#!ps # Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_cfa2mg _database_code_depnum_ccdc_archive 'CCDC 903114' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H30 Cu3 N6' _chemical_formula_sum 'C45 H30 Cu3 N6' _chemical_formula_weight 845.37 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' Cu Cu -1.9646 0.5888 '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' _symmetry_cell_setting tetragonal _space_group_name_H-M_alt 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 30.835(14) _cell_length_b 30.835(14) _cell_length_c 29.306(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 27865(19) _cell_formula_units_Z 16 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9775 _cell_measurement_theta_min 7.079 _cell_measurement_theta_max 133.3 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6864 _exptl_absorpt_coefficient_mu 1.235 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5957 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4167 _diffrn_reflns_number 120701 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 66.81 _reflns_number_total 12341 _reflns_number_gt 10383 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Instrument Service v3.0.25' _computing_cell_refinement 'APEX2 v2012.12-0 (Bruker AXS)' _computing_data_reduction 'SAINT V8.27B (Bruker AXS Inc., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Mercury _computing_publication_material Word _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.031 -0.048 0.384 15171 6811 ' ' _platon_squeeze_details ; 2DEF and MeOH solvent molecules were confirmed by TG/IR and CHN analysis. ; _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^)+(0.0850P)^2^+0.2711P] 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 12341 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Cu1 Cu 0.076552(9) 0.380434(9) -0.021465(10) 0.03324(10) Uani 1 1 d . . . Cu2 Cu 0.128492(9) 0.323738(9) 0.055104(9) 0.03228(10) Uani 1 1 d . . . Cu3 Cu 0.149946(9) 0.425672(10) 0.038828(10) 0.03436(10) Uani 1 1 d . . . N1 N 0.05361(5) 0.32862(5) -0.00085(5) 0.0317(4) Uani 1 1 d . . . N2 N 0.07906(5) 0.30279(5) 0.02593(6) 0.0325(4) Uani 1 1 d . . . N3 N 0.17357(6) 0.34987(5) 0.08726(6) 0.0342(4) Uani 1 1 d . . . N4 N 0.17531(5) 0.39436(5) 0.08618(6) 0.0345(4) Uani 1 1 d . . . N5 N 0.12888(6) 0.45427(6) -0.01244(6) 0.0372(4) Uani 1 1 d . . . N6 N 0.10147(6) 0.43208(6) -0.04077(6) 0.0370(4) Uani 1 1 d . . . C1 C 0.01622(6) 0.30739(6) -0.00893(6) 0.0304(4) Uani 1 1 d . . . C2 C 0.01698(6) 0.26663(6) 0.01250(6) 0.0297(4) Uani 1 1 d . . . C3 C 0.05744(6) 0.26557(6) 0.03458(6) 0.0291(4) Uani 1 1 d . . . C4 C 0.07781(6) 0.23493(6) 0.06693(7) 0.0311(4) Uani 1 1 d . . . C5 C 0.09127(7) 0.19365(7) 0.05450(8) 0.0405(5) Uani 1 1 d . . . H5 H 0.0854 0.1830 0.0247 0.049 Uiso 1 1 calc R . . C6 C 0.11327(8) 0.16805(7) 0.08555(9) 0.0471(5) Uani 1 1 d . . . H6 H 0.1221 0.1396 0.0771 0.056 Uiso 1 1 calc R . . C7 C 0.12253(7) 0.18340(8) 0.12862(8) 0.0446(5) Uani 1 1 d . . . H7 H 0.1384 0.1659 0.1494 0.053 Uiso 1 1 calc R . . C8 C 0.10888(8) 0.22403(7) 0.14151(7) 0.0410(5) Uani 1 1 d . . . H8 H 0.1149 0.2344 0.1714 0.049 Uiso 1 1 calc R . . C9 C 0.08649(7) 0.24977(7) 0.11108(7) 0.0359(4) Uani 1 1 d . . . H9 H 0.0769 0.2777 0.1202 0.043 Uiso 1 1 calc R . . C10 C -0.01959(7) 0.32817(7) -0.03414(7) 0.0365(5) Uani 1 1 d . . . C11 C -0.04466(8) 0.30483(9) -0.06529(8) 0.0483(6) Uani 1 1 d . . . H11 H -0.0377 0.2755 -0.0720 0.058 Uiso 1 1 calc R . . C12 C -0.07974(9) 0.32454(11) -0.08646(10) 0.0661(8) Uani 1 1 d . . . H12 H -0.0968 0.3085 -0.1076 0.079 Uiso 1 1 calc R . . C13 C -0.09014(10) 0.36703(11) -0.07718(11) 0.0703(8) Uani 1 1 d . . . H13 H -0.1142 0.3802 -0.0919 0.084 Uiso 1 1 calc R . . C14 C -0.06596(9) 0.39033(10) -0.04687(11) 0.0600(7) Uani 1 1 d . . . H14 H -0.0732 0.4197 -0.0406 0.072 Uiso 1 1 calc R . . C15 C -0.03072(8) 0.37105(8) -0.02515(8) 0.0442(5) Uani 1 1 d . . . H15 H -0.0141 0.3874 -0.0039 0.053 Uiso 1 1 calc R . . C16 C 0.20145(6) 0.33616(6) 0.11974(7) 0.0316(4) Uani 1 1 d . . . C17 C 0.22189(7) 0.37193(7) 0.13954(7) 0.0331(4) Uani 1 1 d . . . C18 C 0.20412(7) 0.40795(7) 0.11763(7) 0.0347(4) Uani 1 1 d . . . C19 C 0.20839(7) 0.29005(7) 0.13087(8) 0.0381(5) Uani 1 1 d . . . C20 C 0.21538(8) 0.25926(8) 0.09708(9) 0.0485(6) Uani 1 1 d . . . H20 H 0.2131 0.2672 0.0659 0.058 Uiso 1 1 calc R . . C21 C 0.22570(9) 0.21685(8) 0.10880(11) 0.0616(7) Uani 1 1 d . . . H21 H 0.2307 0.1960 0.0855 0.074 Uiso 1 1 calc R . . C22 C 0.22876(10) 0.20492(8) 0.15394(12) 0.0650(8) Uani 1 1 d . . . H22 H 0.2362 0.1760 0.1617 0.078 Uiso 1 1 calc R . . C23 C 0.22103(9) 0.23486(9) 0.18775(10) 0.0578(7) Uani 1 1 d . . . H23 H 0.2226 0.2265 0.2189 0.069 Uiso 1 1 calc R . . C24 C 0.21094(8) 0.27701(8) 0.17625(8) 0.0454(5) Uani 1 1 d . . . H24 H 0.2056 0.2976 0.1998 0.055 Uiso 1 1 calc R . . C25 C 0.21205(9) 0.45439(7) 0.12473(8) 0.0485(6) Uani 1 1 d . . . C26 C 0.25463(12) 0.46975(9) 0.12922(11) 0.0689(8) Uani 1 1 d . . . H26 H 0.2784 0.4502 0.1272 0.083 Uiso 1 1 calc R . . C27 C 0.26193(19) 0.51388(12) 0.13674(15) 0.1080(17) Uani 1 1 d . . . H27 H 0.2907 0.5245 0.1400 0.130 Uiso 1 1 calc R . . C28 C 0.2271(2) 0.54206(11) 0.13945(17) 0.126(2) Uani 1 1 d . . . H28 H 0.2320 0.5721 0.1445 0.151 Uiso 1 1 calc R . . C29 C 0.1863(2) 0.52730(12) 0.13497(16) 0.1120(17) Uani 1 1 d . . . H29 H 0.1627 0.5470 0.1369 0.134 Uiso 1 1 calc R . . C30 C 0.17815(13) 0.48320(9) 0.12754(12) 0.0741(9) Uani 1 1 d . . . H30 H 0.1492 0.4732 0.1244 0.089 Uiso 1 1 calc R . . C31 C 0.14039(7) 0.49145(7) -0.03356(7) 0.0349(4) Uani 1 1 d . . . C32 C 0.12038(6) 0.49341(6) -0.07617(7) 0.0330(4) Uani 1 1 d . . . C33 C 0.09653(7) 0.45525(7) -0.07930(7) 0.0351(4) Uani 1 1 d . . . C34 C 0.17024(7) 0.52291(8) -0.01288(8) 0.0424(5) Uani 1 1 d . . . C35 C 0.20965(9) 0.51012(10) 0.00540(11) 0.0630(7) Uani 1 1 d . . . H35 H 0.2175 0.4803 0.0056 0.076 Uiso 1 1 calc R . . C36 C 0.23751(12) 0.54098(14) 0.02334(14) 0.0919(12) Uani 1 1 d . . . H36 H 0.2641 0.5320 0.0367 0.110 Uiso 1 1 calc R . . C37 C 0.22747(15) 0.58337(14) 0.02210(15) 0.1017(14) Uani 1 1 d . . . H37 H 0.2474 0.6041 0.0337 0.122 Uiso 1 1 calc R . . C38 C 0.18831(13) 0.59689(11) 0.00406(14) 0.0819(10) Uani 1 1 d . . . H38 H 0.1810 0.6268 0.0037 0.098 Uiso 1 1 calc R . . C39 C 0.16007(10) 0.56661(9) -0.01339(9) 0.0571(7) Uani 1 1 d . . . H39 H 0.1332 0.5758 -0.0260 0.069 Uiso 1 1 calc R . . C40 C 0.07022(8) 0.43907(7) -0.11804(7) 0.0397(5) Uani 1 1 d . . . C41 C 0.02957(9) 0.42152(9) -0.11109(9) 0.0560(7) Uani 1 1 d . . . H41 H 0.0181 0.4202 -0.0810 0.067 Uiso 1 1 calc R . . C42 C 0.00535(11) 0.40583(12) -0.14707(12) 0.0789(10) Uani 1 1 d . . . H42 H -0.0224 0.3935 -0.1418 0.095 Uiso 1 1 calc R . . C43 C 0.02201(14) 0.40832(14) -0.19106(12) 0.0881(11) Uani 1 1 d . . . H43 H 0.0057 0.3974 -0.2160 0.106 Uiso 1 1 calc R . . C44 C 0.06154(13) 0.42628(13) -0.19848(10) 0.0830(10) Uani 1 1 d . . . H44 H 0.0726 0.4282 -0.2287 0.100 Uiso 1 1 calc R . . C45 C 0.08616(10) 0.44193(10) -0.16208(9) 0.0577(7) Uani 1 1 d . . . H45 H 0.1138 0.4545 -0.1675 0.069 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 Cu1 0.03436(17) 0.03142(16) 0.03393(17) 0.01093(11) -0.00517(11) -0.00861(12) Cu2 0.02978(16) 0.03399(17) 0.03306(17) 0.00414(11) -0.00887(11) -0.00667(12) Cu3 0.03290(16) 0.03662(17) 0.03354(17) 0.01204(12) -0.00904(12) -0.00321(12) N1 0.0324(8) 0.0327(8) 0.0301(8) 0.0057(7) -0.0045(7) -0.0064(7) N2 0.0335(9) 0.0326(9) 0.0314(8) 0.0048(7) -0.0047(7) -0.0071(7) N3 0.0351(9) 0.0333(9) 0.0343(9) 0.0026(7) -0.0080(7) -0.0027(7) N4 0.0337(9) 0.0335(9) 0.0364(9) 0.0053(7) -0.0092(7) -0.0021(7) N5 0.0343(9) 0.0398(9) 0.0374(9) 0.0116(7) -0.0083(7) -0.0084(8) N6 0.0370(9) 0.0360(9) 0.0380(9) 0.0112(7) -0.0063(7) -0.0064(8) C1 0.0303(10) 0.0337(10) 0.0271(9) 0.0029(8) 0.0002(7) -0.0043(8) C2 0.0306(9) 0.0303(9) 0.0283(9) -0.0011(8) 0.0021(7) -0.0036(8) C3 0.0324(10) 0.0277(9) 0.0271(9) 0.0015(7) 0.0003(7) -0.0041(8) C4 0.0285(9) 0.0319(10) 0.0330(10) 0.0025(8) 0.0008(8) -0.0052(8) C5 0.0430(12) 0.0349(11) 0.0437(12) -0.0039(9) -0.0014(9) -0.0013(10) C6 0.0474(13) 0.0324(11) 0.0613(15) 0.0025(10) -0.0026(11) 0.0042(10) C7 0.0380(11) 0.0421(12) 0.0535(13) 0.0168(10) -0.0048(10) -0.0022(10) C8 0.0468(12) 0.0419(12) 0.0342(11) 0.0068(9) -0.0076(9) -0.0063(10) C9 0.0421(11) 0.0312(10) 0.0345(10) 0.0021(8) 0.0003(9) -0.0017(9) C10 0.0335(11) 0.0410(12) 0.0350(10) 0.0098(9) -0.0017(8) -0.0046(9) C11 0.0417(12) 0.0595(15) 0.0438(12) 0.0053(11) -0.0132(10) -0.0073(11) C12 0.0536(16) 0.087(2) 0.0579(16) 0.0108(15) -0.0221(13) -0.0057(15) C13 0.0494(15) 0.084(2) 0.078(2) 0.0261(17) -0.0187(14) 0.0030(15) C14 0.0493(14) 0.0563(16) 0.0742(18) 0.0222(14) 0.0007(13) 0.0104(13) C15 0.0414(12) 0.0432(12) 