F6A F 0.207(13) 0.857(5) -0.076(5) 0.078(4) Uani 0.07(2) 1 d PU C 3 F6B F 0.1656(9) 0.8310(4) -0.0968(3) 0.078(4) Uani 0.93(2) 1 d PU C 4 F7 F 0.4190(10) 0.73605(16) 0.0808(3) 0.0609(19) Uani 1 1 d . . . F8 F 0.2066(8) 0.72903(14) 0.1057(3) 0.0508(16) Uani 1 1 d . . . F9 F 0.4135(9) 0.69644(14) 0.1436(3) 0.0608(19) Uani 1 1 d . . . F10 F 0.6910(9) 0.69620(13) 0.3325(3) 0.0565(18) Uani 1 1 d . . . F11 F 0.6753(12) 0.73312(15) 0.3974(3) 0.076(3) Uani 1 1 d . . . F12 F 0.8851(9) 0.73263(15) 0.3707(3) 0.071(2) Uani 1 1 d . . . F13 F 1.2227(7) 0.8394(2) 0.4116(3) 0.074(2) Uani 1 1 d . . . F14 F 1.2879(6) 0.82875(14) 0.5090(2) 0.0352(12) Uani 1 1 d . . . F15 F 1.2689(7) 0.78816(19) 0.4440(3) 0.067(2) Uani 1 1 d . . . F16 F 0.6103(7) 0.84745(15) 0.5045(2) 0.0412(14) Uani 1 1 d . . . F17 F 0.8351(6) 0.83015(18) 0.5766(2) 0.0525(18) Uani 1 1 d . . . F18 F 0.6373(7) 0.79528(15) 0.5300(3) 0.0455(15) Uani 1 1 d . . . F19 F 0.0558(7) 0.95237(16) 0.4542(3) 0.0497(16) Uani 1 1 d . . . F20 F 0.0792(6) 0.89939(15) 0.4789(3) 0.0437(14) Uani 1 1 d . . . F21 F 0.1638(7) 0.91779(17) 0.4083(2) 0.0516(17) Uani 1 1 d . . . F22 F 0.8598(7) 0.95891(18) 0.5467(3) 0.0556(18) Uani 1 1 d . . . F23 F 0.7524(7) 0.91845(15) 0.4820(2) 0.0404(14) Uani 1 1 d . . . F24 F 0.8757(8) 0.9077(2) 0.5797(3) 0.075(2) Uani 1 1 d . . . F25 F 0.6170(10) 1.01577(14) 0.6139(3) 0.067(2) Uani 1 1 d . . . F26 F 0.3524(10) 1.01450(15) 0.5845(2) 0.071(2) Uani 1 1 d . . . F27 F 0.4929(9) 1.05204(12) 0.6492(3) 0.0502(17) Uani 1 1 d . . . F28 F 0.7257(9) 1.01519(15) 0.9028(3) 0.0589(19) Uani 1 1 d . . . F29 F 0.4651(9) 1.02280(14) 0.8789(3) 0.0551(18) Uani 1 1 d . . . F30 F 0.5962(10) 1.05423(13) 0.8381(3) 0.059(2) Uani 1 1 d . . . F31 F 0.9337(7) 0.90142(18) 1.0100(3) 0.0603(18) Uani 1 1 d . D . F32A F 0.845(5) 0.9339(17) 1.0813(17) 0.065(5) Uani 0.24(3) 1 d PU D 5 F32B F 0.8424(12) 0.9133(6) 1.0798(4) 0.065(5) Uani 0.76(3) 1 d PU D 6 F33 F 0.9658(7) 0.95184(18) 1.0419(3) 0.066(2) Uani 1 1 d . D . F34 F 0.2599(6) 0.92795(15) 1.0053(2) 0.0373(13) Uani 1 1 d . . . F35 F 0.1877(7) 0.97451(16) 0.9544(3) 0.0548(17) Uani 1 1 d . . . F36 F 0.1239(7) 0.92722(19) 0.9062(3) 0.0598(19) Uani 1 1 d . . . N1 N 0.4238(8) 0.78679(16) 0.1752(3) 0.0160(13) Uani 1 1 d . . . N2 N 0.6402(8) 0.78698(15) 0.3054(3) 0.0159(13) Uani 1 1 d . . . N3 N 0.4945(8) 0.96179(15) 0.6809(3) 0.0147(13) Uani 1 1 d . . . N4 N 0.5370(8) 0.96323(15) 0.8094(3) 0.0145(13) Uani 1 1 d . . . Ru1 Ru 0.53066(7) 0.823895(14) 0.24026(3) 0.01320(13) Uani 1 1 d . . . Ru2 Ru 0.50807(7) 0.925916(14) 0.74594(3) 0.01323(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(4) 0.014(4) 0.014(4) -0.006(3) 0.003(3) -0.004(3) C2 0.020(4) 0.021(4) 0.018(4) 0.001(3) 0.006(4) -0.004(3) C3 0.017(4) 0.025(4) 0.025(5) -0.008(3) 0.005(4) -0.003(3) C4 0.022(4) 0.027(5) 0.011(4) -0.002(3) 0.003(4) -0.005(3) C5 0.033(5) 0.030(5) 0.015(4) -0.003(3) 0.006(4) -0.004(4) C6 0.024(5) 0.034(5) 0.023(4) -0.004(4) 0.018(4) 0.000(4) C7 0.029(5) 0.041(5) 0.032(5) 0.000(4) 0.011(5) 0.003(4) C8 0.039(6) 0.062(7) 0.033(6) 0.004(5) 0.019(5) 0.000(6) C9 0.021(4) 0.018(4) 0.019(4) -0.003(3) 0.008(4) -0.008(3) C10 0.048(6) 0.021(5) 0.021(4) -0.005(3) 0.000(5) 0.004(4) C11 0.037(5) 0.013(3) 0.029(4) 0.000(3) 0.015(4) 0.001(3) C12 0.030(5) 0.020(4) 0.025(4) 0.009(3) 0.011(4) 0.005(4) C13 0.068(8) 0.017(5) 0.034(6) 0.002(4) 0.010(6) 0.003(5) C14 0.023(4) 0.015(4) 0.011(4) 0.002(3) 0.008(3) 0.004(3) C15 0.020(4) 0.028(4) 0.017(4) 0.005(3) 0.008(4) 0.010(4) C16 0.008(4) 0.040(5) 0.018(4) 0.010(4) 0.002(3) 0.002(3) C17 0.018(4) 0.032(5) 0.010(4) 0.003(3) 0.003(3) 0.008(4) C18 0.010(4) 0.029(4) 0.020(4) 0.003(3) 0.006(3) 0.005(3) C19 0.015(4) 0.024(4) 0.026(4) 0.013(3) 0.009(4) 0.005(3) C20 0.019(5) 0.057(6) 0.022(4) 0.012(4) 0.005(4) 0.008(4) C21 0.019(4) 0.050(6) 0.017(4) -0.006(4) 0.004(4) 0.000(4) C22 0.030(5) 0.012(4) 0.053(6) 0.000(4) 0.025(5) 0.000(3) C23 0.024(4) 0.013(4) 0.010(4) 0.004(3) -0.007(3) 0.001(3) C24 0.039(5) 0.007(3) 0.021(4) -0.003(3) 0.018(4) -0.004(3) C25 0.015(4) 0.013(4) 0.028(5) -0.002(3) -0.003(4) 0.005(3) C26 0.055(6) 0.008(4) 0.026(5) 0.003(3) 0.017(5) 0.001(4) C27 0.049(7) 0.024(5) 0.164(14) -0.012(7) 0.074(10) -0.007(5) C28 0.084(9) 0.015(5) 0.038(6) -0.004(4) -0.025(6) 0.000(5) C29 0.089(9) 0.015(5) 0.091(9) -0.007(5) 0.080(8) -0.004(5) C30 0.036(6) 0.023(5) 0.080(9) -0.010(5) -0.014(6) 0.008(5) C31 0.151(14) 0.019(5) 0.041(6) 0.007(4) 0.055(8) -0.003(7) C32 0.020(4) 0.011(4) 0.005(4) 0.002(3) 0.000(3) -0.001(3) C33 0.021(5) 0.036(5) 0.022(4) 0.002(3) 0.015(4) -0.003(4) C34 0.019(5) 0.030(4) 0.020(4) -0.004(3) 0.009(4) -0.005(4) C35 0.030(5) 0.027(4) 0.014(4) 0.000(3) 0.009(4) -0.003(4) C36 0.017(4) 0.034(5) 0.020(4) 0.005(4) 0.010(4) 0.002(4) C37 0.018(4) 0.023(4) 0.005(4) 0.005(3) -0.002(3) -0.003(3) C38 0.041(6) 0.055(6) 0.014(4) 0.002(4) 0.011(4) -0.004(5) C40 0.038(6) 0.057(6) 0.022(4) 0.002(4) 0.017(5) 