0.0480(13) 0.0097(10) 0.0009(10) -0.0010(10) C16 0.0287(9) 0.0323(10) 0.0338(10) 0.0025(8) -0.0059(8) 0.0022(8) C17 0.0305(10) 0.0346(10) 0.0343(10) 0.0000(8) -0.0073(8) 0.0012(8) C18 0.0341(10) 0.0332(10) 0.0368(10) 0.0031(8) -0.0092(8) -0.0010(9) C19 0.0337(11) 0.0329(10) 0.0477(12) 0.0023(9) -0.0095(9) -0.0034(9) C20 0.0486(13) 0.0417(12) 0.0551(14) -0.0059(11) -0.0064(11) -0.0012(11) C21 0.0600(16) 0.0388(13) 0.086(2) -0.0128(13) -0.0097(14) -0.0004(12) C22 0.0581(16) 0.0336(13) 0.103(2) 0.0093(14) -0.0205(16) 0.0002(12) C23 0.0553(15) 0.0475(14) 0.0704(17) 0.0200(13) -0.0189(13) -0.0080(12) C24 0.0473(13) 0.0412(12) 0.0479(13) 0.0089(10) -0.0124(10) -0.0036(10) C25 0.0674(16) 0.0339(11) 0.0443(13) 0.0037(9) -0.0192(11) -0.0006(11) C26 0.086(2) 0.0492(15) 0.0716(18) 0.0107(13) -0.0299(16) -0.0258(15) C27 0.159(4) 0.057(2) 0.107(3) 0.013(2) -0.057(3) -0.049(3) C28 0.225(6) 0.0326(17) 0.121(4) -0.0011(19) -0.060(4) -0.018(3) C29 0.178(5) 0.0438(18) 0.114(3) -0.0131(19) -0.034(3) 0.035(3) C30 0.101(2) 0.0452(15) 0.076(2) -0.0041(14) -0.0233(18) 0.0217(16) C31 0.0301(10) 0.0366(11) 0.0381(10) 0.0106(8) -0.0009(8) -0.0032(9) C32 0.0305(10) 0.0320(10) 0.0366(10) 0.0079(8) -0.0007(8) -0.0029(8) C33 0.0336(10) 0.0369(11) 0.0348(10) 0.0101(8) -0.0016(8) 0.0000(9) C34 0.0411(12) 0.0469(13) 0.0393(11) 0.0101(9) -0.0022(9) -0.0125(10) C35 0.0492(14) 0.0651(17) 0.0748(18) 0.0170(14) -0.0200(13) -0.0162(13) C36 0.067(2) 0.109(3) 0.100(3) 0.020(2) -0.0375(19) -0.038(2) C37 0.115(3) 0.091(3) 0.099(3) -0.005(2) -0.031(2) -0.063(3) C38 0.096(3) 0.0599(18) 0.089(2) -0.0076(17) -0.010(2) -0.0288(18) C39 0.0651(16) 0.0473(14) 0.0590(15) 0.0020(12) -0.0025(13) -0.0111(13) C40 0.0481(12) 0.0351(11) 0.0359(11) 0.0061(9) -0.0057(9) -0.0049(10) C41 0.0539(15) 0.0639(16) 0.0502(14) 0.0101(12) -0.0134(12) -0.0176(13) C42 0.072(2) 0.093(2) 0.072(2) 0.0069(17) -0.0249(16) -0.0337(18) C43 0.099(3) 0.107(3) 0.0579(19) -0.0094(18) -0.0269(18) -0.031(2) C44 0.103(3) 0.107(3) 0.0393(15) -0.0066(16) -0.0053(15) -0.013(2) C45 0.0636(16) 0.0664(17) 0.0429(13) 0.0014(12) -0.0001(12) -0.0069(14) _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 Cu1 N1 1.8487(18) . ? Cu1 N6 1.8565(19) . ? Cu2 N3 1.8626(18) . ? Cu2 N2 1.8631(18) . ? Cu3 N5 1.8593(17) . ? Cu3 N4 1.8628(17) . ? N1 C1 1.347(3) . ? N1 N2 1.366(2) . ? N2 C3 1.351(3) . ? N3 C16 1.351(3) . ? N3 N4 1.373(3) . ? N4 C18 1.347(3) . ? N5 C31 1.350(3) . ? N5 N6 1.368(3) . ? N6 C33 1.345(3) . ? C1 C2 1.405(3) . ? C1 C10 1.475(3) . ? C2 C3 1.406(3) . ? C2 C2 1.466(4) 6_454 ? C3 C4 1.478(3) . ? C4 C5 1.388(3) . ? C4 C9 1.398(3) . ? C5 C6 1.383(3) . ? C5 H5 0.9500 . ? C6 C7 1.378(4) . ? C6 H6 0.9500 . ? C7 C8 1.374(4) . ? C7 H7 0.9500 . ? C8 C9 1.379(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.391(3) . ? C10 C11 1.396(3) . ? C11 C12 1.387(4) . ? C11 H11 0.9500 . ? C12 C13 1.376(5) . ? C12 H12 0.9500 . ? C13 C14 1.364(5) . ? C13 H13 0.9500 . ? C14 C15 1.393(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.397(3) . ? C16 C19 1.474(3) . ? C17 C18 1.395(3) . ? C17 C32 1.469(3) 3 ? C18 C25 1.468(3) . ? C19 C20 1.389(3) . ? C19 C24 1.391(3) . ? C20 C21 1.389(4) . ? C20 H20 0.9500 . ? C21 C22 1.376(5) . ? C21 H21 0.9500 . ? C22 C23 1.375(5) . ? C22 H22 0.9500 . ? C23 C24 1.378(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.374(4) . ? C25 C26 1.402(4) . ? C26 C27 1.397(5) . ? C26 H26 0.9500 . ? C27 C28 1.384(8) . ? C27 H27 0.9500 . ? C28 C29 1.344(8) . ? C28 H28 0.9500 . ? C29 C30 1.400(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.394(3) . ? C31 C34 1.468(3) . ? C32 C33 1.391(3) . ? C32 C17 1.469(3) 4_454 ? C33 C40 1.482(3) . ? C34 C39 1.383(4) . ? C34 C35 1.386(4) . ? C35 C36 1.385(5) . ? C35 H35 0.9500 . ? C36 C37 1.344(6) . ? C36 H36 0.9500 . ? C37 C38 1.383(6) . ? C37 H37 0.9500 . ? C38 C39 1.375(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.380(4) . ? C40 C45 1.384(4) . ? C41 C42 1.380(4) . ? C41 H41 0.9500 . ? C42 C43 1.390(5) . ? C42 H42 0.9500 . ? C43 C44 1.357(5) . ? C43 H43 0.9500 . ? C44 C45 1.395(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? 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 Cu1 N6 177.78(8) . . ? N3 Cu2 N2 173.04(8) . . ? N5 Cu3 N4 174.02(8) . . ? C1 N1 N2 108.02(15) . . ? C1 N1 Cu1 133.64(13) . . ? N2 N1 Cu1 118.15(12) . . ? C3 N2 N1 108.63(15) . . ? C3 N2 Cu2 127.73(14) . . ? N1 N2 Cu2 122.10(12) . . ? C16 N3 N4 107.70(16) . . ? C16 N3 Cu2 134.13(14) . . ? N4 N3 Cu2 116.72(12) . . ? C18 N4 N3 108.72(16) . . ? C18 N4 Cu3 128.71(14) . . ? N3 N4 Cu3 121.24(13) . . ? C31 N5 N6 107.98(16) . . ? C31 N5 Cu3 132.95(15) . . ? N6 N5 Cu3 117.97(13) . . ? C33 N6 N5 108.29(16) . . ? C33 N6 Cu1 131.66(15) . . ? N5 N6 Cu1 119.99(13) . . ? N1 C1 C2 110.00(17) . . ? N1 C1 C10 121.18(17) . . ? C2 C1 C10 128.67(18) . . ? C1 C2 C3 103.97(17) . . ? C1 C2 C2 127.9(2) . 6_454 ? C3 C2 C2 128.1(2) . 6_454 ? N2 C3 C2 109.37(17) . . ? N2 C3 C4 116.96(17) . . ? C2 C3 C4 133.41(18) . . ? C5 C4 C9 119.07(19) . . ? C5 C4 C3 123.01(18) . . ? C9 C4 C3 117.76(18) . . ? C6 C5 C4 119.9(2) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 120.6(2) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 120.1(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.0(2) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C4 120.4(2) . . ? C8 C9 H9 119.8 . . ? C4 C9 H9 119.8 . . ? C15 C10 C11 118.5(2) . . ? C15 C10 C1 120.2(2) . . ? C11 C10 C1 121.2(2) . . ? C12 C11 C10 119.9(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 120.2(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C10 C15 C14 120.8(2) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? N3 C16 C17 109.45(17) . . ? N3 C16 C19 123.37(18) . . ? C17 C16 C19 127.18(18) . . ? C18 C17 C16 105.09(17) . . ? C18 C17 C32 128.83(19) . 3 ? C16 C17 C32 125.96(18) . 3 ? N4 C18 C17 109.04(18) . . ? N4 C18 C25 120.71(18) . . ? C17 C18 C25 130.25(19) . . ? C20 C19 C24 118.4(2) . . ? C20 C19 C16 121.6(2) . . ? C24 C19 C16 119.9(2) . . ? C19 C20 C21 120.2(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 120.3(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.1(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 119.7(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C19 121.3(3) . . ? C23 C24 H24 119.4 . . ? C19 C24 H24 119.4 . . ? C30 C25 C26 119.2(3) . . ? C30 C25 C18 120.8(3) . . ? C26 C25 C18 119.9(2) . . ? C27 C26 C25 119.7(4) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C28 C27 C26 119.7(4) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 120.5(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C30 120.8(4) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C25 C30 C29 120.0(4) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? N5 C31 C32 109.34(18) . . ? N5 C31 C34 122.44(18) . . ? C32 C31 C34 128.21(18) . . ? C33 C32 C31 104.85(17) . . ? C33 C32 C17 126.07(19) . 4_454 ? C31 C32 C17 129.05(19) . 4_454 ? N6 C33 C32 109.54(18) . . ? N6 C33 C40 121.77(19) . . ? C32 C33 C40 128.66(18) . . ? C39 C34 C35 118.7(2) . . ? C39 C34 C31 119.8(2) . . ? C35 C34 C31 121.4(2) . . ? C36 C35 C34 119.7(3) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C37 C36 C35 121.0(3) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C39 C38 C37 119.4(3) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C34 120.9(3) . . ? C38 C39 H39 119.5 . . ? C34 C39 H39 119.5 . . ? C41 C40 C45 119.0(2) . . ? C41 C40 C33 121.1(2) . . ? C45 C40 C33 119.9(2) . . ? C42 C41 C40 121.1(3) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C41 C42 C43 119.3(3) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C44 C43 C42 120.2(3) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.5(3) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C40 C45 C44 119.9(3) . . ? C40 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 66.81 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.451 _refine_diff_density_min -0.828 _refine_diff_density_rms 0.060 data_ag19 _database_code_depnum_ccdc_archive 'CCDC 903115' #TrackingRef 'CFA3_corrected.cif' _audit_creation_date 2013-01-31T09:26:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H30 Ag1 N5 O2' _chemical_formula_sum 'C90 H60 Ag6 N12' _chemical_formula_weight 1956.76 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _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 16.3399(3) _cell_length_b 32.7506(4) _cell_length_c 16.2624(3) _cell_angle_alpha 90 _cell_angle_beta 107.382(2) _cell_angle_gamma 90 _cell_volume 8305.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25192 _cell_measurement_theta_min 3.0953 _cell_measurement_theta_max 28.5265 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3863 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.438 _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_absorpt_correction_T_min 0.4369 _exptl_absorpt_correction_T_max 0.8814 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 10.3756 _diffrn_orient_matrix_ub_11 0.0242412 _diffrn_orient_matrix_ub_12 -0.0035243 _diffrn_orient_matrix_ub_13 0.043486 _diffrn_orient_matrix_ub_21 -0.0111535 _diffrn_orient_matrix_ub_22 -0.0209829 _diffrn_orient_matrix_ub_23 -0.004778 _diffrn_orient_matrix_ub_31 0.0368461 _diffrn_orient_matrix_ub_32 -0.0040376 _diffrn_orient_matrix_ub_33 -0.0132056 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0322 _diffrn_reflns_number 52721 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.1 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 14520 _reflns_number_gt 10703 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0457P)^2^+42.6456P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 14520 _refine_ls_number_parameters 1007 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 1.09 _refine_ls_restrained_S_all 1.09 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.106 _refine_diff_density_min -1.719 _refine_diff_density_rms 0.113 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.897 1.102 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ag1 Ag 0.76495(3) 0.190472(14) 0.99727(3) 0.03663(13) Uani 1 1 d . . . Ag2 Ag 0.65986(3) 0.285348(13) 0.94820(3) 0.03766(14) Uani 1 1 d . . . Ag3 Ag 0.87015(3) 0.285006(14) 1.03841(3) 0.03978(15) Uani 1 1 d . . . Ag4 Ag 0.30644(4) 0.066365(14) 0.61031(3) 0.04180(15) Uani 1 1 d . . . Ag5 Ag 0.27137(4) 0.153248(14) 0.49140(3) 0.04160(15) Uani 1 1 d . . . Ag6 Ag 0.21963(3) 0.066404(14) 0.37229(3) 0.03977(15) Uani 1 1 d . . . N1 N 0.6033(3) 0.23109(14) 0.8930(3) 0.0303(12) Uani 1 1 d . . . N2 N 0.6389(3) 0.19320(14) 0.9156(3) 0.0313(12) Uani 1 1 d . . . N3 N 0.7225(3) 0.33985(14) 0.9934(3) 0.0350(13) Uani 1 1 d . . . N4 N 0.8075(3) 0.34043(14) 0.9982(3) 0.0348(13) Uani 1 1 d . . . N5 N 0.8913(3) 0.19361(15) 1.0771(3) 0.0341(13) Uani 1 1 d . . . N6 N 0.9295(3) 0.23131(15) 1.0937(3) 0.0349(13) Uani 1 1 d . . . N7 N 0.3518(3) 0.15137(15) 0.6171(3) 0.0368(13) Uani 1 1 d . . . N8 N 0.3407(4) 0.12224(14) 0.6731(3) 0.0381(14) Uani 1 1 d . . . N9 N 0.2787(4) 0.01393(14) 0.5344(3) 0.0369(13) Uani 1 1 d . . . N10 N 0.2331(3) 0.01447(14) 0.4488(3) 0.0364(13) Uani 1 1 d . . . N11 N 0.1974(3) 0.12325(14) 0.3090(3) 0.0334(13) Uani 1 1 d . . . N12 N 0.1905(3) 0.15260(14) 0.3668(3) 0.0335(12) Uani 1 1 d . . . C1 C 0.5281(4) 0.22648(17) 0.8327(4) 0.0291(14) Uani 1 1 d . . . C2 C 0.5138(4) 0.18479(17) 0.8133(4) 0.0276(13) Uani 1 1 d . . . C3 C 0.5859(4) 0.16538(17) 0.8672(4) 0.0290(14) Uani 1 1 d . . . C4 C 0.6067(4) 0.12121(18) 0.8743(4) 0.0365(16) Uani 1 1 d . . . C5 C 0.6311(5) 0.1018(2) 0.9528(5) 0.058(2) Uani 1 1 d . . . H5 H 0.6382 0.1169 1.003 0.07 Uiso 1 1 calc R . . C6 C 0.6453(6) 0.0600(3) 0.9578(7) 0.077(3) Uani 1 1 d . . . H6 H 0.6587 0.0469 1.011 0.092 Uiso 1 1 calc R . . C7 C 0.6397(7) 0.0377(2) 0.8843(7) 0.082(3) Uani 1 1 d . . . H7 H 0.6511 0.0099 0.8878 0.099 Uiso 1 1 calc R . . C8 C 0.6170(6) 0.0571(2) 0.8061(6) 0.070(3) Uani 1 1 d . . . H8 H 0.6128 0.0423 0.7562 0.084 Uiso 1 1 calc R . . C9 C 0.6003(5) 0.0986(2) 0.8007(5) 0.0484(19) Uani 1 1 d . . . H9 H 0.5847 0.1114 0.7473 0.058 Uiso 1 1 calc R . . C10 C 0.4734(4) 0.26232(17) 0.7967(4) 0.0314(15) Uani 1 1 d . . . C11 C 0.3896(5) 0.2647(2) 0.7987(5) 0.0470(19) Uani 1 1 d . . . H11 H 0.3662 0.2435 0.8227 0.056 Uiso 1 1 calc R . . C12 C 0.3405(5) 0.2986(3) 0.7650(5) 0.061(2) Uani 1 1 d . . . H12 H 0.2844 0.3003 0.7671 0.073 Uiso 1 1 calc R . . C13 C 0.3737(6) 0.3294(2) 0.7286(6) 0.064(3) Uani 1 1 d . . . H13 H 0.34 0.3519 0.7054 0.077 Uiso 1 1 calc R . . C14 C 0.4557(6) 0.3274(2) 0.7263(5) 0.060(2) Uani 1 1 d . . . H14 H 0.4778 0.3487 0.7016 0.072 Uiso 1 1 calc R . . C15 C 0.5071(5) 0.29417(19) 0.7600(4) 0.0420(17) Uani 1 1 d . . . H15 H 0.5634 0.2931 0.7581 0.05 Uiso 1 1 calc R . . C16 C 0.4421(4) 0.16567(17) 0.7464(4) 0.0279(14) Uani 1 1 d . . . C17 C 0.4121(4) 0.17751(18) 0.6598(4) 0.0315(14) Uani 1 1 d . . . C18 C 0.3947(4) 0.13077(17) 0.7522(4) 0.0318(15) Uani 1 1 d . . . C19 C 0.3926(4) 0.10743(19) 0.8289(4) 0.0384(16) Uani 1 1 d . . . C20 C 0.3879(5) 0.1283(2) 0.9010(5) 0.054(2) Uani 1 1 d . . . H20 H 0.3879 0.1567 0.901 0.065 Uiso 1 1 calc R . . C21 C 0.3832(7) 0.1075(3) 0.9732(6) 0.080(3) Uani 1 1 d . . . H21 H 0.3795 0.122 1.0213 0.096 Uiso 1 1 calc R . . C22 C 0.3838(8) 0.0660(3) 0.9746(6) 0.091(4) Uani 1 1 d . . . H22 H 0.3798 0.052 1.023 0.109 Uiso 1 1 calc R . . C23 C 0.3905(8) 0.0447(3) 0.9039(7) 0.099(4) Uani 1 1 d . . . H23 H 0.3915 0.0163 0.9049 0.119 Uiso 1 1 calc R . . C24 C 0.3957(6) 0.0653(2) 0.8313(5) 0.063(2) Uani 1 1 d . . . H24 H 0.4013 0.0507 0.7841 0.075 Uiso 1 1 calc R . . C25 C 0.4376(4) 0.21190(18) 0.6156(4) 0.0363(16) Uani 1 1 d . . . C26 C 0.3785(5) 0.2403(2) 0.5708(4) 0.0434(17) Uani 1 1 d . . . H26 H 0.3211 0.2374 0.5679 0.052 Uiso 1 1 calc R . . C27 C 0.4040(6) 0.2731(2) 0.5300(5) 0.057(2) Uani 1 1 d . . . H27 H 0.3636 0.2922 0.5006 0.069 Uiso 1 1 calc R . . C28 C 0.4862(7) 0.2774(2) 0.5328(5) 0.062(2) Uani 1 1 d . . . H28 H 0.5021 0.2992 0.5041 0.074 Uiso 1 1 calc R . . C29 C 0.5482(6) 0.2500(3) 0.5778(5) 0.060(2) Uani 1 1 d . . . H29 H 0.6054 0.2537 0.5809 0.072 Uiso 1 1 calc R . . C30 C 0.5235(5) 0.2170(2) 0.6183(5) 0.0478(18) Uani 1 1 d . . . H30 H 0.5643 0.1981 0.6475 0.057 Uiso 1 1 calc R . . C31 C 0.9464(4) 0.16633(17) 1.1264(4) 0.0301(14) Uani 1 1 d . . . C32 C 1.0203(4) 0.18583(17) 1.1740(4) 0.0292(14) Uani 1 1 d . . . C33 C 1.0069(4) 0.22706(18) 1.1521(4) 0.0324(15) Uani 1 1 d . . . C34 C 0.9223(4) 0.12284(18) 1.1279(4) 0.0373(16) Uani 1 1 d . . . C35 C 0.9343(5) 0.1029(2) 1.2068(5) 0.052(2) Uani 1 1 d . . . H35 H 0.9576 0.117 1.2581 0.062 Uiso 1 1 calc R . . C36 C 0.9119(7) 0.0622(3) 1.2091(7) 0.077(3) Uani 1 1 d . . . H36 H 0.9199 0.049 1.2616 0.093 Uiso 1 1 calc R . . C37 C 0.8778(8) 0.0415(3) 1.1334(8) 0.093(4) Uani 1 1 d . . . H37 H 0.8623 0.0143 1.135 0.111 Uiso 1 1 calc R . . C38 C 0.8661(7) 0.0600(3) 1.0566(7) 0.085(3) Uani 1 1 d . . . H38 H 0.8445 0.0452 1.0059 0.102 Uiso 1 1 calc R . . C39 C 0.8864(6) 0.1008(2) 1.0532(5) 0.060(2) Uani 1 1 d . . . H39 H 0.8758 0.1136 1 0.072 Uiso 1 1 calc R . . C40 C 1.0946(4) 0.16715(17) 1.2395(4) 0.0295(14) Uani 1 1 d . . . C41 C 1.1399(4) 0.13191(17) 1.2319(4) 0.0326(15) Uani 1 1 d . . . C42 C 1.1385(4) 0.10873(18) 1.1544(4) 0.0376(16) Uani 1 1 d . . . C43 C 1.1251(8) 0.0671(2) 1.1473(6) 0.081(3) Uani 1 1 d . . . H43 H 1.1149 0.0526 1.1925 0.097 Uiso 1 1 calc R . . C44 C 1.1270(10) 0.0465(3) 1.0724(8) 0.117(5) Uani 1 1 d . . . H44 H 1.1185 0.0184 1.0683 0.141 Uiso 1 1 calc R . . C45 C 1.1411(9) 0.0675(4) 1.0051(7) 0.103(4) Uani 1 1 d . . . H45 H 1.146 0.0537 0.9569 0.123 Uiso 1 1 calc R . . C46 C 1.1476(8) 0.1082(3) 1.0098(6) 0.086(3) Uani 1 1 d . . . H46 H 1.1524 0.123 0.9627 0.104 Uiso 1 1 calc R . . C47 C 1.1473(6) 0.1283(3) 1.0844(5) 0.066(2) Uani 1 1 d . . . H47 H 1.1534 0.1566 1.0865 0.079 Uiso 1 1 calc R . . C48 C 1.0619(4) 0.26328(18) 1.1834(4) 0.0387(17) Uani 1 1 d . . . C49 C 1.0315(5) 0.2953(2) 1.2199(5) 0.056(2) Uani 1 1 d . . . H49 H 0.9759 0.2945 1.224 0.067 Uiso 1 1 calc R . . C50 C 1.0834(7) 0.3293(2) 1.2512(7) 0.081(3) Uani 1 1 d . . . H50 H 1.0627 0.3508 1.2768 0.097 Uiso 1 1 calc R . . C51 C 1.1659(6) 0.3311(3) 1.2439(7) 0.082(3) Uani 1 1 d . . . H51 H 1.2 0.354 1.2624 0.098 Uiso 1 1 calc R . . C52 C 1.1959(5) 0.2986(3) 1.2091(6) 0.072(3) Uani 1 1 d . . . H52 H 1.2519 0.2991 1.2062 0.086 Uiso 1 1 calc R . . C53 C 1.1451(5) 0.2649(2) 1.1779(5) 0.053(2) Uani 1 1 d . . . H53 H 1.1666 0.2433 1.1533 0.063 Uiso 1 1 calc R . . C54 C 0.8334(4) 0.37950(17) 1.0022(4) 0.0304(14) Uani 1 1 d . D . C55 C 0.7652(4) 0.40509(17) 1.0022(4) 0.0306(14) Uani 1 1 d . . . C56 C 0.6956(4) 0.37899(17) 0.9968(4) 0.0324(15) Uani 1 1 d . . . C57 C 0.9219(4) 0.3905(2) 1.0028(4) 0.0393(16) Uani 1 1 d D . . C60 C 1.0862(6) 0.4125(3) 1.0023(6) 0.078(3) Uani 1 1 d D . . H60 H 1.1415 0.4197 1.0029 0.094 Uiso 1 1 calc R A 3 C63 C 0.7614(4) 0.44990(17) 1.0042(4) 0.0310(15) Uani 1 1 d . . . C64 C 0.6078(4) 0.38936(18) 0.9939(4) 0.0343(15) Uani 1 1 d . . . C65 C 0.5380(5) 0.3721(3) 0.9353(6) 0.064(2) Uani 1 1 d . . . H65 H 0.5462 0.3521 0.8979 0.077 Uiso 1 1 calc R . . C66 C 0.4559(5) 0.3838(3) 0.9311(7) 0.081(3) Uani 1 1 d . . . H66 H 0.4091 0.3708 0.8932 0.098 Uiso 1 1 calc R . . C67 C 0.4437(6) 0.4144(3) 0.9827(7) 0.081(3) Uani 1 1 d . . . H67 H 0.3884 0.4231 0.9783 0.098 Uiso 1 1 calc R . . C68 C 0.5111(6) 0.4323(3) 1.0399(7) 0.076(3) Uani 1 1 d . . . H68 H 0.502 0.4529 1.0754 0.092 Uiso 1 1 calc R . . C69 C 0.5940(5) 0.4201(3) 1.0462(5) 0.059(2) Uani 1 1 d . . . H69 H 0.6404 0.4326 1.0857 