0.005(5) C41 0.022(4) 0.024(4) 0.023(4) 0.005(3) 0.012(4) -0.001(4) C42 0.063(7) 0.025(5) 0.023(5) -0.004(4) 0.003(5) 0.003(5) C43 0.049(5) 0.010(3) 0.031(4) 0.002(3) 0.027(5) 0.005(3) C44 0.023(5) 0.021(4) 0.023(4) 0.001(3) 0.006(4) 0.005(4) C45 0.066(8) 0.032(5) 0.037(5) 0.000(4) 0.031(6) -0.002(5) C46 0.029(5) 0.015(4) 0.008(4) -0.004(3) 0.009(3) -0.004(3) C47 0.015(4) 0.032(5) 0.016(4) 0.000(3) 0.002(4) 0.000(4) C48 0.006(4) 0.049(5) 0.015(4) -0.003(4) -0.004(4) -0.001(4) C49 0.026(5) 0.034(5) 0.015(4) -0.004(3) 0.011(4) -0.012(4) C50 0.013(4) 0.025(4) 0.017(4) -0.003(3) 0.009(3) 0.001(3) C51 0.011(4) 0.028(4) 0.013(4) 0.002(3) 0.003(3) 0.005(3) C52 0.020(5) 0.078(8) 0.016(5) 0.010(5) -0.001(4) 0.004(5) C53 0.034(5) 0.041(5) 0.017(4) -0.006(4) 0.009(4) -0.008(5) C54 0.015(4) 0.017(4) 0.032(5) 0.001(4) 0.002(4) 0.000(3) C55 0.035(5) 0.014(4) 0.020(4) 0.002(3) 0.014(4) 0.004(4) C56 0.028(5) 0.019(4) 0.039(6) 0.005(4) 0.021(5) 0.000(3) C57 0.030(5) 0.015(4) 0.018(4) 0.002(3) -0.003(4) -0.001(4) C58 0.039(5) 0.009(4) 0.026(5) -0.005(3) 0.025(4) -0.003(4) C59 0.022(5) 0.024(5) 0.068(7) 0.006(5) 0.002(5) 0.007(4) C60 0.114(11) 0.016(5) 0.042(6) 0.009(4) 0.036(7) 0.011(6) C61 0.031(6) 0.029(5) 0.121(11) -0.010(6) 0.050(7) -0.011(4) C62 0.049(7) 0.041(6) 0.030(6) 0.003(5) -0.028(5) -0.018(5) C63 0.078(8) 0.025(5) 0.060(7) 0.000(5) 0.053(7) 0.003(5) C64 0.062(8) 0.050(7) 0.053(6) 0.010(5) 0.039(7) 0.020(6) C65 0.080(8) 0.036(5) 0.061(7) -0.017(5) 0.061(8) -0.015(5) C66 0.042(7) 0.074(9) 0.042(6) -0.010(6) 0.012(5) -0.020(6) C67 0.041(6) 0.056(7) 0.066(8) -0.004(6) 0.003(6) -0.003(5) C68 0.059(8) 0.032(5) 0.072(8) -0.013(5) 0.017(7) -0.008(5) C69 0.037(6) 0.066(8) 0.052(6) -0.006(6) 0.021(6) 0.003(6) C70 0.042(7) 0.064(8) 0.074(9) -0.027(8) -0.028(7) 0.027(7) C71 0.039(7) 0.111(12) 0.067(9) -0.028(9) 0.020(7) -0.015(8) C72A 0.06(4) 0.07(4) 0.05(4) 0.01(3) 0.05(3) 0.01(3) C73A 0.04(3) 0.05(3) 0.07(4) -0.02(3) 0.03(3) -0.01(2) C72B 0.21(5) 0.058(17) 0.07(2) -0.019(13) 0.07(3) -0.05(2) C73B 0.15(4) 0.049(13) 0.07(2) -0.005(11) 0.05(3) 0.015(17) C74 0.068(9) 0.082(10) 0.067(9) 0.021(8) 0.019(8) 0.007(8) C75 0.050(8) 0.052(8) 0.061(8) 0.015(6) -0.035(7) -0.016(6) F1 0.024(3) 0.111(6) 0.050(3) -0.026(4) 0.017(3) 0.008(3) F2 0.020(3) 0.068(4) 0.050(3) 0.023(3) 0.008(3) 0.008(3) F3 0.026(3) 0.059(4) 0.064(4) 0.007(3) 0.015(3) -0.015(3) F4 0.089(5) 0.094(5) 0.049(4) 0.000(4) 0.043(4) -0.038(5) F5 0.099(6) 0.091(5) 0.063(4) 0.010(4) 0.064(5) 0.019(5) F6A 0.037(5) 0.176(12) 0.019(4) 0.039(6) 0.007(4) -0.002(6) F6B 0.037(4) 0.176(12) 0.018(3) 0.039(5) 0.007(3) -0.002(5) F7 0.106(6) 0.048(4) 0.029(3) -0.018(3) 0.027(4) 0.005(4) F8 0.050(4) 0.036(3) 0.044(4) -0.015(3) -0.008(3) -0.010(3) F9 0.087(5) 0.021(3) 0.046(3) -0.013(2) -0.007(4) 0.006(3) F10 0.095(5) 0.016(3) 0.041(3) 0.006(2) 0.005(3) -0.003(3) F11 0.160(8) 0.041(4) 0.027(3) 0.011(3) 0.037(5) 0.002(4) F12 0.058(4) 0.033(3) 0.078(5) 0.009(3) -0.027(4) 0.013(3) F13 0.022(3) 0.159(7) 0.039(3) 0.040(4) 0.009(3) -0.024(4) F14 0.017(3) 0.059(4) 0.027(2) -0.002(2) 0.005(2) -0.006(2) F15 0.019(3) 0.108(6) 0.072(5) -0.037(4) 0.013(3) 0.013(3) F16 0.035(3) 0.059(4) 0.036(3) -0.006(3) 0.020(3) 0.013(3) F17 0.025(3) 0.120(6) 0.017(2) -0.020(3) 0.013(2) 0.002(3) F18 0.043(3) 0.058(4) 0.045(3) 0.011(3) 0.028(3) -0.003(3) F19 0.026(3) 0.067(4) 0.041(3) 0.007(3) -0.005(3) 0.001(3) F20 0.028(3) 0.063(4) 0.035(3) -0.001(3) 0.005(3) -0.022(3) F21 0.035(3) 0.099(5) 0.019(3) -0.011(3) 0.008(3) -0.022(3) F22 0.036(3) 0.094(5) 0.048(4) -0.021(3) 0.029(3) -0.025(3) F23 0.039(3) 0.062(4) 0.031(3) -0.002(2) 0.025(3) 0.007(3) F24 0.044(4) 0.134(7) 0.063(4) 0.059(4) 0.038(4) 0.057(4) F25 0.130(7) 0.033(3) 0.072(5) 0.012(3) 0.078(5) -0.002(4) F26 0.122(7) 0.031(3) 0.028(3) 0.009(2) -0.009(4) 0.003(4) F27 0.103(5) 0.013(3) 0.033(3) 0.009(2) 0.023(3) 0.003(3) F28 0.083(5) 0.040(3) 0.033(3) -0.014(3) -0.001(4) -0.022(3) F29 0.094(5) 0.029(3) 0.065(4) -0.016(3) 0.057(4) -0.002(3) F30 0.134(7) 0.016(3) 0.045(3) -0.010(2) 0.053(4) -0.014(3) F31 0.037(3) 0.077(5) 0.054(4) 0.007(3) 0.002(3) 0.025(3) F32A 0.033(4) 0.136(14) 0.027(4) 0.050(7) 0.012(4) 0.024(8) F32B 0.033(4) 0.135(14) 0.027(3) 0.050(7) 0.012(3) 0.024(7) F33 0.024(3) 0.081(5) 0.064(4) -0.007(4) -0.016(3) -0.008(3) F34 0.026(3) 0.066(4) 0.030(3) 0.005(2) 0.023(3) -0.001(3) F35 0.046(4) 0.067(4) 0.068(4) 0.014(3) 0.041(3) 0.027(3) F36 0.025(3) 0.117(6) 0.041(3) -0.025(3) 0.017(3) -0.032(4) N1 0.014(3) 0.024(3) 0.012(3) -0.004(2) 0.006(3) -0.003(3) N2 0.019(3) 0.014(3) 0.015(3) -0.004(3) 0.007(3) -0.006(3) N3 0.015(3) 0.011(3) 0.018(3) -0.001(2) 0.006(3) 0.004(3) N4 0.014(3) 0.014(3) 0.019(3) 0.000(2) 0.011(3) -0.003(3) Ru1 0.0146(3) 0.0131(3) 0.0120(3) 0.0004(2) 0.0052(3) -0.0001(2) Ru2 0.0154(3) 0.0136(3) 0.0124(3) -0.0002(2) 0.0071(3) -0.0001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.380(11) . ? C1 C2 1.390(11) . ? C1 