0.071 Uiso 1 1 calc R . . C70 C 0.1284(4) 0.17908(18) 0.3252(4) 0.0336(15) Uani 1 1 d . . . C71 C 0.1036(5) 0.21395(19) 0.3701(4) 0.0380(16) Uani 1 1 d . . . C72 C 0.0194(5) 0.2190(2) 0.3700(5) 0.052(2) Uani 1 1 d . . . H72 H -0.0215 0.1998 0.3425 0.062 Uiso 1 1 calc R . . C73 C -0.0047(6) 0.2520(3) 0.4100(6) 0.066(2) Uani 1 1 d . . . H73 H -0.0618 0.2553 0.408 0.079 Uiso 1 1 calc R . . C74 C 0.0560(7) 0.2804(3) 0.4532(6) 0.073(3) Uani 1 1 d . . . H74 H 0.04 0.3024 0.4813 0.088 Uiso 1 1 calc R . . C75 C 0.1392(7) 0.2760(3) 0.4542(6) 0.073(3) Uani 1 1 d . . . H75 H 0.1797 0.2953 0.4824 0.088 Uiso 1 1 calc R . . C76 C 0.1644(5) 0.2426(2) 0.4130(5) 0.056(2) Uani 1 1 d . . . H76 H 0.2214 0.2397 0.4144 0.067 Uiso 1 1 calc R . . C77 C 0.2825(4) -0.02480(17) 0.5630(4) 0.0293(14) Uani 1 1 d . . . C78 C 0.3314(5) -0.03648(18) 0.6518(4) 0.0430(18) Uani 1 1 d . . . C79 C 0.4169(6) -0.0302(3) 0.6815(6) 0.085(3) Uani 1 1 d . . . H79 H 0.4457 -0.0174 0.6471 0.102 Uiso 1 1 calc R . . C80 C 0.4626(8) -0.0435(4) 0.7666(8) 0.117(5) Uani 1 1 d . . . H80 H 0.5215 -0.0394 0.7874 0.141 Uiso 1 1 calc R . . C81 C 0.4224(10) -0.0617(4) 0.8165(7) 0.104(5) Uani 1 1 d . . . H81 H 0.453 -0.0703 0.8716 0.125 Uiso 1 1 calc R . . C82 C 0.3401(12) -0.0673(5) 0.7881(8) 0.140(6) Uani 1 1 d . . . H82 H 0.312 -0.0798 0.8235 0.168 Uiso 1 1 calc R . . C83 C 0.2925(8) -0.0549(4) 0.7047(7) 0.109(5) Uani 1 1 d . . . H83 H 0.2337 -0.0594 0.6856 0.131 Uiso 1 1 calc R . . C84 C 0.2087(4) -0.02412(17) 0.4250(4) 0.0313(14) Uani 1 1 d . . . C85 C 0.1601(5) -0.03441(19) 0.3350(5) 0.0467(19) Uani 1 1 d D . . C88 C 0.0709(9) -0.0571(4) 0.1683(8) 0.104(4) Uani 1 1 d D . . H88 H 0.0416 -0.0647 0.1122 0.125 Uiso 1 1 calc R B 1 C86A C 0.0750(8) -0.0474(4) 0.3183(8) 0.079(4) Uani 0.780(11) 1 d P C 1 H86A H 0.0487 -0.0493 0.3616 0.094 Uiso 0.780(11) 1 calc PR C 1 C87A C 0.0318(10) -0.0573(5) 0.2321(10) 0.103(6) Uani 0.780(11) 1 d P C 1 H87A H -0.0259 -0.0642 0.2177 0.123 Uiso 0.780(11) 1 calc PR C 1 C89A C 0.1552(13) -0.0451(6) 0.1911(8) 0.110(6) Uani 0.780(11) 1 d P C 1 H89A H 0.1834 -0.0452 0.1492 0.132 Uiso 0.780(11) 1 calc PR C 1 C90A C 0.2003(8) -0.0328(4) 0.2743(7) 0.070(4) Uani 0.780(11) 1 d P C 1 H90A H 0.2568 -0.0238 0.2874 0.084 Uiso 0.780(11) 1 calc PR C 1 C86B C 0.0920(19) -0.0146(10) 0.280(2) 0.048(9) Uiso 0.220(11) 1 d PD C 2 H86B H 0.0727 0.0082 0.3032 0.058 Uiso 0.220(11) 1 calc PR C 2 C87B C 0.048(2) -0.0236(12) 0.196(2) 0.059(11) Uiso 0.220(11) 1 d PD C 2 H87B H 0.0047 -0.007 0.1622 0.071 Uiso 0.220(11) 1 calc PR C 2 C89B C 0.137(3) -0.0788(15) 0.202(3) 0.075(13) Uiso 0.220(11) 1 d PD C 2 H89B H 0.1513 -0.101 0.1736 0.09 Uiso 0.220(11) 1 calc PR C 2 C90B C 0.187(2) -0.0671(11) 0.287(2) 0.047(9) Uiso 0.220(11) 1 d PD C 2 H90B H 0.239 -0.0805 0.3128 0.057 Uiso 0.220(11) 1 calc PR C 2 C58A C 0.9359(6) 0.4268(3) 0.9631(7) 0.060(3) Uani 0.856(12) 1 d P D 3 H58A H 0.8895 0.4433 0.9354 0.073 Uiso 0.856(12) 1 calc PR D 3 C59A C 1.0183(7) 0.4385(3) 0.9645(8) 0.075(4) Uani 0.856(12) 1 d P D 3 H59A H 1.0276 0.4631 0.9405 0.09 Uiso 0.856(12) 1 calc PR D 3 C61A C 1.0732(7) 0.3776(4) 1.0376(11) 0.100(6) Uani 0.856(12) 1 d P D 3 H61A H 1.1194 0.3607 1.063 0.12 Uiso 0.856(12) 1 calc PR D 3 C62A C 0.9925(6) 0.3663(3) 1.0372(8) 0.072(4) Uani 0.856(12) 1 d P D 3 H62A H 0.9852 0.3412 1.0611 0.086 Uiso 0.856(12) 1 calc PR D 3 C58B C 0.958(5) 0.424(2) 1.047(4) 0.10(3) Uiso 0.144(12) 1 d PD D 4 H58B H 0.9265 0.4401 1.0734 0.119 Uiso 0.144(12) 1 calc PR D 4 C59B C 1.041(5) 0.435(2) 1.052(4) 0.09(2) Uiso 0.144(12) 1 d PD D 4 H59B H 1.0672 0.4562 1.0871 0.102 Uiso 0.144(12) 1 calc PR D 4 C61B C 1.047(4) 0.3747(16) 0.972(3) 0.045(14) Uiso 0.144(12) 1 d PD D 4 H61B H 1.0784 0.3545 0.9549 0.053 Uiso 0.144(12) 1 calc PR D 4 C62B C 0.964(3) 0.3677(15) 0.969(3) 0.043(14) Uiso 0.144(12) 1 d PD D 4 H62B H 0.937 0.3447 0.9396 0.052 Uiso 0.144(12) 1 calc PR D 4 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 Ag1 0.0288(2) 0.0303(2) 0.0380(3) 0.0000(2) -0.0096(2) 0.0003(2) Ag2 0.0363(3) 0.0194(2) 0.0468(3) -0.0051(2) -0.0035(2) -0.0062(2) Ag3 0.0361(3) 0.0206(2) 0.0527(3) 0.0052(2) -0.0020(2) 0.0080(2) Ag4 0.0487(3) 0.0212(2) 0.0441(3) -0.0064(2) -0.0034(2) -0.0057(2) Ag5 0.0476(3) 0.0295(2) 0.0303(3) -0.0010(2) -0.0150(2) -0.0004(2) Ag6 0.0447(3) 0.0217(2) 0.0429(3) 0.0062(2) -0.0022(2) 0.0025(2) N1 0.027(3) 0.022(2) 0.034(3) -0.005(2) -0.004(2) -0.001(2) N2 0.028(3) 0.025(3) 0.032(3) -0.002(2) -0.005(2) -0.004(2) N3 0.027(3) 0.017(2) 0.050(3) -0.001(2) -0.006(2) -0.001(2) N4 0.030(3) 0.016(2) 0.050(3) -0.001(2) 0.001(2) 0.002(2) N5 0.029(3) 0.023(3) 0.039(3) 0.002(2) -0.007(2) 0.005(2) N6 0.029(3) 0.022(3) 0.042(3) 0.004(2) -0.008(2) 0.003(2) N7 0.044(3) 0.024(3) 0.027(3) -0.002(2) -0.013(2) -0.004(2) N8 0.048(3) 0.020(3) 0.031(3) -0.002(2) -0.012(2) -0.005(2) N9 0.046(3) 0.016(2) 0.040(3) -0.003(2) 0.000(3) -0.007(2) N10 0.041(3) 0.017(2) 0.042(3) 0.002(2) -0.001(3) -0.001(2) N11 0.038(3) 0.018(2) 0.031(3) 0.000(2) -0.008(2) 0.004(2) N12 0.038(3) 0.023(3) 0.030(3) 0.000(2) -0.005(2) 0.004(2) C1 0.030(3) 0.024(3) 0.028(3) -0.001(2) 0.001(3) -0.001(3) C2 0.031(3) 0.020(3) 0.025(3) -0.001(2) -0.001(3) -0.005(2) C3 0.028(3) 0.023(3) 0.030(3) 0.000(2) -0.001(3) -0.003(2) C4 0.031(4) 0.024(3) 0.045(4) 0.003(3) -0.004(3) -0.006(3) C5 0.064(5) 0.039(4) 0.056(5) 0.009(4) -0.007(4) -0.001(4) C6 0.092(7) 0.041(5) 0.080(7) 0.027(5) 0.001(5) 0.003(5) C7 0.095(8) 0.024(4) 0.111(8) 0.006(5) 0.006(6) 0.014(4) C8 0.080(7) 0.041(5) 0.085(7) -0.012(4) 0.019(5) 0.015(4) C9 0.056(5) 0.032(4) 0.053(5) 0.000(3) 0.009(4) 0.006(3) C10 0.033(4) 0.023(3) 0.031(3) -0.005(2) -0.002(3) -0.003(3) C11 0.041(4) 0.039(4) 0.050(4) 0.000(3) -0.005(3) -0.002(3) C12 0.048(5) 0.060(5) 0.065(5) -0.003(4) 0.003(4) 0.016(4) C13 0.068(6) 0.041(5) 0.063(5) 0.000(4) -0.013(4) 0.021(4) C14 0.074(6) 0.031(4) 0.060(5) 0.013(4) -0.003(4) 0.001(4) C15 0.053(4) 0.031(4) 0.035(4) 0.000(3) 0.005(3) -0.003(3) C16 0.029(3) 0.022(3) 0.023(3) -0.003(2) -0.006(2) -0.001(2) C17 0.032(3) 0.025(3) 0.029(3) 0.000(2) -0.003(3) 0.001(3) C18 0.032(3) 0.022(3) 0.031(3) -0.001(2) -0.007(3) -0.002(3) C19 0.039(4) 0.028(3) 0.038(4) 0.002(3) -0.003(3) -0.010(3) C20 0.072(6) 0.041(4) 0.044(4) 0.001(3) 0.009(4) -0.009(4) C21 0.115(9) 0.079(7) 0.046(5) -0.001(5) 0.022(5) -0.021(6) C22 0.129(10) 0.083(7) 0.053(6) 0.027(5) 0.014(6) -0.031(7) C23 0.165(12) 0.046(5) 0.077(7) 0.024(5) 0.021(7) -0.024(6) C24 0.098(7) 0.024(4) 0.055(5) 0.004(3) 0.007(5) -0.012(4) C25 0.045(4) 0.028(3) 0.026(3) -0.005(3) -0.004(3) -0.006(3) C26 0.047(4) 0.035(4) 0.039(4) 0.004(3) -0.002(3) -0.001(3) C27 0.077(6) 0.036(4) 0.048(5) 0.012(3) 0.001(4) 0.000(4) C28 0.094(7) 0.048(5) 0.046(5) 0.009(4) 0.025(5) -0.012(5) C29 0.070(6) 0.065(5) 0.048(5) -0.005(4) 0.024(4) -0.015(5) C30 0.058(5) 0.046(4) 0.037(4) -0.002(3) 0.011(4) 0.002(4) C31 0.032(3) 0.022(3) 0.029(3) 0.002(2) -0.002(3) 0.004(3) C32 0.030(3) 0.023(3) 0.027(3) -0.001(2) -0.004(3) 0.005(2) C33 0.032(3) 0.023(3) 0.035(4) 0.002(3) -0.002(3) 0.004(3) C34 0.038(4) 0.022(3) 0.043(4) -0.001(3) -0.002(3) 0.003(3) C35 0.064(5) 0.037(4) 0.048(4) 0.005(3) 0.007(4) -0.004(4) C36 0.098(8) 0.051(5) 0.080(7) 0.020(5) 0.022(6) -0.013(5) C37 0.118(9) 0.041(5) 0.108(9) -0.006(6) 0.017(7) -0.029(6) C38 0.106(8) 0.041(5) 0.086(7) -0.024(5) -0.004(6) -0.017(5) C39 0.077(6) 0.035(4) 0.050(5) -0.006(3) -0.010(4) -0.002(4) C40 0.030(3) 0.019(3) 0.030(3) 0.001(2) -0.006(3) 0.000(2) C41 0.035(4) 0.018(3) 0.034(3) 0.004(2) -0.006(3) 0.000(3) C42 0.047(4) 0.024(3) 0.032(4) -0.002(3) -0.003(3) 0.009(3) C43 0.153(10) 0.032(4) 0.052(5) -0.003(4) 0.023(6) 0.004(5) C44 0.216(16) 0.042(6) 0.086(8) -0.027(6) 0.033(9) 0.011(7) C45 0.168(13) 0.080(8) 0.050(6) -0.019(5) 0.018(7) 0.026(8) C46 0.128(10) 0.081(7) 0.050(6) -0.001(5) 0.026(6) 0.013(7) C47 0.104(7) 0.048(5) 0.043(5) 0.000(4) 0.017(5) 0.008(5) C48 0.037(4) 0.023(3) 0.042(4) 0.004(3) -0.009(3) -0.001(3) C49 0.046(5) 0.033(4) 0.074(6) -0.012(4) -0.006(4) 0.001(3) C50 0.092(8) 0.032(4) 0.098(8) -0.022(4) -0.005(6) -0.004(5) C51 0.061(6) 0.042(5) 0.118(9) -0.010(5) -0.009(6) -0.021(4) C52 0.037(5) 0.063(6) 0.099(7) 0.011(5) -0.006(4) -0.017(4) C53 0.039(4) 0.040(4) 0.071(5) 0.006(4) 0.003(4) -0.005(3) C54 0.022(3) 0.020(3) 0.043(4) 0.003(3) -0.001(3) -0.002(2) C55 0.031(3) 0.015(3) 0.038(4) 0.003(2) -0.001(3) 0.002(3) C56 0.031(3) 0.020(3) 0.035(3) -0.002(2) -0.007(3) -0.002(3) C57 0.037(4) 0.031(3) 0.044(4) -0.004(3) 0.004(3) 0.002(3) C60 0.035(5) 0.114(9) 0.086(7) 0.019(6) 0.020(5) -0.011(5) C63 0.027(3) 0.016(3) 0.044(4) 0.000(3) 0.000(3) 0.001(2) C64 0.028(3) 0.026(3) 0.047(4) 0.000(3) 0.009(3) 0.005(3) C65 0.035(4) 0.062(5) 0.083(6) -0.031(5) 0.000(4) 0.005(4) C66 0.035(5) 0.100(8) 0.096(8) -0.038(6) -0.001(5) -0.005(5) C67 0.041(5) 0.099(8) 0.100(8) -0.029(6) 0.015(5) 0.010(5) C68 0.059(6) 0.085(7) 0.093(7) -0.044(6) 0.035(5) -0.002(5) C69 0.045(5) 0.065(5) 0.066(5) -0.033(4) 0.015(4) -0.007(4) C70 0.033(4) 0.030(3) 0.030(3) 0.002(3) -0.004(3) 0.006(3) C71 0.045(4) 0.031(3) 0.029(3) -0.002(3) -0.001(3) 0.007(3) C72 0.062(5) 0.048(4) 0.040(4) -0.001(3) 0.007(4) 0.002(4) C73 0.068(6) 0.073(6) 0.058(5) -0.005(5) 0.019(5) 0.024(5) C74 0.102(8) 0.059(6) 0.054(5) -0.015(4) 0.015(5) 0.033(5) C75 0.093(8) 0.048(5) 0.065(6) -0.030(4) 0.000(5) 0.010(5) C76 0.053(5) 0.041(4) 0.057(5) -0.014(4) -0.008(4) 0.008(4) C77 0.031(3) 0.020(3) 0.035(3) 0.001(2) 0.007(3) -0.002(2) C78 0.060(5) 0.021(3) 0.036(4) -0.001(3) -0.005(3) -0.004(3) C79 0.055(6) 0.107(8) 0.073(7) 0.020(6) -0.012(5) -0.014(5) C80 0.091(9) 0.130(11) 0.087(9) 0.011(8) -0.039(7) -0.008(8) C81 0.139(12) 0.076(8) 0.063(7) 0.022(6) -0.023(8) -0.008(8) C82 0.166(15) 0.169(15) 0.069(8) 0.050(9) 0.011(9) -0.041(12) C83 0.081(8) 0.160(12) 0.075(7) 0.050(8) 0.008(6) -0.030(8) C84 0.029(3) 0.021(3) 0.038(4) 0.001(3) 0.002(3) 0.000(3) C85 0.053(5) 0.025(3) 0.048(4) 0.001(3) -0.007(4) 0.003(3) C88 0.114(10) 0.105(10) 0.058(7) -0.017(6) -0.029(7) -0.003(8) C86A 0.061(8) 0.092(10) 0.064(8) 0.012(7) -0.011(6) -0.014(7) C87A 0.084(10) 0.113(13) 0.078(10) 0.005(9) -0.025(8) -0.042(9) C89A 0.160(17) 0.125(15) 0.040(7) -0.013(8) 0.024(9) 0.008(12) C90A 0.073(8) 0.087(10) 0.045(6) -0.004(6) 0.011(6) -0.005(7) C58A 0.042(6) 0.055(6) 0.084(8) 0.025(5) 0.019(5) 0.000(4) C59A 0.063(7) 0.073(7) 0.092(9) 0.028(6) 0.028(6) -0.013(6) C61A 0.029(6) 0.116(11) 0.151(15) 0.071(10) 0.024(7) 0.014(6) C62A 0.045(6) 0.052(6) 0.110(10) 0.038(6) 0.012(6) 0.010(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ag1 N5 2.087(5) . ? Ag1 N2 2.093(5) . ? Ag2 N1 2.079(5) . ? Ag2 N3 2.080(5) . ? Ag2 Ag3 3.3087(7) . ? Ag3 N6 2.079(5) . ? Ag3 N4 2.091(5) . ? Ag4 N9 2.085(5) . ? Ag4 N8 2.089(5) . ? Ag5 N12 2.062(5) . ? Ag5 N7 2.075(5) . ? Ag6 N10 2.080(5) . ? Ag6 N11 2.106(5) . ? N1 C1 1.332(7) . ? N1 N2 1.373(7) . ? N2 C3 1.339(7) . ? N3 C56 1.361(7) . ? N3 N4 1.369(7) . ? N4 C54 1.343(7) . ? N5 C31 1.350(7) . ? N5 N6 1.374(7) . ? N6 C33 1.342(7) . ? N7 C17 1.333(7) . ? N7 N8 1.368(7) . ? N8 C18 1.354(7) . ? N9 C77 1.346(7) . ? N9 N10 1.368(7) . ? N10 C84 1.347(7) . ? N11 C41 1.354(7) 1_454 ? N11 N12 1.373(7) . ? N12 C70 1.353(7) . ? C1 C2 1.405(8) . ? C1 C10 1.486(8) . ? C2 C3 1.394(8) . ? C2 C16 1.479(7) . ? C3 C4 1.483(8) . ? C4 C5 1.373(10) . ? C4 C9 1.385(10) . ? C5 C6 1.387(11) . ? C5 H5 0.93 . ? C6 C7 1.380(14) . ? C6 H6 0.93 . ? C7 C8 1.370(13) . ? C7 H7 0.93 . ? C8 C9 1.382(10) . ? C8 H8 0.93 . ? C9 H9 0.93 . ? C10 C11 1.383(10) . ? C10 C15 1.394(9) . ? C11 C12 1.383(10) . ? C11 H11 0.93 . ? C12 C13 1.362(12) . ? C12 H12 0.93 . ? C13 C14 1.353(12) . ? C13 H13 0.93 . ? C14 C15 1.385(10) . ? C14 H14 0.93 . ? C15 H15 0.93 . ? C16 C18 1.399(8) . ? C16 C17 1.401(8) . ? C17 C25 1.461(9) . ? C18 C19 1.472(9) . ? C19 C20 1.381(10) . ? C19 C24 1.382(9) . ? C20 C21 1.379(11) . ? C20 H20 0.93 . ? C21 C22 1.361(13) . ? C21 H21 0.93 . ? C22 C23 1.377(15) . ? C22 H22 0.93 . ? C23 C24 1.384(12) . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 C26 1.380(9) . ? C25 C30 1.401(10) . ? C26 C27 1.392(10) . ? C26 H26 0.93 . ? C27 C28 1.338(12) . ? C27 H27 0.93 . ? C28 C29 1.387(12) . ? C28 H28 0.93 . ? C29 C30 1.387(11) . ? C29 H29 0.93 . ? C30 H30 0.93 . ? C31 C32 1.381(8) . ? C31 C34 1.480(8) . ? C32 C33 1.397(8) . ? C32 C40 1.486(8) . ? C33 C48 1.484(8) . ? C34 C39 1.383(9) . ? C34 C35 1.401(10) . ? C35 C36 1.385(11) . ? C35 H35 0.93 . ? C36 C37 1.369(14) . ? C36 H36 0.93 . ? C37 C38 1.349(14) . ? C37 H37 0.93 . ? C38 C39 1.383(11) . ? C38 H38 0.93 . ? C39 H39 0.93 . ? C40 C70 1.393(8) 1_656 ? C40 C41 1.397(8) . ? C41 N11 1.354(7) 1_656 ? C41 C42 1.465(9) . ? C42 C47 1.351(10) . ? C42 C43 1.380(10) . ? C43 C44 1.400(13) . ? C43 H43 0.93 . ? C44 C45 1.367(16) . ? C44 H44 0.93 . ? C45 C46 1.337(14) . ? C45 H45 0.93 . ? C46 C47 1.382(12) . ? C46 H46 0.93 . ? C47 H47 0.93 . ? C48 C49 1.371(10) . ? C48 C53 1.390(10) . ? C49 C50 1.401(11) . ? C49 H49 0.93 . ? C50 C51 1.389(14) . ? C50 H50 0.93 . ? C51 C52 1.365(13) . ? C51 H51 0.93 . ? C52 C53 1.383(11) . ? C52 H52 0.93 . ? C53 H53 0.93 . ? C54 C55 1.395(8) . ? C54 C57 1.487(9) . ? C55 C56 1.403(9) . ? C55 C63 1.470(8) . ? C56 C64 1.462(9) . ? C57 C62B 1.25(5) . ? C57 C58B 1.34(9) . ? C57 C62A 1.375(11) . ? C57 C58A 1.403(11) . ? C60 C61A 1.325(15) . ? C60 C59A 1.386(14) . ? C60 C61B 1.41(5) . ? C60 C59B 1.44(8) . ? C60 H60 0.93 . ? C63 C77 1.388(8) 2_656 ? C63 C84 1.397(8) 2_656 ? C64 C65 1.372(9) . ? C64 C69 1.378(10) . ? C65 C66 1.376(11) . ? C65 H65 0.93 . ? C66 C67 1.360(13) . ? C66 H66 0.93 . ? C67 C68 1.345(12) . ? C67 H67 0.93 . ? C68 C69 1.387(12) . ? C68 H68 0.93 . ? C69 H69 0.93 . ? C70 C40 1.393(8) 1_454 ? C70 C71 1.476(9) . ? C71 C72 1.385(11) . ? C71 C76 1.392(10) . ? C72 C73 1.379(11) . ? C72 H72 0.93 . ? C73 C74 1.388(13) . ? C73 H73 0.93 . ? C74 C75 1.361(14) . ? C74 H74 0.93 . ? C75 C76 1.408(11) . ? C75 H75 0.93 . ? C76 H76 0.93 . ? C77 C63 1.388(8) 2_646 ? C77 C78 1.477(9) . ? C78 C79 1.351(11) . ? C78 C83 1.353(12) . ? C79 C80 1.431(14) . ? C79 H79 0.93 . ? C80 C81 1.328(18) . ? C80 H80 0.93 . ? C81 C82 1.298(19) . ? C81 H81 0.93 . ? C82 C83 1.408(15) . ? C82 H82 0.93 . ? C83 H83 0.93 . ? C84 C63 1.397(8) 2_646 ? C84 C85 1.480(9) . ? C85 C90A 1.340(14) . ? C85 C86B 1.36(3) . ? C85 C86A 1.401(14) . ? C85 C90B 1.47(4) . ? C88 C89B 1.27(5) . ? C88 C87B 1.28(4) . ? C88 C87A 1.37(2) . ? C88 C89A 1.37(2) . ? C88 H88 0.93 . ? C86A C87A 1.406(18) . ? C86A H86A 0.93 . ? C87A H87A 0.93 . ? C89A C90A 1.394(17) . ? C89A H89A 0.93 . ? C90A H90A 0.93 . ? C86B C87B 1.38(5) . ? C86B H86B 0.93 . ? C87B H87B 0.93 . ? C89B C90B 1.44(6) . ? C89B H89B 0.93 . ? C90B H90B 0.93 . ? C58A C59A 1.394(14) . ? C58A H58A 0.93 . ? C59A H59A 0.93 . ? C61A C62A 1.368(14) . ? C61A H61A 0.93 . ? C62A H62A 0.93 . ? C58B C59B 1.38(10) . ? C58B H58B 0.93 . ? C59B H59B 0.93 . ? C61B C62B 1.36(7) . ? C61B H61B 0.93 . ? C62B H62B 0.93 . ? 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 N5 Ag1 N2 174.66(19) . . ? N1 Ag2 N3 174.1(2) . . ? N1 Ag2 Ag3 117.20(14) . . ? N3 Ag2 Ag3 60.65(14) . . ? N6 Ag3 N4 172.5(2) . . ? N6 Ag3 Ag2 118.90(14) . . ? N4 Ag3 Ag2 60.78(14) . . ? N9 Ag4 N8 172.1(2) . . ? N12 Ag5 N7 177.66(19) . . ? N10 Ag6 N11 170.9(2) . . ? C1 N1 N2 108.6(4) . . ? C1 N1 Ag2 127.4(4) . . ? N2 N1 Ag2 124.0(3) . . ? C3 N2 N1 108.0(4) . . ? C3 N2 Ag1 133.3(4) . . ? N1 N2 Ag1 117.8(3) . . ? C56 N3 N4 108.6(5) . . ? C56 N3 Ag2 133.8(4) . . ? N4 N3 Ag2 114.6(4) . . ? C54 N4 N3 108.4(5) . . ? C54 N4 Ag3 134.0(4) . . ? N3 N4 Ag3 113.5(4) . . ? C31 N5 N6 107.1(5) . . ? C31 N5 Ag1 134.2(4) . . ? N6 N5 Ag1 118.3(3) . . ? C33 N6 N5 108.9(5) . . ? C33 N6 Ag3 127.8(4) . . ? N5 N6 Ag3 123.3(3) . . ? C17 N7 N8 109.0(5) . . ? C17 N7 Ag5 130.3(4) . . ? N8 N7 Ag5 120.4(4) . . ? C18 N8 N7 108.1(5) . . ? C18 N8 Ag4 130.4(4) . . ? N7 N8 Ag4 110.8(4) . . ? C77 N9 N10 108.6(5) . . ? C77 N9 Ag4 126.3(4) . . ? N10 N9 Ag4 123.2(4) . . ? C84 N10 N9 107.8(5) . . ? C84 N10 Ag6 128.7(4) . . ? N9 N10 Ag6 123.2(4) . . ? C41 N11 N12 108.1(5) 1_454 . ? C41 N11 Ag6 127.5(4) 1_454 . ? N12 N11 Ag6 108.8(4) . . ? C70 N12 N11 108.0(5) . . ? C70 N12 Ag5 130.5(4) . . ? N11 N12 Ag5 121.3(4) . . ? N1 C1 C2 109.3(5) . . ? N1 C1 C10 121.0(5) . . ? C2 C1 C10 129.7(5) . . ? C3 C2 C1 104.4(5) . . ? C3 C2 C16 127.2(5) . . ? C1 C2 C16 128.2(5) . . ? N2 C3 C2 109.6(5) . . ? N2 C3 C4 121.6(5) . . ? C2 C3 C4 128.7(5) . . ? C5 C4 C9 118.8(6) . . ? C5 C4 C3 121.3(6) . . ? C9 C4 C3 119.9(6) . . ? C4 C5 C6 120.5(8) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 120.3(8) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 119.3(8) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 120.5(8) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C4 120.6(7) . . ? C8 C9 H9 119.7 . . ? C4 C9 H9 119.7 . . ? C11 C10 C15 119.3(6) . . ? C11 C10 C1 121.2(6) . . ? C15 C10 C1 119.5(6) . . ? C10 C11 C12 119.7(7) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 120.6(8) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 120.2(7) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 121.0(8) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C10 119.2(7) . . ? C14 C15 H15 120.4 . . ? C10 C15 H15 120.4 . . ? C18 C16 C17 105.1(5) . . ? C18 C16 C2 129.0(5) . . ? C17 C16 C2 125.8(5) . . ? N7 C17 C16 109.1(5) . . ? N7 C17 C25 120.9(5) . . ? C16 C17 C25 130.0(5) . . ? N8 C18 C16 108.8(5) . . ? N8 C18 C19 121.6(5) . . ? C16 C18 C19 129.4(5) . . ? C20 C19 C24 118.8(7) . . ? C20 C19 C18 119.0(6) . . ? C24 C19 C18 122.2(7) . . ? C21 C20 C19 