N1 1.463(10) . ? C2 C3 1.391(12) . ? C2 H2 0.9500 . ? C3 C4 1.377(11) . ? C3 C7 1.517(13) . ? C4 C5 1.407(12) . ? C4 H4 0.9500 . ? C5 C6 1.390(12) . ? C5 C8 1.514(12) . ? C6 H6 0.9500 . ? C7 F1 1.334(10) . ? C7 F2 1.336(11) . ? C7 F3 1.354(11) . ? C8 F6B 1.300(12) . ? C8 F4 1.329(13) . ? C8 F5 1.343(12) . ? C8 F6A 1.49(14) . ? C9 N1 1.334(10) . ? C9 C11 1.403(11) . ? C9 C10 1.526(11) . ? C10 F7 1.327(11) . ? C10 F9 1.340(10) . ? C10 F8 1.364(12) . ? C11 C12 1.386(12) . ? C11 H11 0.9500 . ? C12 N2 1.369(10) . ? C12 C13 1.517(12) . ? C13 F12 1.327(13) . ? C13 F11 1.329(12) . ? C13 F10 1.357(10) . ? C14 C15 1.404(11) . ? C14 C19 1.404(10) . ? C14 N2 1.436(10) . ? C15 C16 1.407(12) . ? C15 H15 0.9500 . ? C16 C17 1.381(11) . ? C16 C20 1.524(12) . ? C17 C18 1.392(11) . ? C17 H17 0.9500 . ? C18 C19 1.401(11) . ? C18 C21 1.479(11) . ? C19 H19 0.9500 . ? C20 F13 1.330(10) . ? C20 F15 1.337(11) . ? C20 F14 1.338(10) . ? C21 F17 1.344(10) . ? C21 F18 1.347(11) . ? C21 F16 1.361(11) . ? C22 C26 1.416(13) . ? C22 C23 1.438(12) . ? C22 C27 1.522(12) . ? C22 Ru1 2.148(8) . ? C23 C24 1.385(12) . ? C23 C28 1.500(12) . ? C23 Ru1 2.222(8) . ? C24 C25 1.452(11) . ? C24 C29 1.512(11) . ? C24 Ru1 2.159(7) . ? C25 C26 1.407(13) . ? C25 C30 1.525(13) . ? C25 Ru1 2.210(8) . ? C26 C31 1.524(12) . ? C26 Ru1 2.211(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.379(11) . ? C32 C33 1.399(11) . ? C32 N3 1.464(9) . ? C33 C34 1.395(11) . ? C33 H33 0.9500 . ? C34 C35 1.392(12) . ? C34 C38 1.502(13) . ? C35 C36 1.409(12) . ? C35 H35 0.9500 . ? C36 C37 1.387(11) . ? C36 C40 1.525(12) . ? C37 H37 0.9500 . ? C38 F19 1.330(11) . ? C38 F21 1.355(10) . ? C38 F20 1.358(11) . ? C40 F22 1.328(12) . ? C40 F24 1.334(11) . ? C40 F23 1.336(10) . ? C41 N3 1.351(10) . ? C41 C43 1.379(11) . ? C41 C42 1.521(12) . ? C42 F26 1.336(12) . ? C42 F27 1.355(10) . ? C42 F25 1.357(13) . ? C43 C44 1.374(11) . ? C43 H43 0.9500 . ? C44 N4 1.370(10) . ? C44 C45 1.539(12) . ? C45 F30 1.331(10) . ? C45 F28 1.339(13) . ? C45 F29 1.345(12) . ? C46 C47 1.385(11) . ? C46 C51 1.395(11) . ? C46 N4 1.456(9) . ? C47 C48 1.403(11) . ? C47 H47 0.9500 . ? C48 C49 1.396(12) . ? C48 C52 1.512(12) . ? C49 C50 1.388(12) . ? C49 H49 0.9500 . ? C50 C51 1.395(11) . ? C50 C53 1.539(12) . ? C51 H51 0.9500 . ? C52 F32A 1.32(4) . ? C52 F33 1.317(12) . ? C52 F31 1.345(12) . ? C52 F32B 1.370(15) . ? C53 F36 1.326(10) . ? C53 F34 1.326(10) . ? C53 F35 1.332(11) . ? C54 C58 1.436(12) . ? C54 C55 1.445(12) . ? C54 C59 1.517(12) . ? C54 Ru2 2.148(8) . ? C55 C56 1.406(12) . ? C55 C60 1.496(12) . ? C55 Ru2 2.210(8) . ? C56 C57 1.447(12) . ? C56 C61 1.528(11) . ? C56 Ru2 2.154(7) . ? C57 C58 1.423(13) . ? C57 C62 1.509(12) . ? C57 Ru2 2.215(8) . ? C58 C63 1.510(11) . ? C58 Ru2 2.223(7) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C69 1.355(15) . ? C64 C65 1.400(16) . ? C64 H64 0.9500 . ? C65 C66 1.359(16) . ? C65 H65 0.9500 . ? C66 C67 1.369(16) . ? C66 H66 0.9500 . ? C67 C68 1.408(16) . ? C67 H67 0.9500 . ? C68 C69 1.378(15) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C75 1.369(19) . ? C70 C71 1.395(19) . ? C70 H70 0.9500 . ? C71 C72B 1.37(3) . ? C71 C72A 1.378(15) . ? C71 H71 0.9500 . ? C72A C73A 1.39(3) . ? C72A H72A 0.9500 . ? C73A C74 1.37(2) . ? C73A H73A 0.9500 . ? C72B C73B 1.38(3) . ? C72B H72B 0.9500 . ? C73B C74 1.370(17) . ? C73B H73B 0.9500 . ? C74 C75 1.317(19) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? F4 F6A 1.59(10) . ? N1 Ru1 2.055(6) . ? N2 Ru1 2.056(6) . ? N3 Ru2 2.035(6) . ? N4 Ru2 2.025(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 119.8(8) . . ? C6 C1 N1 121.4(7) . . ? C2 C1 N1 118.8(7) . . ? C1 C2 C3 119.6(7) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C4 C3 C2 121.4(8) . . ? C4 C3 C7 120.1(8) . . ? C2 C3 C7 118.5(7) . . ? C3 C4 C5 118.7(8) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 120.1(7) . . ? C6 C5 C8 120.3(8) . . ? C4 C5 C8 119.6(8) . . ? C1 C6 C5 120.5(8) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? F1 C7 F2 107.9(8) . . ? F1 C7 F3 106.7(8) . . ? F2 C7 F3 105.7(8) . . ? F1 C7 C3 111.3(8) . . ? F2 C7 C3 113.0(8) . . ? F3 C7 C3 111.8(8) . . ? F6B C8 F4 110.9(10) . . ? F6B C8 F5 105.5(10) . . ? F4 C8 F5 103.9(9) . . ? F6B C8 F6A 48(6) . . ? F4 C8 F6A 68(6) . . ? F5 C8 F6A 137(4) . . ? F6B C8 C5 113.8(8) . . ? F4 C8 C5 111.6(8) . . ? F5 C8 C5 110.5(9) . . ? F6A C8 C5 112(4) . . ? N1 C9 C11 125.1(7) . . ? N1 C9 C10 121.2(7) . . ? C11 C9 C10 113.6(7) . . ? F7 C10 F9 107.1(8) . . ? F7 C10 F8 107.0(7) . . ? F9 C10 F8 103.7(8) . . ? F7 C10 C9 112.9(8) . . ? F9 C10 C9 113.5(7) . . ? F8 C10 C9 111.9(7) . . ? C12 C11 C9 127.4(7) . . ? C12 C11 H11 116.3 . . ? C9 C11 H11 116.3 . . ? N2 C12 C11 124.2(7) . . ? N2 C12 C13 119.2(7) . . ? C11 C12 C13 116.6(7) . . ? F12 C13 F11 108.0(9) . . ? F12 C13 F10 106.3(8) . . ? F11 C13 F10 105.0(8) . . ? F12 C13 C12 114.1(8) . . ? F11 C13 C12 111.9(8) . . ? F10 C13 C12 111.0(8) . . ? C15 C14 C19 119.1(7) . . ? C15 C14 N2 119.7(6) . . ? C19 C14 N2 121.2(7) . . ? C14 C15 C16 119.6(7) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 121.4(7) . . ? C17 C16 C20 121.2(7) . . ? C15 C16 C20 117.4(7) . . ? C16 C17 C18 118.9(7) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C17 C18 C19 121.0(7) . . ? C17 C18 C21 120.6(7) . . ? C19 C18 C21 118.3(7) . . ? C18 C19 C14 120.0(7) . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? F13 C20 F15 106.7(8) . . ? F13 C20 F14 107.1(8) . . ? F15 C20 F14 107.5(7) . . ? F13 C20 C16 111.1(7) . . ? F15 C20 C16 111.5(8) . . ? F14 C20 C16 112.6(7) . . ? F17 C21 F18 106.6(7) . . ? F17 C21 F16 106.1(7) . . ? F18 C21 F16 103.6(7) . . ? F17 C21 C18 113.9(7) . . ? F18 C21 C18 113.0(8) . . ? F16 C21 C18 112.8(7) . . ? C26 C22 C23 108.0(7) . . ? C26 C22 C27 127.2(10) . . ? C23 C22 C27 124.2(10) . . ? C26 C22 Ru1 73.5(5) . . ? C23 C22 Ru1 73.6(4) . . ? C27 C22 Ru1 126.0(6) . . ? C24 C23 C22 107.5(7) . . ? C24 C23 C28 127.2(9) . . ? C22 C23 C28 124.5(9) . . ? C24 C23 Ru1 69.1(4) . . ? C22 C23 Ru1 68.0(4) . . ? C28 C23 Ru1 135.5(6) . . ? C23 C24 C25 108.5(7) . . ? C23 C24 C29 128.7(8) . . ? C25 C24 C29 122.1(9) . . ? C23 C24 Ru1 74.1(5) . . ? C25 C24 Ru1 72.5(4) . . ? C29 C24 Ru1 126.2(5) . . ? C26 C25 C24 107.1(8) . . ? C26 C25 C30 126.4(9) . . ? C24 C25 C30 126.2(9) . . ? C26 C25 Ru1 71.5(4) . . ? C24 C25 Ru1 68.7(4) . . ? C30 C25 Ru1 129.8(6) . . ? C25 C26 C22 108.2(7) . . ? C25 C26 C31 128.0(10) . . ? C22 C26 C31 123.4(10) . . ? C25 C26 Ru1 71.4(4) . . ? C22 C26 Ru1 68.6(5) . . ? C31 C26 Ru1 130.8(6) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 119.3(7) . . ? C37 C32 N3 119.9(7) . . ? C33 C32 N3 120.8(7) . . ? C34 C33 C32 120.0(8) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 121.3(8) . . ? C35 C34 C38 120.1(7) . . ? C33 C34 C38 118.5(8) . . ? C34 C35 C36 117.6(7) . . ? C34 C35 H35 121.2 . . ? C36 C35 H35 121.2 . . ? C37 C36 C35 121.1(7) . . ? C37 C36 C40 118.1(8) . . ? C35 C36 C40 120.9(7) . . ? C32 C37 C36 120.7(7) . . ? C32 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? F19 C38 F21 106.6(7) . . ? F19 C38 F20 106.6(8) . . ? F21 C38 F20 105.2(8) . . ? F19 C38 C34 113.8(8) . . ? F21 C38 C34 113.1(8) . . ? F20 C38 C34 110.9(7) . . ? F22 C40 F24 107.3(9) . . ? F22 C40 F23 107.5(7) . . ? F24 C40 F23 107.2(8) . . ? F22 C40 C36 111.6(8) . . ? F24 C40 C36 111.1(7) . . ? F23 C40 C36 111.9(8) . . ? N3 C41 C43 124.0(7) . . ? N3 C41 C42 119.9(7) . . ? C43 C41 C42 116.1(7) . . ? F26 C42 F27 105.1(8) . . ? F26 C42 F25 106.7(8) . . ? F27 C42 F25 103.8(8) . . ? F26 C42 C41 114.4(9) . . ? F27 C42 C41 112.2(7) . . ? F25 C42 C41 113.8(8) . . ? C44 C43 C41 128.5(7) . . ? C44 C43 H43 115.8 . . ? C41 C43 H43 115.8 . . ? N4 C44 C43 123.3(7) . . ? N4 C44 C45 121.4(7) . . ? C43 C44 C45 115.3(7) . . ? F30 C45 F28 107.3(9) . . ? F30 C45 F29 105.9(8) . . ? F28 C45 F29 107.3(8) . . ? F30 C45 C44 111.8(7) . . ? F28 C45 C44 112.6(8) . . ? F29 C45 C44 111.6(8) . . ? C47 C46 C51 120.9(7) . . ? C47 C46 N4 121.1(7) . . ? C51 C46 N4 118.1(7) . . ? C46 C47 C48 119.6(8) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C49 C48 C47 120.4(8) . . ? C49 C48 C52 120.6(8) . . ? C47 C48 C52 118.9(8) . . ? C50 C49 C48 118.7(7) . . ? C50 C49 H49 120.6 . . ? C48 C49 H49 120.6 . . ? C49 C50 C51 121.7(7) . . ? C49 C50 C53 120.3(7) . . ? C51 C50 C53 117.9(7) . . ? C50 C51 C46 118.7(7) . . ? C50 C51 H51 120.7 . . ? C46 C51 H51 120.7 . . ? F32A C52 F33 85(3) . . ? F32A C52 F31 132(2) . . ? F33 C52 F31 104.3(8) . . ? F33 C52 F32B 112.0(11) . . ? F31 C52 F32B 101.7(12) . . ? F32A C52 C48 106.2(18) . . ? F33 C52 C48 112.4(9) . . ? F31 C52 C48 112.3(8) . . ? F32B C52 C48 113.3(8) . . ? F36 C53 F34 108.4(8) . . ? F36 C53 F35 107.0(8) . . ? F34 C53 F35 107.5(7) . . ? F36 C53 C50 111.1(7) . . ? F34 C53 C50 111.1(8) . . ? F35 C53 C50 111.7(7) . . ? C58 C54 C55 108.7(8) . . ? C58 C54 C59 125.1(9) . . ? C55 C54 C59 125.7(8) . . ? C58 C54 Ru2 73.6(5) . . ? C55 C54 Ru2 73.0(4) . . ? C59 C54 Ru2 125.8(6) . . ? C56 C55 C54 106.2(7) . . ? C56 C55 C60 127.2(9) . . ? C54 C55 C60 125.5(9) . . ? C56 C55 Ru2 69.1(4) . . ? C54 C55 Ru2 68.3(4) . . ? C60 C55 Ru2 136.2(6) . . ? C55 C56 C57 110.1(7) . . ? C55 C56 C61 124.8(9) . . ? C57 C56 C61 124.5(9) . . ? C55 C56 Ru2 73.4(5) . . ? C57 C56 Ru2 73.0(4) . . ? C61 C56 Ru2 127.4(5) . . ? C58 C57 C56 106.7(7) . . ? C58 C57 C62 128.1(9) . . ? C56 C57 C62 124.8(9) . . ? C58 C57 Ru2 71.6(5) . . ? C56 C57 Ru2 68.4(4) . . ? C62 C57 Ru2 130.8(6) . . ? C57 C58 C54 107.9(7) . . ? C57 C58 C63 127.8(9) . . ? C54 C58 C63 124.0(9) . . ? C57 C58 Ru2 71.0(5) . . ? C54 C58 Ru2 68.1(5) . . ? C63 C58 Ru2 131.2(6) . . ? C54 C59 H59A 109.5 . . ? C54 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C54 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C55 C60 H60A 109.5 . . ? C55 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C56 