120.7(8) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C22 C21 C20 120.3(9) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 119.7(9) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C24 120.4(9) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 120.0(9) . . ? C19 C24 H24 120 . . ? C23 C24 H24 120 . . ? C26 C25 C30 118.1(6) . . ? C26 C25 C17 121.5(7) . . ? C30 C25 C17 120.5(6) . . ? C25 C26 C27 120.7(7) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C28 C27 C26 120.4(8) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 121.1(8) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 119.0(8) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C25 120.7(7) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? N5 C31 C32 110.1(5) . . ? N5 C31 C34 120.9(5) . . ? C32 C31 C34 128.9(5) . . ? C31 C32 C33 105.0(5) . . ? C31 C32 C40 127.0(5) . . ? C33 C32 C40 127.8(5) . . ? N6 C33 C32 108.9(5) . . ? N6 C33 C48 120.4(5) . . ? C32 C33 C48 130.7(5) . . ? C39 C34 C35 117.9(6) . . ? C39 C34 C31 122.2(6) . . ? C35 C34 C31 119.9(6) . . ? C36 C35 C34 120.5(8) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C35 119.5(9) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C38 C37 C36 121.2(9) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 120.1(9) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C34 C39 C38 120.8(8) . . ? C34 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C70 C40 C41 105.0(5) 1_656 . ? C70 C40 C32 126.5(5) 1_656 . ? C41 C40 C32 128.2(5) . . ? N11 C41 C40 109.3(5) 1_656 . ? N11 C41 C42 121.1(5) 1_656 . ? C40 C41 C42 129.1(5) . . ? C47 C42 C43 116.9(7) . . ? C47 C42 C41 120.0(6) . . ? C43 C42 C41 123.0(7) . . ? C42 C43 C44 120.2(9) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 120.5(9) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C46 C45 C44 119.0(10) . . ? C46 C45 H45 120.5 . . ? C44 C45 H45 120.5 . . ? C45 C46 C47 120.3(10) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C42 C47 C46 122.8(8) . . ? C42 C47 H47 118.6 . . ? C46 C47 H47 118.6 . . ? C49 C48 C53 119.2(6) . . ? C49 C48 C33 120.0(7) . . ? C53 C48 C33 120.8(6) . . ? C48 C49 C50 120.5(8) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C51 C50 C49 120.0(9) . . ? C51 C50 H50 120 . . ? C49 C50 H50 120 . . ? C52 C51 C50 118.8(8) . . ? C52 C51 H51 120.6 . . ? C50 C51 H51 120.6 . . ? C51 C52 C53 121.6(9) . . ? C51 C52 H52 119.2 . . ? C53 C52 H52 119.2 . . ? C52 C53 C48 119.9(8) . . ? C52 C53 H53 120.1 . . ? C48 C53 H53 120.1 . . ? N4 C54 C55 109.4(5) . . ? N4 C54 C57 121.6(5) . . ? C55 C54 C57 129.0(5) . . ? C54 C55 C56 105.5(5) . . ? C54 C55 C63 129.7(6) . . ? C56 C55 C63 124.8(6) . . ? N3 C56 C55 108.1(5) . . ? N3 C56 C64 122.9(5) . . ? C55 C56 C64 129.0(5) . . ? C62B C57 C58B 121(5) . . ? C62B C57 C62A 48(2) . . ? C58B C57 C62A 94(3) . . ? C62B C57 C58A 97(2) . . ? C58B C57 C58A 56(2) . . ? C62A C57 C58A 116.4(8) . . ? C62B C57 C54 121(3) . . ? C58B C57 C54 118(4) . . ? C62A C57 C54 123.9(7) . . ? C58A C57 C54 119.6(6) . . ? C61A C60 C59A 120.6(9) . . ? C61A C60 C61B 44(2) . . ? C59A C60 C61B 100(2) . . ? C61A C60 C59B 91(3) . . ? C59A C60 C59B 57(2) . . ? C61B C60 C59B 112(4) . . ? C61A C60 H60 119.7 . . ? C59A C60 H60 119.7 . . ? C61B C60 H60 124.2 . . ? C59B C60 H60 121.8 . . ? C77 C63 C84 104.9(5) 2_656 2_656 ? C77 C63 C55 126.5(5) 2_656 . ? C84 C63 C55 128.3(5) 2_656 . ? C65 C64 C69 118.3(7) . . ? C65 C64 C56 122.1(6) . . ? C69 C64 C56 119.4(6) . . ? C64 C65 C66 121.1(8) . . ? C64 C65 H65 119.5 . . ? C66 C65 H65 119.5 . . ? C67 C66 C65 119.7(8) . . ? C67 C66 H66 120.2 . . ? C65 C66 H66 120.2 . . ? C68 C67 C66 120.4(9) . . ? C68 C67 H67 119.8 . . ? C66 C67 H67 119.8 . . ? C67 C68 C69 120.4(8) . . ? C67 C68 H68 119.8 . . ? C69 C68 H68 119.8 . . ? C64 C69 C68 120.1(7) . . ? C64 C69 H69 120 . . ? C68 C69 H69 120 . . ? N12 C70 C40 109.5(5) . 1_454 ? N12 C70 C71 121.6(5) . . ? C40 C70 C71 128.9(5) 1_454 . ? C72 C71 C76 118.8(7) . . ? C72 C71 C70 120.6(6) . . ? C76 C71 C70 120.6(7) . . ? C73 C72 C71 121.0(8) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? C72 C73 C74 120.2(9) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C75 C74 C73 119.6(8) . . ? C75 C74 H74 120.2 . . ? C73 C74 H74 120.2 . . ? C74 C75 C76 120.7(8) . . ? C74 C75 H75 119.7 . . ? C76 C75 H75 119.7 . . ? C71 C76 C75 119.7(8) . . ? C71 C76 H76 120.2 . . ? C75 C76 H76 120.2 . . ? N9 C77 C63 109.3(5) . 2_646 ? N9 C77 C78 122.5(5) . . ? C63 C77 C78 128.1(5) 2_646 . ? C79 C78 C83 118.2(8) . . ? C79 C78 C77 120.6(7) . . ? C83 C78 C77 121.2(7) . . ? C78 C79 C80 118.9(11) . . ? C78 C79 H79 120.5 . . ? C80 C79 H79 120.5 . . ? C81 C80 C79 121.2(12) . . ? C81 C80 H80 119.4 . . ? C79 C80 H80 119.4 . . ? C82 C81 C80 119.7(11) . . ? C82 C81 H81 120.1 . . ? C80 C81 H81 120.1 . . ? C81 C82 C83 121.1(13) . . ? C81 C82 H82 119.5 . . ? C83 C82 H82 119.5 . . ? C78 C83 C82 120.9(11) . . ? C78 C83 H83 119.6 . . ? C82 C83 H83 119.6 . . ? N10 C84 C63 109.5(5) . 2_646 ? N10 C84 C85 121.6(5) . . ? C63 C84 C85 128.9(5) 2_646 . ? C90A C85 C86B 89.2(14) . . ? C90A C85 C86A 123.1(9) . . ? C86B C85 C86A 56.5(11) . . ? C90A C85 C90B 49.1(13) . . ? C86B C85 C90B 109(2) . . ? C86A C85 C90B 96.8(15) . . ? C90A C85 C84 118.8(8) . . ? C86B C85 C84 129.0(16) . . ? C86A C85 C84 118.0(9) . . ? C90B C85 C84 122.0(15) . . ? C89B C88 C87B 129(3) . . ? C89B C88 C87A 101(2) . . ? C87B C88 C87A 59.0(16) . . ? C89B C88 C89A 52(2) . . ? C87B C88 C89A 92.3(19) . . ? C87A C88 C89A 117.0(11) . . ? C89B C88 H88 113.3 . . ? C87B C88 H88 117.1 . . ? C87A C88 H88 121.5 . . ? C89A C88 H88 121.5 . . ? C85 C86A C87A 115.9(13) . . ? C85 C86A H86A 122.1 . . ? C87A C86A H86A 122.1 . . ? C88 C87A C86A 123.0(13) . . ? C88 C87A H87A 118.5 . . ? C86A C87A H87A 118.5 . . ? C88 C89A C90A 122.8(15) . . ? C88 C89A H89A 118.6 . . ? C90A C89A H89A 118.6 . . ? C85 C90A C89A 118.0(13) . . ? C85 C90A H90A 121 . . ? C89A C90A H90A 121 . . ? C85 C86B C87B 129(3) . . ? C85 C86B H86B 115.4 . . ? C87B C86B H86B 115.4 . . ? C88 C87B C86B 114(3) . . ? C88 C87B H87B 122.9 . . ? C86B C87B H87B 122.9 . . ? C88 C89B C90B 116(4) . . ? C88 C89B H89B 122.1 . . ? C90B C89B H89B 122.1 . . ? C89B C90B C85 122(3) . . ? C89B C90B H90B 119.2 . . ? C85 C90B H90B 119.2 . . ? C59A C58A C57 120.9(9) . . ? C59A C58A H58A 119.5 . . ? C57 C58A H58A 119.5 . . ? C60 C59A C58A 118.7(9) . . ? C60 C59A H59A 120.6 . . ? C58A C59A H59A 120.6 . . ? C60 C61A C62A 120.9(10) . . ? C60 C61A H61A 119.6 . . ? C62A C61A H61A 119.6 . . ? C61A C62A C57 122.3(9) . . ? C61A C62A H62A 118.8 . . ? C57 C62A H62A 118.8 . . ? C57 C58B C59B 121(7) . . ? C57 C58B H58B 119.7 . . ? C59B C58B H58B 119.7 . . ? C58B C59B C60 120(7) . . ? C58B C59B H59B 120 . . ? C60 C59B H59B 120 . . ? C62B C61B C60 120(5) . . ? C62B C61B H61B 119.9 . . ? C60 C61B H61B 119.9 . . ? C57 C62B C61B 124(5) . . ? C57 C62B H62B 118.1 . . ? C61B C62B H62B 118.1 . . ? 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 N1 Ag2 Ag3 N6 -31.0(2) . . . . ? N3 Ag2 Ag3 N6 155.3(3) . . . . ? N1 Ag2 Ag3 N4 157.6(2) . . . . ? N3 Ag2 Ag3 N4 -16.2(3) . . . . ? N3 Ag2 N1 C1 -90.9(19) . . . . ? Ag3 Ag2 N1 C1 -158.2(5) . . . . ? N3 Ag2 N1 N2 90.4(19) . . . . ? Ag3 Ag2 N1 N2 23.2(5) . . . . ? C1 N1 N2 C3 1.6(7) . . . . ? Ag2 N1 N2 C3 -179.6(4) . . . . ? C1 N1 N2 Ag1 172.0(4) . . . . ? Ag2 N1 N2 Ag1 -9.2(6) . . . . ? N5 Ag1 N2 C3 158(2) . . . . ? N5 Ag1 N2 N1 -9(3) . . . . ? N1 Ag2 N3 C56 111.4(18) . . . . ? Ag3 Ag2 N3 C56 -178.4(7) . . . . ? N1 Ag2 N3 N4 -46(2) . . . . ? Ag3 Ag2 N3 N4 24.1(3) . . . . ? C56 N3 N4 C54 -1.5(7) . . . . ? Ag2 N3 N4 C54 161.5(4) . . . . ? C56 N3 N4 Ag3 159.0(4) . . . . ? Ag2 N3 N4 Ag3 -38.0(5) . . . . ? N6 Ag3 N4 C54 88.1(17) . . . . ? Ag2 Ag3 N4 C54 177.8(7) . . . . ? N6 Ag3 N4 N3 -65.9(16) . . . . ? Ag2 Ag3 N4 N3 23.8(3) . . . . ? N2 Ag1 N5 C31 176(2) . . . . ? N2 Ag1 N5 N6 4(3) . . . . ? C31 N5 N6 C33 0.2(7) . . . . ? Ag1 N5 N6 C33 174.3(4) . . . . ? C31 N5 N6 Ag3 -177.4(4) . . . . ? Ag1 N5 N6 Ag3 -3.3(7) . . . . ? N4 Ag3 N6 C33 -74.9(17) . . . . ? Ag2 Ag3 N6 C33 -160.4(5) . . . . ? N4 Ag3 N6 N5 102.2(15) . . . . ? Ag2 Ag3 N6 N5 16.7(6) . . . . ? N12 Ag5 N7 C17 162(5) . . . . ? N12 Ag5 N7 N8 -26(6) . . . . ? C17 N7 N8 C18 0.6(7) . . . . ? Ag5 N7 N8 C18 -173.1(4) . . . . ? C17 N7 N8 Ag4 -148.1(4) . . . . ? Ag5 N7 N8 Ag4 38.3(6) . . . . ? N9 Ag4 N8 C18 -121.8(14) . . . . ? N9 Ag4 N8 N7 17.7(17) . . . . ? N8 Ag4 N9 C77 146.0(13) . . . . ? N8 Ag4 N9 N10 -51.4(18) . . . . ? C77 N9 N10 C84 0.2(8) . . . . ? Ag4 N9 N10 C84 -165.1(4) . . . . ? C77 N9 N10 Ag6 -173.8(4) . . . . ? Ag4 N9 N10 Ag6 21.0(7) . . . . ? N11 Ag6 N10 C84 129.4(12) . . . . ? N11 Ag6 N10 N9 -58.0(15) . . . . ? N10 Ag6 N11 C41 -111.0(12) . . . 