C61 H61A 109.5 . . ? C56 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C56 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C58 C63 H63A 109.5 . . ? C58 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C58 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C69 C64 C65 121.1(10) . . ? C69 C64 H64 119.5 . . ? C65 C64 H64 119.5 . . ? C66 C65 C64 119.0(10) . . ? C66 C65 H65 120.5 . . ? C64 C65 H65 120.5 . . ? C65 C66 C67 121.6(11) . . ? C65 C66 H66 119.2 . . ? C67 C66 H66 119.2 . . ? C66 C67 C68 118.4(11) . . ? C66 C67 H67 120.8 . . ? C68 C67 H67 120.8 . . ? C69 C68 C67 120.5(10) . . ? C69 C68 H68 119.7 . . ? C67 C68 H68 119.7 . . ? C64 C69 C68 119.3(11) . . ? C64 C69 H69 120.4 . . ? C68 C69 H69 120.4 . . ? C75 C70 C71 121.0(11) . . ? C75 C70 H70 119.5 . . ? C71 C70 H70 119.5 . . ? C72B C71 C70 115.7(13) . . ? C72A C71 C70 115.4(16) . . ? C72B C71 H71 118.1 . . ? C72A C71 H71 122.3 . . ? C70 C71 H71 122.3 . . ? C71 C72A C73A 119.5(18) . . ? C71 C72A H72A 120.2 . . ? C73A C72A H72A 120.2 . . ? C74 C73A C72A 120.2(19) . . ? C74 C73A H73A 119.9 . . ? C72A C73A H73A 119.9 . . ? C71 C72B C73B 121.0(18) . . ? C71 C72B H72B 119.5 . . ? C73B C72B H72B 119.5 . . ? C74 C73B C72B 120.9(17) . . ? C74 C73B H73B 119.5 . . ? C72B C73B H73B 119.5 . . ? C75 C74 C73B 118.2(14) . . ? C75 C74 C73A 115(2) . . ? C75 C74 H74 122.6 . . ? C73B C74 H74 112.7 . . ? C73A C74 H74 122.6 . . ? C74 C75 C70 121.9(12) . . ? C74 C75 H75 119.0 . . ? C70 C75 H75 119.0 . . ? C8 F4 F6A 61(7) . . ? C8 F6A F4 51(3) . . ? C9 N1 C1 116.1(6) . . ? C9 N1 Ru1 126.9(5) . . ? C1 N1 Ru1 117.0(5) . . ? C12 N2 C14 116.6(6) . . ? C12 N2 Ru1 126.6(5) . . ? C14 N2 Ru1 116.6(4) . . ? C41 N3 C32 115.5(6) . . ? C41 N3 Ru2 127.4(5) . . ? C32 N3 Ru2 117.0(4) . . ? C44 N4 C46 114.4(6) . . ? C44 N4 Ru2 127.6(5) . . ? C46 N4 Ru2 117.9(4) . . ? N1 Ru1 N2 89.6(2) . . ? N1 Ru1 C22 133.4(3) . . ? N2 Ru1 C22 118.9(3) . . ? N1 Ru1 C24 137.5(3) . . ? N2 Ru1 C24 116.8(3) . . ? C22 Ru1 C24 63.8(3) . . ? N1 Ru1 C25 106.7(3) . . ? N2 Ru1 C25 154.5(3) . . ? C22 Ru1 C25 63.3(3) . . ? C24 Ru1 C25 38.8(3) . . ? N1 Ru1 C26 105.5(3) . . ? N2 Ru1 C26 156.1(3) . . ? C22 Ru1 C26 37.9(4) . . ? C24 Ru1 C26 63.5(3) . . ? C25 Ru1 C26 37.1(3) . . ? N1 Ru1 C23 168.0(3) . . ? N2 Ru1 C23 102.4(3) . . ? C22 Ru1 C23 38.4(3) . . ? C24 Ru1 C23 36.8(3) . . ? C25 Ru1 C23 62.6(3) . . ? C26 Ru1 C23 62.8(3) . . ? N4 Ru2 N3 89.3(2) . . ? N4 Ru2 C54 119.9(3) . . ? N3 Ru2 C54 132.9(3) . . ? N4 Ru2 C56 115.8(3) . . ? N3 Ru2 C56 138.3(3) . . ? C54 Ru2 C56 64.0(3) . . ? N4 Ru2 C55 101.5(3) . . ? N3 Ru2 C55 169.0(3) . . ? C54 Ru2 C55 38.7(3) . . ? C56 Ru2 C55 37.5(3) . . ? N4 Ru2 C57 152.8(3) . . ? N3 Ru2 C57 107.2(3) . . ? C54 Ru2 C57 63.9(3) . . ? C56 Ru2 C57 38.7(3) . . ? C55 Ru2 C57 63.8(3) . . ? N4 Ru2 C58 157.8(3) . . ? N3 Ru2 C58 105.4(3) . . ? C54 Ru2 C58 38.3(3) . . ? C56 Ru2 C58 63.5(3) . . ? C55 Ru2 C58 63.7(3) . . ? C57 Ru2 C58 37.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.3(12) . . . . ? N1 C1 C2 C3 -179.7(7) . . . . ? C1 C2 C3 C4 0.5(12) . . . . ? C1 C2 C3 C7 178.6(7) . . . . ? C2 C3 C4 C5 -0.2(12) . . . . ? C7 C3 C4 C5 -178.2(8) . . . . ? C3 C4 C5 C6 0.6(12) . . . . ? C3 C4 C5 C8 -178.3(8) . . . . ? C2 C1 C6 C5 1.7(12) . . . . ? N1 C1 C6 C5 -179.9(7) . . . . ? C4 C5 C6 C1 -1.3(12) . . . . ? C8 C5 C6 C1 177.6(8) . . . . ? C4 C3 C7 F1 -134.0(8) . . . . ? C2 C3 C7 F1 48.0(11) . . . . ? C4 C3 C7 F2 -12.3(12) . . . . ? C2 C3 C7 F2 169.6(7) . . . . ? C4 C3 C7 F3 106.8(9) . . . . ? C2 C3 C7 F3 -71.2(10) . . . . ? C6 C5 C8 F6B 172.5(11) . . . . ? C4 C5 C8 F6B -8.6(15) . . . . ? C6 C5 C8 F4 -61.0(12) . . . . ? C4 C5 C8 F4 117.9(10) . . . . ? C6 C5 C8 F5 54.0(12) . . . . ? C4 C5 C8 F5 -127.1(9) . . . . ? C6 C5 C8 F6A -135(7) . . . . ? C4 C5 C8 F6A 44(7) . . . . ? N1 C9 C10 F7 55.8(11) . . . . ? C11 C9 C10 F7 -121.2(8) . . . . ? N1 C9 C10 F9 178.0(8) . . . . ? C11 C9 C10 F9 0.9(12) . . . . ? N1 C9 C10 F8 -65.0(10) . . . . ? C11 C9 C10 F8 117.9(8) . . . . ? N1 C9 C11 C12 0.5(14) . . . . ? C10 C9 C11 C12 177.5(8) . . . . ? C9 C11 C12 N2 -2.6(14) . . . . ? C9 C11 C12 C13 178.7(8) . . . . ? N2 C12 C13 F12 -63.9(11) . . . . ? C11 C12 C13 F12 114.9(9) . . . . ? N2 C12 C13 F11 59.2(12) . . . . ? C11 C12 C13 F11 -122.0(9) . . . . ? N2 C12 C13 F10 176.2(8) . . . . ? C11 C12 C13 F10 -5.0(13) . . . . ? C19 C14 C15 C16 0.3(11) . . . . ? N2 C14 C15 C16 -178.8(7) . . . . ? C14 C15 C16 C17 0.5(12) . . . . ? C14 C15 C16 C20 -179.5(8) . . . . ? C15 C16 C17 C18 -0.1(12) . . . . ? C20 C16 C17 C18 179.9(8) . . . . ? C16 C17 C18 C19 -1.1(12) . . . . ? C16 C17 C18 C21 -179.2(8) . . . . ? C17 C18 C19 C14 1.9(12) . . . . ? C21 C18 C19 C14 -180.0(7) . . . . ? C15 C14 C19 C18 -1.4(11) . . . . ? N2 C14 C19 C18 177.6(7) . . . . ? C17 C16 C20 F13 -122.6(9) . . . . ? C15 C16 C20 F13 57.4(12) . . . . ? C17 C16 C20 F15 118.4(9) . . . . ? C15 C16 C20 F15 -61.5(10) . . . . ? C17 C16 C20 F14 -2.5(12) . . . . ? C15 C16 C20 F14 177.6(7) . . . . ? C17 C18 C21 F17 -3.6(12) . . . . ? C19 C18 C21 F17 178.2(8) . . . . ? C17 C18 C21 F18 -125.5(8) . . . . ? C19 C18 C21 F18 56.3(10) . . . . ? C17 C18 C21 F16 117.4(9) . . . . ? C19 C18 C21 F16 -60.8(10) . . . . ? C26 C22 C23 C24 8.1(8) . . . . ? C27 C22 C23 C24 179.3(7) . . . . ? Ru1 C22 C23 C24 -57.9(5) . . . . ? C26 C22 C23 C28 -163.0(8) . . . . ? C27 C22 C23 C28 8.3(12) . . . . ? Ru1 C22 C23 C28 131.0(8) . . . . ? C26 C22 C23 Ru1 66.0(5) . . . . ? C27 C22 C23 Ru1 -122.8(8) . . . . ? C22 C23 C24 C25 -7.6(9) . . . . ? C28 C23 C24 C25 163.2(8) . . . . ? Ru1 C23 C24 C25 -64.8(5) . . . . ? C22 C23 C24 C29 -178.7(7) . . . . ? C28 C23 C24 C29 -8.0(13) . . . . ? Ru1 C23 C24 C29 124.0(8) . . . . ? C22 C23 C24 Ru1 57.2(5) . . . . ? C28 C23 C24 Ru1 -132.0(8) . . . . ? C23 C24 C25 C26 4.3(9) . . . . ? C29 C24 C25 C26 176.2(7) . . . . ? Ru1 C24 C25 C26 -61.5(5) . . . . ? C23 C24 C25 C30 -169.6(8) . . . . ? C29 C24 C25 C30 2.2(13) . . . . ? Ru1 C24 C25 C30 124.5(9) . . . . ? C23 C24 C25 Ru1 65.8(5) . . . . ? C29 C24 C25 Ru1 -122.3(7) . . . . ? C24 C25 C26 C22 0.7(9) . . . . ? C30 C25 C26 C22 174.7(8) . . . . ? Ru1 C25 C26 C22 -59.0(5) . . . . ? C24 C25 C26 C31 -172.6(8) . . . . ? C30 C25 C26 C31 1.4(13) . . . . ? Ru1 C25 C26 C31 127.7(9) . . . . ? C24 C25 C26 Ru1 59.7(5) . . . . ? C30 C25 C26 Ru1 -126.3(8) . . . . ? C23 C22 C26 C25 -5.3(8) . . . . ? C27 C22 C26 C25 -176.3(7) . . . . ? Ru1 C22 C26 C25 60.7(5) . . . . ? C23 C22 C26 C31 168.3(8) . . . . ? C27 C22 C26 C31 -2.6(13) . . . . ? Ru1 C22 C26 C31 -125.6(8) . . . . ? C23 C22 C26 Ru1 -66.1(5) . . . . ? C27 C22 C26 Ru1 123.0(8) . . . . ? C37 C32 C33 C34 1.8(11) . . . . ? N3 C32 C33 C34 180.0(7) . . . . ? C32 C33 C34 C35 -2.2(13) . . . . ? C32 C33 C34 C38 -178.7(8) . . . . ? C33 C34 C35 C36 1.6(12) . . . . ? C38 C34 C35 C36 178.0(8) . . . . ? C34 C35 C36 C37 -0.7(12) . . . . ? C34 C35 C36 C40 179.2(8) . . . . ? C33 C32 C37 C36 -0.9(11) . . . . ? N3 C32 C37 C36 -179.1(7) . . . . ? C35 C36 C37 C32 0.3(12) . . . . ? C40 C36 C37 C32 -179.5(7) . . . . ? C35 C34 C38 F19 -124.1(9) . . . . ? C33 C34 C38 F19 52.4(11) . . . . ? C35 C34 C38 F21 -2.2(13) . . . . ? C33 C34 C38 F21 174.3(8) . . . . ? C35 C34 C38 F20 115.8(9) . . . . ? C33 C34 C38 F20 -67.7(11) . . . . ? C37 C36 C40 F22 -61.1(10) . . . . ? C35 C36 C40 F22 119.1(9) . . . . ? C37 C36 C40 F24 58.6(12) . . . . ? C35 C36 C40 F24 -121.3(9) . . . . ? C37 C36 C40 F23 178.4(7) . . . . ? C35 C36 C40 F23 -1.5(12) . . . . ? N3 C41 C42 F26 55.1(12) . . . . ? C43 C41 C42 F26 -122.8(9) . . . . ? N3 C41 C42 F27 174.7(8) . . . . ? C43 C41 C42 F27 -3.3(13) . . . . ? N3 C41 C42 F25 -67.8(11) . . . . ? C43 C41 C42 F25 114.2(9) . . . . ? N3 C41 C43 C44 1.5(16) . . . . ? C42 C41 C43 C44 179.3(9) . . . . ? C41 C43 C44 N4 -2.1(16) . . . . ? C41 C43 C44 C45 174.7(9) . . . . ? N4 C44 C45 F30 176.6(8) . . . . ? C43 C44 C45 F30 -0.3(13) . . . . ? N4 C44 C45 F28 55.6(12) . . . . ? C43 C44 C45 F28 -121.2(9) . . . . ? N4 C44 C45 F29 -65.1(11) . . . . ? C43 C44 C45 F29 118.1(9) . . . . ? C51 C46 C47 C48 -0.4(12) . . . . ? N4 C46 C47 C48 179.7(7) . . . . ? C46 C47 C48 C49 0.9(13) . . . . ? C46 C47 C48 C52 178.3(8) . . . . ? C47 C48 C49 C50 -0.8(13) . . . . ? C52 C48 C49 C50 -178.2(8) . . . . ? C48 C49 C50 C51 0.2(13) . . . . ? C48 C49 C50 C53 -178.0(8) . . . . ? C49 C50 C51 C46 0.4(12) . . . . ? C53 C50 C51 C46 178.6(7) . . . . ? C47 C46 C51 C50 -0.3(11) . . . . ? N4 C46 C51 C50 179.6(7) . . . . ? C49 C48 C52 F32A -29(3) . . . . ? C47 C48 C52 F32A 153(3) . . . . ? C49 C48 C52 F33 -120.7(10) . . . . ? C47 C48 C52 F33 61.9(12) . . . . ? C49 C48 C52 F31 122.0(9) . . . . ? C47 C48 C52 F31 -55.4(12) . . . . ? C49 C48 C52 F32B 7.5(17) . . . . ? C47 C48 C52 F32B -170.0(13) . . . . ? C49 C50 C53 F36 -133.9(8) . . . . ? C51 C50 C53 F36 47.8(11) . . . . ? C49 C50 C53 F34 -13.2(11) . . . . ? C51 C50 C53 F34 168.5(7) . . . . ? C49 C50 C53 F35 106.8(9) . . . . ? C51 C50 C53 F35 -71.5(9) . . . . ? C58 C54 C55 C56 -6.6(9) . . . . ? C59 C54 C55 C56 -178.9(8) . . . . ? Ru2 C54 C55 C56 58.9(5) . . . . ? C58 C54 C55 C60 162.4(8) . . . . ? C59 C54 C55 C60 -9.9(13) . . . . ? Ru2 C54 C55 C60 -132.1(8) . . . . ? C58 C54 C55 Ru2 -65.5(6) . . . . ? C59 C54 C55 Ru2 122.2(8) . . . . ? C54 C55 C56 C57 5.7(9) . . . . ? C60 C55 C56 C57 -163.0(8) . . . . ? Ru2 C55 C56 C57 64.2(5) . . . . ? C54 C55 C56 C61 177.2(7) . . . . ? C60 C55 C56 C61 8.4(13) . . . . ? Ru2 C55 C56 C61 -124.3(8) . . . . ? C54 C55 C56 Ru2 -58.5(5) . . . . ? C60 C55 C56 Ru2 132.8(8) . . . . ? C55 C56 C57 C58 -2.8(9) . . . . ? C61 C56 C57 C58 -174.2(7) . . . . ? Ru2 C56 C57 C58 61.7(6) . . . . ? C55 C56 C57 C62 170.0(8) . . . . ? C61 C56 C57 C62 -1.5(13) . . . . ? Ru2 C56 C57 C62 -125.5(9) . . . . ? C55 C56 C57 Ru2 -64.5(6) . . . . ? C61 C56 C57 Ru2 124.0(8) . . . . ? C56 C57 C58 C54 -1.4(9) . . . . ? C62 C57 C58 C54 -173.8(9) . . . . ? Ru2 C57 