1_454 ? N10 Ag6 N11 N12 21.5(15) . . . . ? C41 N11 N12 C70 0.4(7) 1_454 . . . ? Ag6 N11 N12 C70 -141.6(4) . . . . ? C41 N11 N12 Ag5 -176.4(4) 1_454 . . . ? Ag6 N11 N12 Ag5 41.6(5) . . . . ? N7 Ag5 N12 C70 137(6) . . . . ? N7 Ag5 N12 N11 -47(6) . . . . ? N2 N1 C1 C2 -1.2(7) . . . . ? Ag2 N1 C1 C2 180.0(4) . . . . ? N2 N1 C1 C10 178.7(6) . . . . ? Ag2 N1 C1 C10 -0.1(9) . . . . ? N1 C1 C2 C3 0.4(7) . . . . ? C10 C1 C2 C3 -179.5(7) . . . . ? N1 C1 C2 C16 -175.3(6) . . . . ? C10 C1 C2 C16 4.8(12) . . . . ? N1 N2 C3 C2 -1.3(7) . . . . ? Ag1 N2 C3 C2 -169.7(5) . . . . ? N1 N2 C3 C4 178.6(6) . . . . ? Ag1 N2 C3 C4 10.2(10) . . . . ? C1 C2 C3 N2 0.6(7) . . . . ? C16 C2 C3 N2 176.4(6) . . . . ? C1 C2 C3 C4 -179.3(7) . . . . ? C16 C2 C3 C4 -3.5(11) . . . . ? N2 C3 C4 C5 50.5(10) . . . . ? C2 C3 C4 C5 -129.7(8) . . . . ? N2 C3 C4 C9 -130.6(7) . . . . ? C2 C3 C4 C9 49.3(10) . . . . ? C9 C4 C5 C6 -2.9(12) . . . . ? C3 C4 C5 C6 176.1(8) . . . . ? C4 C5 C6 C7 3.6(15) . . . . ? C5 C6 C7 C8 -2.3(16) . . . . ? C6 C7 C8 C9 0.3(16) . . . . ? C7 C8 C9 C4 0.3(14) . . . . ? C5 C4 C9 C8 1.0(12) . . . . ? C3 C4 C9 C8 -178.0(7) . . . . ? N1 C1 C10 C11 -124.2(7) . . . . ? C2 C1 C10 C11 55.6(10) . . . . ? N1 C1 C10 C15 55.9(9) . . . . ? C2 C1 C10 C15 -124.2(7) . . . . ? C15 C10 C11 C12 -0.4(10) . . . . ? C1 C10 C11 C12 179.7(6) . . . . ? C10 C11 C12 C13 0.9(12) . . . . ? C11 C12 C13 C14 -0.9(13) . . . . ? C12 C13 C14 C15 0.3(13) . . . . ? C13 C14 C15 C10 0.1(11) . . . . ? C11 C10 C15 C14 -0.1(10) . . . . ? C1 C10 C15 C14 179.8(6) . . . . ? C3 C2 C16 C18 48.0(11) . . . . ? C1 C2 C16 C18 -137.2(7) . . . . ? C3 C2 C16 C17 -126.0(7) . . . . ? C1 C2 C16 C17 48.8(10) . . . . ? N8 N7 C17 C16 -0.1(7) . . . . ? Ag5 N7 C17 C16 172.8(5) . . . . ? N8 N7 C17 C25 179.8(6) . . . . ? Ag5 N7 C17 C25 -7.4(10) . . . . ? C18 C16 C17 N7 -0.4(7) . . . . ? C2 C16 C17 N7 174.8(6) . . . . ? C18 C16 C17 C25 179.8(7) . . . . ? C2 C16 C17 C25 -5.0(11) . . . . ? N7 N8 C18 C16 -0.8(7) . . . . ? Ag4 N8 C18 C16 139.4(5) . . . . ? N7 N8 C18 C19 174.0(6) . . . . ? Ag4 N8 C18 C19 -45.8(9) . . . . ? C17 C16 C18 N8 0.8(7) . . . . ? C2 C16 C18 N8 -174.2(6) . . . . ? C17 C16 C18 C19 -173.5(7) . . . . ? C2 C16 C18 C19 11.5(11) . . . . ? N8 C18 C19 C20 -129.1(7) . . . . ? C16 C18 C19 C20 44.5(11) . . . . ? N8 C18 C19 C24 51.2(10) . . . . ? C16 C18 C19 C24 -135.1(8) . . . . ? C24 C19 C20 C21 -2.3(12) . . . . ? C18 C19 C20 C21 178.0(8) . . . . ? C19 C20 C21 C22 0.5(15) . . . . ? C20 C21 C22 C23 1.0(18) . . . . ? C21 C22 C23 C24 -0.6(19) . . . . ? C20 C19 C24 C23 2.6(13) . . . . ? C18 C19 C24 C23 -177.7(9) . . . . ? C22 C23 C24 C19 -1.2(17) . . . . ? N7 C17 C25 C26 56.7(9) . . . . ? C16 C17 C25 C26 -123.5(8) . . . . ? N7 C17 C25 C30 -123.7(7) . . . . ? C16 C17 C25 C30 56.0(10) . . . . ? C30 C25 C26 C27 -0.4(10) . . . . ? C17 C25 C26 C27 179.2(6) . . . . ? C25 C26 C27 C28 0.8(12) . . . . ? C26 C27 C28 C29 -1.6(13) . . . . ? C27 C28 C29 C30 1.9(13) . . . . ? C28 C29 C30 C25 -1.5(11) . . . . ? C26 C25 C30 C29 0.7(10) . . . . ? C17 C25 C30 C29 -178.8(6) . . . . ? N6 N5 C31 C32 -0.7(7) . . . . ? Ag1 N5 C31 C32 -173.5(5) . . . . ? N6 N5 C31 C34 176.1(6) . . . . ? Ag1 N5 C31 C34 3.4(10) . . . . ? N5 C31 C32 C33 1.0(8) . . . . ? C34 C31 C32 C33 -175.6(7) . . . . ? N5 C31 C32 C40 176.5(6) . . . . ? C34 C31 C32 C40 -0.1(12) . . . . ? N5 N6 C33 C32 0.4(8) . . . . ? Ag3 N6 C33 C32 177.9(5) . . . . ? N5 N6 C33 C48 -178.8(6) . . . . ? Ag3 N6 C33 C48 -1.3(10) . . . . ? C31 C32 C33 N6 -0.8(8) . . . . ? C40 C32 C33 N6 -176.3(6) . . . . ? C31 C32 C33 C48 178.3(7) . . . . ? C40 C32 C33 C48 2.8(12) . . . . ? N5 C31 C34 C39 48.4(10) . . . . ? C32 C31 C34 C39 -135.4(8) . . . . ? N5 C31 C34 C35 -130.5(7) . . . . ? C32 C31 C34 C35 45.7(11) . . . . ? C39 C34 C35 C36 0.9(12) . . . . ? C31 C34 C35 C36 179.9(8) . . . . ? C34 C35 C36 C37 0.1(15) . . . . ? C35 C36 C37 C38 0.4(18) . . . . ? C36 C37 C38 C39 -1.9(19) . . . . ? C35 C34 C39 C38 -2.4(13) . . . . ? C31 C34 C39 C38 178.7(8) . . . . ? C37 C38 C39 C34 2.9(16) . . . . ? C31 C32 C40 C70 -123.1(8) . . . 1_656 ? C33 C32 C40 C70 51.4(11) . . . 1_656 ? C31 C32 C40 C41 49.8(11) . . . . ? C33 C32 C40 C41 -135.7(7) . . . . ? C70 C40 C41 N11 0.1(7) 1_656 . . 1_656 ? C32 C40 C41 N11 -173.9(6) . . . 1_656 ? C70 C40 C41 C42 -172.4(7) 1_656 . . . ? C32 C40 C41 C42 13.5(11) . . . . ? N11 C41 C42 C47 -122.9(8) 1_656 . . . ? C40 C41 C42 C47 48.9(11) . . . . ? N11 C41 C42 C43 59.6(11) 1_656 . . . ? C40 C41 C42 C43 -128.6(9) . . . . ? C47 C42 C43 C44 4.3(15) . . . . ? C41 C42 C43 C44 -178.1(10) . . . . ? C42 C43 C44 C45 -1(2) . . . . ? C43 C44 C45 C46 -4(2) . . . . ? C44 C45 C46 C47 5(2) . . . . ? C43 C42 C47 C46 -3.2(14) . . . . ? C41 C42 C47 C46 179.1(9) . . . . ? C45 C46 C47 C42 -1.6(18) . . . . ? N6 C33 C48 C49 56.4(10) . . . . ? C32 C33 C48 C49 -122.5(8) . . . . ? N6 C33 C48 C53 -125.0(7) . . . . ? C32 C33 C48 C53 56.1(11) . . . . ? C53 C48 C49 C50 0.2(12) . . . . ? C33 C48 C49 C50 178.8(7) . . . . ? C48 C49 C50 C51 1.1(14) . . . . ? C49 C50 C51 C52 -2.5(15) . . . . ? C50 C51 C52 C53 2.7(15) . . . . ? C51 C52 C53 C48 -1.4(14) . . . . ? C49 C48 C53 C52 -0.1(11) . . . . ? C33 C48 C53 C52 -178.7(7) . . . . ? N3 N4 C54 C55 1.5(7) . . . . ? Ag3 N4 C54 C55 -153.5(5) . . . . ? N3 N4 C54 C57 -176.4(6) . . . . ? Ag3 N4 C54 C57 28.6(10) . . . . ? N4 C54 C55 C56 -0.8(7) . . . . ? C57 C54 C55 C56 176.9(6) . . . . ? N4 C54 C55 C63 -178.7(6) . . . . ? C57 C54 C55 C63 -1.0(11) . . . . ? N4 N3 C56 C55 1.0(7) . . . . ? Ag2 N3 C56 C55 -157.4(5) . . . . ? N4 N3 C56 C64 -179.5(6) . . . . ? Ag2 N3 C56 C64 22.1(10) . . . . ? C54 C55 C56 N3 -0.1(7) . . . . ? C63 C55 C56 N3 177.9(6) . . . . ? C54 C55 C56 C64 -179.6(6) . . . . ? C63 C55 C56 C64 -1.6(11) . . . . ? N4 C54 C57 C62B 27(3) . . . . ? C55 C54 C57 C62B -151(3) . . . . ? N4 C54 C57 C58B -148(2) . . . . ? C55 C54 C57 C58B 34(2) . . . . ? N4 C54 C57 C62A -30.5(12) . . . . ? C55 C54 C57 C62A 152.0(9) . . . . ? N4 C54 C57 C58A 146.5(8) . . . . ? C55 C54 C57 C58A -31.0(11) . . . . ? C54 C55 C63 C77 109.2(8) . . . 2_656 ? C56 C55 C63 C77 -68.4(10) . . . 2_656 ? C54 C55 C63 C84 -79.3(10) . . . 2_656 ? C56 C55 C63 C84 103.2(8) . . . 2_656 ? N3 C56 C64 C65 -46.1(10) . . . . ? C55 C56 C64 C65 133.3(8) . . . . ? N3 C56 C64 C69 139.9(7) . . . . ? C55 C56 C64 C69 -40.7(11) . . . . ? C69 C64 C65 C66 -2.7(14) . . . . ? C56 C64 C65 C66 -176.8(9) . . . . ? C64 C65 C66 C67 3.5(17) . . . . ? C65 C66 C67 C68 -2.6(18) . . . . ? C66 C67 C68 C69 1.0(18) . . . . ? C65 C64 C69 C68 1.1(13) . . . . ? C56 C64 C69 C68 175.4(8) . . . . ? C67 C68 C69 C64 -0.3(16) . . . . ? N11 N12 C70 C40 -0.3(7) . . . 1_454 ? Ag5 N12 C70 C40 176.1(4) . . . 1_454 ? N11 N12 C70 C71 178.6(6) . . . . ? Ag5 N12 C70 C71 -5.0(10) . . . . ? N12 C70 C71 C72 -123.7(7) . . . . ? C40 C70 C71 C72 54.9(10) 1_454 . . . ? N12 C70 C71 C76 56.8(10) . . . . ? C40 C70 C71 C76 -124.6(8) 1_454 . . . ? C76 C71 C72 C73 1.2(11) . . . . ? C70 C71 C72 C73 -178.3(7) . . . . ? C71 C72 C73 C74 -1.6(13) . . . . ? C72 C73 C74 C75 1.5(14) . . . . ? C73 C74 C75 C76 -1.0(15) . . . . ? C72 C71 C76 C75 -0.6(11) . . . . ? C70 C71 C76 C75 178.9(7) . . . . ? C74 C75 C76 C71 0.6(14) . . . . ? N10 N9 C77 C63 -0.4(8) . . . 2_646 ? Ag4 N9 C77 C63 164.3(4) . . . 2_646 ? N10 N9 C77 C78 176.5(6) . . . . ? Ag4 N9 C77 C78 -18.8(9) . . . . ? N9 C77 C78 C79 -60.6(11) . . . . ? C63 C77 C78 C79 115.7(9) 2_646 . . . ? N9 C77 C78 C83 121.7(10) . . . . ? C63 C77 C78 C83 -62.1(12) 2_646 . . . ? C83 C78 C79 C80 0.5(16) . . . . ? C77 C78 C79 C80 -177.3(9) . . . . ? C78 C79 C80 C81 0(2) . . . . ? C79 C80 C81 C82 0(2) . . . . ? C80 C81 C82 C83 1(3) . . . . ? C79 C78 C83 C82 -0.3(19) . . . . ? C77 C78 C83 C82 177.5(12) . . . . ? C81 C82 C83 C78 0(2) . . . . ? N9 N10 C84 C63 0.1(7) . . . 2_646 ? Ag6 N10 C84 C63 173.6(4) . . . 