C58 C54 58.2(6) . . . . ? C56 C57 C58 C63 172.5(7) . . . . ? C62 C57 C58 C63 0.0(14) . . . . ? Ru2 C57 C58 C63 -127.9(8) . . . . ? C56 C57 C58 Ru2 -59.7(5) . . . . ? C62 C57 C58 Ru2 127.9(9) . . . . ? C55 C54 C58 C57 5.0(9) . . . . ? C59 C54 C58 C57 177.4(8) . . . . ? Ru2 C54 C58 C57 -60.1(6) . . . . ? C55 C54 C58 C63 -169.2(7) . . . . ? C59 C54 C58 C63 3.2(14) . . . . ? Ru2 C54 C58 C63 125.7(8) . . . . ? C55 C54 C58 Ru2 65.1(6) . . . . ? C59 C54 C58 Ru2 -122.5(9) . . . . ? C69 C64 C65 C66 -3.3(15) . . . . ? C64 C65 C66 C67 0.7(16) . . . . ? C65 C66 C67 C68 2.2(17) . . . . ? C66 C67 C68 C69 -2.7(18) . . . . ? C65 C64 C69 C68 2.7(16) . . . . ? C67 C68 C69 C64 0.3(17) . . . . ? C75 C70 C71 C72B -11(4) . . . . ? C75 C70 C71 C72A 12(4) . . . . ? C72B C71 C72A C73A 91(7) . . . . ? C70 C71 C72A C73A -4(8) . . . . ? C71 C72A C73A C74 -17(10) . . . . ? C72A C71 C72B C73B -84(5) . . . . ? C70 C71 C72B C73B 9(6) . . . . ? C71 C72B C73B C74 -1(6) . . . . ? C72B C73B C74 C75 -8(5) . . . . ? C72B C73B C74 C73A 82(4) . . . . ? C72A C73A C74 C75 31(7) . . . . ? C72A C73A C74 C73B -73(6) . . . . ? C73B C74 C75 C70 7(4) . . . . ? C73A C74 C75 C70 -24(4) . . . . ? C71 C70 C75 C74 2.7(18) . . . . ? F6B C8 F4 F6A 22(5) . . . . ? F5 C8 F4 F6A 135(5) . . . . ? C5 C8 F4 F6A -106(5) . . . . ? F6B C8 F6A F4 -151(5) . . . . ? F5 C8 F6A F4 -87(8) . . . . ? C5 C8 F6A F4 106(2) . . . . ? C11 C9 N1 C1 -173.5(7) . . . . ? C10 C9 N1 C1 9.8(11) . . . . ? C11 C9 N1 Ru1 3.6(11) . . . . ? C10 C9 N1 Ru1 -173.1(6) . . . . ? C6 C1 N1 C9 -91.2(9) . . . . ? C2 C1 N1 C9 87.2(8) . . . . ? C6 C1 N1 Ru1 91.4(7) . . . . ? C2 C1 N1 Ru1 -90.2(7) . . . . ? C11 C12 N2 C14 -175.3(8) . . . . ? C13 C12 N2 C14 3.4(11) . . . . ? C11 C12 N2 Ru1 0.2(12) . . . . ? C13 C12 N2 Ru1 178.9(6) . . . . ? C15 C14 N2 C12 84.3(9) . . . . ? C19 C14 N2 C12 -94.7(9) . . . . ? C15 C14 N2 Ru1 -91.7(7) . . . . ? C19 C14 N2 Ru1 89.3(7) . . . . ? C43 C41 N3 C32 -175.7(8) . . . . ? C42 C41 N3 C32 6.5(11) . . . . ? C43 C41 N3 Ru2 -1.2(12) . . . . ? C42 C41 N3 Ru2 -179.0(7) . . . . ? C37 C32 N3 C41 82.8(9) . . . . ? C33 C32 N3 C41 -95.4(9) . . . . ? C37 C32 N3 Ru2 -92.3(7) . . . . ? C33 C32 N3 Ru2 89.6(7) . . . . ? C43 C44 N4 C46 -175.4(8) . . . . ? C45 C44 N4 C46 8.0(11) . . . . ? C43 C44 N4 Ru2 2.5(12) . . . . ? C45 C44 N4 Ru2 -174.1(7) . . . . ? C47 C46 N4 C44 -92.9(9) . . . . ? C51 C46 N4 C44 87.2(9) . . . . ? C47 C46 N4 Ru2 89.0(8) . . . . ? C51 C46 N4 Ru2 -90.9(7) . . . . ? C9 N1 Ru1 N2 -4.3(6) . . . . ? C1 N1 Ru1 N2 172.8(5) . . . . ? C9 N1 Ru1 C22 126.8(6) . . . . ? C1 N1 Ru1 C22 -56.1(7) . . . . ? C9 N1 Ru1 C24 -135.5(6) . . . . ? C1 N1 Ru1 C24 41.5(7) . . . . ? C9 N1 Ru1 C25 -164.4(6) . . . . ? C1 N1 Ru1 C25 12.7(6) . . . . ? C9 N1 Ru1 C26 157.0(6) . . . . ? C1 N1 Ru1 C26 -26.0(6) . . . . ? C9 N1 Ru1 C23 169.0(12) . . . . ? C1 N1 Ru1 C23 -14.0(16) . . . . ? C12 N2 Ru1 N1 2.4(7) . . . . ? C14 N2 Ru1 N1 177.9(5) . . . . ? C12 N2 Ru1 C22 -138.9(6) . . . . ? C14 N2 Ru1 C22 36.7(6) . . . . ? C12 N2 Ru1 C24 147.7(6) . . . . ? C14 N2 Ru1 C24 -36.8(6) . . . . ? C12 N2 Ru1 C25 133.2(8) . . . . ? C14 N2 Ru1 C25 -51.3(9) . . . . ? C12 N2 Ru1 C26 -127.6(8) . . . . ? C14 N2 Ru1 C26 47.9(9) . . . . ? C12 N2 Ru1 C23 -176.1(7) . . . . ? C14 N2 Ru1 C23 -0.6(6) . . . . ? C26 C22 Ru1 N1 52.0(6) . . . . ? C23 C22 Ru1 N1 167.0(4) . . . . ? C27 C22 Ru1 N1 -72.3(12) . . . . ? C26 C22 Ru1 N2 172.6(5) . . . . ? C23 C22 Ru1 N2 -72.4(5) . . . . ? C27 C22 Ru1 N2 48.3(11) . . . . ? C26 C22 Ru1 C24 -79.7(5) . . . . ? C23 C22 Ru1 C24 35.3(4) . . . . ? C27 C22 Ru1 C24 156.0(12) . . . . ? C26 C22 Ru1 C25 -36.2(5) . . . . ? C23 C22 Ru1 C25 78.8(5) . . . . ? C27 C22 Ru1 C25 -160.5(12) . . . . ? C23 C22 Ru1 C26 115.0(6) . . . . ? C27 C22 Ru1 C26 -124.3(13) . . . . ? C26 C22 Ru1 C23 -115.0(6) . . . . ? C27 C22 Ru1 C23 120.7(12) . . . . ? C23 C24 Ru1 N1 -163.4(4) . . . . ? C25 C24 Ru1 N1 -47.5(7) . . . . ? C29 C24 Ru1 N1 69.9(10) . . . . ? C23 C24 Ru1 N2 74.0(5) . . . . ? C25 C24 Ru1 N2 -170.1(5) . . . . ? C29 C24 Ru1 N2 -52.7(10) . . . . ? C23 C24 Ru1 C22 -36.7(5) . . . . ? C25 C24 Ru1 C22 79.2(6) . . . . ? C29 C24 Ru1 C22 -163.4(10) . . . . ? C23 C24 Ru1 C25 -115.9(7) . . . . ? C29 C24 Ru1 C25 117.4(11) . . . . ? C23 C24 Ru1 C26 -79.2(5) . . . . ? C25 C24 Ru1 C26 36.7(5) . . . . ? C29 C24 Ru1 C26 154.1(10) . . . . ? C25 C24 Ru1 C23 115.9(7) . . . . ? C29 C24 Ru1 C23 -126.7(10) . . . . ? C26 C25 Ru1 N1 -93.7(5) . . . . ? C24 C25 Ru1 N1 148.6(5) . . . . ? C30 C25 Ru1 N1 28.6(10) . . . . ? C26 C25 Ru1 N2 138.5(7) . . . . ? C24 C25 Ru1 N2 20.9(10) . . . . ? C30 C25 Ru1 N2 -99.1(11) . . . . ? C26 C25 Ru1 C22 36.9(5) . . . . ? C24 C25 Ru1 C22 -80.7(6) . . . . ? C30 C25 Ru1 C22 159.3(11) . . . . ? C26 C25 Ru1 C24 117.6(7) . . . . ? C30 C25 Ru1 C24 -120.0(12) . . . . ? C24 C25 Ru1 C26 -117.6(7) . . . . ? C30 C25 Ru1 C26 122.4(11) . . . . ? C26 C25 Ru1 C23 80.2(5) . . . . ? C24 C25 Ru1 C23 -37.4(5) . . . . ? C30 C25 Ru1 C23 -157.4(11) . . . . ? C25 C26 Ru1 N1 97.4(5) . . . . ? C22 C26 Ru1 N1 -143.6(5) . . . . ? C31 C26 Ru1 N1 -27.2(12) . . . . ? C25 C26 Ru1 N2 -135.2(7) . . . . ? C22 C26 Ru1 N2 -16.2(10) . . . . ? C31 C26 Ru1 N2 100.2(12) . . . . ? C25 C26 Ru1 C22 -119.1(7) . . . . ? C31 C26 Ru1 C22 116.4(13) . . . . ? C25 C26 Ru1 C24 -38.3(5) . . . . ? C22 C26 Ru1 C24 80.7(5) . . . . ? C31 C26 Ru1 C24 -162.9(13) . . . . ? C22 C26 Ru1 C25 119.1(7) . . . . ? C31 C26 Ru1 C25 -124.6(13) . . . . ? C25 C26 Ru1 C23 -79.8(5) . . . . ? C22 C26 Ru1 C23 39.2(5) . . . . ? C31 C26 Ru1 C23 155.6(13) . . . . ? C24 C23 Ru1 N1 68.3(15) . . . . ? C22 C23 Ru1 N1 -51.8(16) . . . . ? C28 C23 Ru1 N1 -169.3(12) . . . . ? C24 C23 Ru1 N2 -118.6(4) . . . . ? C22 C23 Ru1 N2 121.3(5) . . . . ? C28 C23 Ru1 N2 3.8(11) . . . . ? C24 C23 Ru1 C22 120.1(6) . . . . ? C28 C23 Ru1 C22 -117.5(13) . . . . ? C22 C23 Ru1 C24 -120.1(6) . . . . ? C28 C23 Ru1 C24 122.4(13) . . . . ? C24 C23 Ru1 C25 39.4(4) . . . . ? C22 C23 Ru1 C25 -80.7(5) . . . . ? C28 C23 Ru1 C25 161.8(12) . . . . ? C24 C23 Ru1 C26 81.4(5) . . . . ? C22 C23 Ru1 C26 -38.7(5) . . . . ? C28 C23 Ru1 C26 -156.2(13) . . . . ? C44 N4 Ru2 N3 -1.8(7) . . . . ? C46 N4 Ru2 N3 176.1(5) . . . . ? C44 N4 Ru2 C54 139.3(7) . . . . ? C46 N4 Ru2 C54 -42.9(7) . . . . ? C44 N4 Ru2 C56 -147.3(7) . . . . ? C46 N4 Ru2 C56 30.6(7) . . . . ? C44 N4 Ru2 C55 175.9(7) . . . . ? C46 N4 Ru2 C55 -6.2(6) . . . . ? C44 N4 Ru2 C57 -130.3(7) . . . . ? C46 N4 Ru2 C57 47.6(9) . . . . ? C44 N4 Ru2 C58 130.2(8) . . . . ? C46 N4 Ru2 C58 -52.0(10) . . . . ? C41 N3 Ru2 N4 1.2(7) . . . . ? C32 N3 Ru2 N4 175.6(5) . . . . ? C41 N3 Ru2 C54 -130.7(7) . . . . ? C32 N3 Ru2 C54 43.7(7) . . . . ? C41 N3 Ru2 C56 131.0(7) . . . . ? C32 N3 Ru2 C56 -54.6(7) . . . . ? C41 N3 Ru2 C55 -167.1(15) . . . . ? C32 N3 Ru2 C55 7.3(19) . . . . ? C41 N3 Ru2 C57 159.2(7) . . . . ? C32 N3 Ru2 C57 -26.4(6) . . . . ? C41 N3 Ru2 C58 -161.8(7) . . . . ? C32 N3 Ru2 C58 12.6(6) . . . . ? C58 C54 Ru2 N4 -174.5(4) . . . . ? C55 C54 Ru2 N4 69.5(5) . . . . ? C59 C54 Ru2 N4 -52.7(9) . . . . ? C58 C54 Ru2 N3 -53.5(6) . . . . ? C55 C54 Ru2 N3 -169.6(4) . . . . ? C59 C54 Ru2 N3 68.2(9) . . . . ? C58 C54 Ru2 C56 79.4(6) . . . . ? C55 C54 Ru2 C56 -36.7(5) . . . . ? C59 C54 Ru2 C56 -158.8(9) . . . . ? C58 C54 Ru2 C55 116.1(7) . . . . ? C59 C54 Ru2 C55 -122.2(10) . . . . ? C58 C54 Ru2 C57 36.2(5) . . . . ? C55 C54 Ru2 C57 -79.9(5) . . . . ? C59 C54 Ru2 C57 158.0(9) . . . . ? C55 C54 Ru2 C58 -116.1(7) . . . . ? C59 C54 Ru2 C58 121.8(10) . . . . ? C55 C56 Ru2 N4 -74.5(5) . . . . ? C57 C56 Ru2 N4 167.7(5) . . . . ? C61 C56 Ru2 N4 46.9(10) . . . . ? C55 C56 Ru2 N3 164.0(4) . . . . ? C57 C56 Ru2 N3 46.2(6) . . . . ? C61 C56 Ru2 N3 -74.6(11) . . . . ? C55 C56 Ru2 C54 37.8(5) . . . . ? C57 C56 Ru2 C54 -80.1(5) . . . . ? C61 C56 Ru2 C54 159.1(11) . . . . ? C57 C56 Ru2 C55 -117.8(6) . . . . ? C61 C56 Ru2 C55 121.4(12) . . . . ? C55 C56 Ru2 C57 117.8(7) . . . . ? C61 C56 Ru2 C57 -120.8(12) . . . . ? C55 C56 Ru2 C58 80.7(5) . . . . ? C57 C56 Ru2 C58 -37.1(5) . . . . ? C61 C56 Ru2 C58 -157.9(11) . . . . ? C56 C55 Ru2 N4 117.7(5) . . . . ? C54 C55 Ru2 N4 -124.0(5) . . . . ? C60 C55 Ru2 N4 -4.7(12) . . . . ? C56 C55 Ru2 N3 -74.2(17) . . . . ? C54 C55 Ru2 N3 44.1(18) . . . . ? C60 C55 Ru2 N3 163.4(14) . . . . ? C56 C55 Ru2 C54 -118.3(7) . . . . ? C60 C55 Ru2 C54 119.3(13) . . . . ? C54 C55 Ru2 C56 118.3(7) . . . . ? C60 C55 Ru2 C56 -122.4(13) . . . . ? C56 C55 Ru2 C57 -38.0(5) . . . . ? C54 C55 Ru2 C57 80.3(5) . . . . ? C60 C55 Ru2 C57 -160.4(12) . . . . ? C56 C55 Ru2 C58 -79.9(5) . . . . ? C54 C55 Ru2 C58 38.4(5) . . . . ? C60 C55 Ru2 C58 157.7(12) . . . . ? C58 C57 Ru2 N4 -142.1(6) . . . . ? C56 C57 Ru2 N4 -24.9(9) . . . . ? C62 C57 Ru2 N4 93.0(11) . . . . ? C58 C57 Ru2 N3 92.9(5) . . . . ? C56 C57 Ru2 N3 -149.8(4) . . . . ? C62 C57 Ru2 N3 -31.9(10) . . . . ? C58 C57 Ru2 C54 -37.0(5) . . . . ? C56 C57 Ru2 C54 80.2(5) . . . . ? C62 C57 Ru2 C54 -161.9(11) . . . . ? C58 C57 Ru2 C56 -117.2(7) . . . . ? C62 C57 Ru2 C56 117.9(12) . . . . ? C58 C57 Ru2 C55 -80.3(5) . . . . ? C56 C57 Ru2 C55 36.9(5) . . . . ? C62 C57 Ru2 C55 154.9(11) . . . . ? C56 C57 Ru2 C58 117.2(7) . . . . ? C62 C57 Ru2 C58 -124.8(12) . . . . ? C57 C58 Ru2 N4 132.0(7) . . . . ? C54 C58 Ru2 N4 12.8(10) . . . . ? C63 C58 Ru2 N4 -103.8(10) . . . . ? C57 C58 Ru2 N3 -98.4(5) . . . . ? C54 C58 Ru2 N3 142.4(5) . . . . ? C63 C58 Ru2 N3 25.7(10) . . . . ? C57 C58 Ru2 C54 119.2(7) . . . . ? C63 C58 Ru2 C54 -116.6(12) . . . . ? C57 C58 Ru2 C56 38.4(5) . . . . ? C54 C58 Ru2 C56 -80.9(5) . . . . ? C63 C58 Ru2 C56 162.5(11) . . . . ? C57 C58 Ru2 C55 80.5(5) . . . . ? C54 C58 Ru2 C55 -38.8(5) . . . . ? C63 C58 Ru2 C55 -155.4(11) . . . . ? C54 C58 Ru2 C57 -119.2(7) . . . . ? C63 C58 Ru2 C57 124.1(12) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.300 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.116