2_646 ? N9 N10 C84 C85 -178.2(6) . . . . ? Ag6 N10 C84 C85 -4.7(10) . . . . ? N10 C84 C85 C90A 70.9(10) . . . . ? C63 C84 C85 C90A -107.0(10) 2_646 . . . ? N10 C84 C85 C86B -44.3(16) . . . . ? C63 C84 C85 C86B 137.8(14) 2_646 . . . ? N10 C84 C85 C86A -112.3(9) . . . . ? C63 C84 C85 C86A 69.8(11) 2_646 . . . ? N10 C84 C85 C90B 128.3(16) . . . . ? C63 C84 C85 C90B -49.6(19) 2_646 . . . ? C90A C85 C86A C87A -2.6(17) . . . . ? C86B C85 C86A C87A 61(2) . . . . ? C90B C85 C86A C87A -47.4(18) . . . . ? C84 C85 C86A C87A -179.2(10) . . . . ? C89B C88 C87A C86A 51(3) . . . . ? C87B C88 C87A C86A -78(3) . . . . ? C89A C88 C87A C86A -2(2) . . . . ? C85 C86A C87A C88 4(2) . . . . ? C89B C88 C89A C90A -85(3) . . . . ? C87B C88 C89A C90A 55(2) . . . . ? C87A C88 C89A C90A -1(2) . . . . ? C86B C85 C90A C89A -48.7(18) . . . . ? C86A C85 C90A C89A -0.6(17) . . . . ? C90B C85 C90A C89A 67(2) . . . . ? C84 C85 C90A C89A 176.0(11) . . . . ? C88 C89A C90A C85 3(2) . . . . ? C90A C85 C86B C87B 51.0(14) . . . . ? C86A C85 C86B C87B -80.6(18) . . . . ? C90B C85 C86B C87B 5.1(18) . . . . ? C84 C85 C86B C87B 178.6(13) . . . . ? C89B C88 C87B C86B -13(4) . . . . ? C87A C88 C87B C86B 66.2(17) . . . . ? C89A C88 C87B C86B -54.2(18) . . . . ? C85 C86B C87B C88 5(2) . . . . ? C87B C88 C89B C90B 8(6) . . . . ? C87A C88 C89B C90B -52(4) . . . . ? C89A C88 C89B C90B 64(3) . . . . ? C88 C89B C90B C85 6(5) . . . . ? C90A C85 C90B C89B -82(3) . . . . ? C86B C85 C90B C89B -10(3) . . . . ? C86A C85 C90B C89B 46(3) . . . . ? C84 C85 C90B C89B 176(3) . . . . ? C62B C57 C58A C59A -50(3) . . . . ? C58B C57 C58A C59A 72(5) . . . . ? C62A C57 C58A C59A -4.4(15) . . . . ? C54 C57 C58A C59A 178.4(9) . . . . ? C61A C60 C59A C58A -1(2) . . . . ? C61B C60 C59A C58A 40(3) . . . . ? C59B C60 C59A C58A -70(4) . . . . ? C57 C58A C59A C60 3.1(17) . . . . ? C59A C60 C61A C62A 0(2) . . . . ? C61B C60 C61A C62A -70(3) . . . . ? C59B C60 C61A C62A 52(3) . . . . ? C60 C61A C62A C57 -2(2) . . . . ? C62B C57 C62A C61A 78(3) . . . . ? C58B C57 C62A C61A -51(3) . . . . ? C58A C57 C62A C61A 3.7(17) . . . . ? C54 C57 C62A C61A -179.1(12) . . . . ? C62B C57 C58B C59B 3(3) . . . . ? C62A C57 C58B C59B 45.1(16) . . . . ? C58A C57 C58B C59B -74(3) . . . . ? C54 C57 C58B C59B 177.6(13) . . . . ? C57 C58B C59B C60 7(2) . . . . ? C61A C60 C59B C58B -56(2) . . . . ? C59A C60 C59B C58B 70(3) . . . . ? C61B C60 C59B C58B -17(4) . . . . ? C61A C60 C61B C62B 85(5) . . . . ? C59A C60 C61B C62B -40(4) . . . . ? C59B C60 C61B C62B 19(5) . . . . ? C58B C57 C62B C61B -1(5) . . . . ? C62A C57 C62B C61B -66(4) . . . . ? C58A C57 C62B C61B 54(4) . . . . ? C54 C57 C62B C61B -175(3) . . . . ? C60 C61B C62B C57 -11(6) . . . . ? data_phbpz_new _database_code_depnum_ccdc_archive 'CCDC 903116' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 N4, C2 H6 O S' _chemical_formula_sum 'C32 H28 N4 O S' _chemical_formula_weight 516.64 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3718(12) _cell_length_b 16.0120(16) _cell_length_c 16.776(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.124(5) _cell_angle_gamma 90.00 _cell_volume 2778.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9887 _cell_measurement_theta_min 4.775 _cell_measurement_theta_max 56.68 _exptl_crystal_description needle-shaped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7110 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; The disordered DMSO has three different orientations with a sod of 70%, 20%, 10%. ; _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 D8 Venture' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4167 _diffrn_reflns_number 49286 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_unetI/netI 0.0244 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4863 _reflns_number_gt 4231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Instrument Service v3.0.25' _computing_cell_refinement 'APEX2 v2012.12-0 (Bruker AXS)' _computing_data_reduction 'SAINT V8.27B (Bruker AXS Inc., 2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diamond _computing_publication_material Word _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^)+(0.0481P)^2^+1.8366P] 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 4863 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1097 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 N1 N 0.86032(14) 0.03218(8) 0.11437(8) 0.0183(3) Uani 1 1 d . . . N2 N 0.82090(14) 0.00810(8) 0.18573(8) 0.0188(3) Uani 1 1 d . . . H2A H 0.8338 -0.0423 0.2057 0.023 Uiso 1 1 calc R . . N3 N 0.53677(14) 0.31141(9) 0.20129(9) 0.0203(3) Uani 1 1 d . . . H3A H 0.4622 0.3378 0.1964 0.024 Uiso 1 1 calc R . . N4 N 0.64331(14) 0.34228(9) 0.24188(9) 0.0199(3) Uani 1 1 d . . . C1 C 0.91642(16) 0.11774(10) -0.02649(10) 0.0185(4) Uani 1 1 d . . . H1 H 0.9299 0.0591 -0.0231 0.022 Uiso 1 1 calc R . . C2 C 0.95822(17) 0.16103(11) -0.09104(11) 0.0226(4) Uani 1 1 d . . . H2 H 1.0000 0.1320 -0.1313 0.027 Uiso 1 1 calc R . . C3 C 0.93964(19) 0.24666(12) -0.09750(11) 0.0270(4) Uani 1 1 d . . . H3 H 0.9699 0.2767 -0.1413 0.032 Uiso 1 1 calc R . . C4 C 0.8762(2) 0.28759(12) -0.03900(11) 0.0283(4) Uani 1 1 d . . . H4 H 0.8615 0.3460 -0.0433 0.034 Uiso 1 1 calc R . . C5 C 0.83361(18) 0.24434(11) 0.02594(11) 0.0236(4) Uani 1 1 d . . . H5 H 0.7897 0.2735 0.0653 0.028 Uiso 1 1 calc R . . C6 C 0.85469(16) 0.15844(10) 0.03401(10) 0.0174(4) Uani 1 1 d . . . C7 C 0.82089(16) 0.11162(10) 0.10549(10) 0.0159(4) Uani 1 1 d . . . C8 C 0.75563(16) 0.13775(10) 0.17301(10) 0.0164(4) Uani 1 1 d . . . C9 C 0.75948(16) 0.06951(10) 0.22329(10) 0.0179(4) Uani 1 1 d . . . C10 C 0.71301(18) 0.05667(10) 0.30321(11) 0.0226(4) Uani 1 1 d . . . C11 C 0.6358(2) -0.01226(12) 0.31805(13) 0.0354(5) Uani 1 1 d . . . H11 H 0.6071 -0.0483 0.2754 0.042 Uiso 1 1 calc R . . C12 C 0.6007(3) -0.02827(13) 0.39479(13) 0.0439(6) Uani 1 1 d . . . H12 H 0.5487 -0.0755 0.4047 0.053 Uiso 1 1 calc R . . C13 C 0.6413(2) 0.02439(13) 0.45687(13) 0.0395(5) Uani 1 1 d . . . H13 H 0.6196 0.0125 0.5097 0.047 Uiso 1 1 calc R . . C14 C 0.7133(2) 0.09423(13) 0.44196(12) 0.0375(5) Uani 1 1 d . . . H14 H 0.7386 0.1314 0.4844 0.045 Uiso 1 1 calc R . . C15 C 0.7491(2) 0.11054(12) 0.36540(11) 0.0285(4) Uani 1 1 d . . . H15 H 0.7986 0.1589 0.3556 0.034 Uiso 1 1 calc R . . C16 C 0.46490(18) 0.10560(11) 0.10338(11) 0.0237(4) Uani 1 1 d . . . H16 H 0.5423 0.0766 0.1196 0.028 Uiso 1 1 calc R . . C17 C 0.36595(18) 0.06419(11) 0.06007(11) 0.0256(4) Uani 1 1 d . . . H17 H 0.3765 0.0071 0.0464 0.031 Uiso 1 1 calc R . . C18 C 0.25199(18) 0.10476(11) 0.03645(11) 0.0246(4) Uani 1 1 d . . . H18 H 0.1847 0.0760 0.0065 0.030 Uiso 1 1 calc R . . C19 C 0.23693(18) 0.18784(11) 0.05694(11) 0.0265(4) Uani 1 1 d . . . H19 H 0.1584 0.2160 0.0416 0.032 Uiso 1 1 calc R . . C20 C 0.33600(18) 0.23006(11) 0.09977(11) 0.0240(4) Uani 1 1 d . . . H20 H 0.3248 0.2871 0.1132 0.029 Uiso 1 1 calc R . . C21 C 0.45200(17) 0.18987(10) 0.12349(10) 0.0187(4) Uani 1 1 d . . . C22 C 0.55690(17) 0.23536(10) 0.16891(10) 0.0176(4) Uani 1 1 d . . . C23 C 0.68591(16) 0.21596(10) 0.18900(10) 0.0159(4) Uani 1 1 d . . . C24 C 0.73466(17) 0.28437(10) 0.23462(10) 0.0172(4) Uani 1 1 d . . . C25 C 0.86533(17) 0.29626(10) 0.27366(10) 0.0186(4) Uani 1 1 d . . . C27 C 0.97578(18) 0.27764(11) 0.23422(11) 0.0228(4) Uani 1 1 d . . . H27 H 0.9674 0.2548 0.1818 0.027 Uiso 1 1 calc R . . C28 C 1.09784(19) 0.29232(13) 0.27105(13) 0.0320(5) Uani 1 1 d . . . H28 H 1.1726 0.2805 0.2435 0.038 Uiso 1 1 calc R . . C29 C 1.1105(2) 0.32426(13) 0.34794(13) 0.0353(5) Uani 1 1 d . . . H29 H 1.1940 0.3342 0.3732 0.042 Uiso 1 1 calc R . . C30 C 1.0016(2) 0.34168(12) 0.38810(12) 0.0313(5) Uani 1 1 d . . . H30 H 1.0106 0.3629 0.4411 0.038 Uiso 1 1 calc R . . C31 C 0.87945(19) 0.32826(11) 0.35123(11) 0.0238(4) Uani 1 1 d . . . H31 H 0.8050 0.3409 0.3788 0.029 Uiso 1 1 calc R . . S1A S 1.28487(6) 0.50996(4) 0.16916(4) 0.02201(16) Uani 0.70 1 d P A 1 O1A O 1.3231(2) 0.42030(12) 0.16747(12) 0.0259(5) Uani 0.70 1 d P A 1 C33A C 1.4125(3) 0.5666(2) 0.1302(3) 0.0528(10) Uani 0.70 1 d P A 1 H33A H 1.4942 0.5520 0.1599 0.079 Uiso 0.70 1 calc PR A 1 H33B H 1.3965 0.6266 0.1355 0.079 Uiso 0.70 1 calc PR A 1 H33C H 1.4175 0.5526 0.0737 0.079 Uiso 0.70 1 calc PR A 1 C32A C 1.3102(5) 0.5424(3) 0.2701(2) 0.0544(12) Uani 0.70 1 d P A 1 H32A H 1.2538 0.5104 0.3032 0.082 Uiso 0.70 1 calc PR A 1 H32B H 1.2901 0.6020 0.2741 0.082 Uiso 0.70 1 calc PR A 1 H32C H 1.4007 0.5329 0.2888 0.082 Uiso 0.70 1 calc PR A 1 S1B S 1.2969(4) 0.4816(2) 0.2641(2) 0.0605(11) Uani 0.20 1 d P B 2 O1B O 1.3522(8) 0.4223(5) 0.2041(5) 0.0259(5) Uani 0.20 1 d P B 2 C33B C 1.1465(12) 0.5052(9) 0.2190(8) 0.059(4) Uani 0.20 1 d P B 2 H33D H 1.1555 0.5223 0.1635 0.089 Uiso 0.20 1 calc PR B 2 H33E H 1.1079 0.5509 0.2480 0.089 Uiso 0.20 1 calc PR B 2 H33F H 1.0908 0.4558 0.2197 0.089 Uiso 0.20 1 calc PR B 2 C32B C 1.3586(19) 0.5813(12) 0.2582(14) 0.075(7) Uani 0.20 1 d P B 2 H32D H 1.4346 0.5870 0.2960 0.113 Uiso 0.20 1 calc PR B 2 H32E H 1.2927 0.6219 0.2714 0.113 Uiso 0.20 1 calc PR B 2 H32F H 1.3834 0.5916 0.2038 0.113 Uiso 0.20 1 calc PR B 2 S1C S 1.4459(6) 0.5661(4) 0.0627(4) 0.0448(14) Uani 0.10 1 d P . 3 O1C O 1.3080(12) 0.5584(7) 0.0741(8) 0.0259(5) Uani 0.10 1 d P C 3 C32C C 1.509(2) 0.4630(16) 0.0501(14) 0.040(5) Uani 0.10 1 d P . 3 C33C C 1.445(3) 0.593(2) -0.0424(18) 0.070(10) Uani 0.10 1 d P . 3 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 N1 0.0205(8) 0.0162(7) 0.0183(8) 0.0003(6) 0.0029(6) 0.0005(6) N2 0.0251(8) 0.0130(7) 0.0189(8) 0.0017(6) 0.0045(6) 0.0017(6) N4 0.0201(8) 0.0176(7) 0.0224(8) -0.0052(6) 0.0037(6) -0.0028(6) N3 0.0175(8) 0.0167(7) 0.0268(8) -0.0054(6) 0.0032(6) 0.0003(6) C6 0.0157(8) 0.0194(9) 0.0166(9) -0.0010(7) -0.0023(7) -0.0008(7) C24 0.0222(9) 0.0151(8) 0.0147(8) 0.0001(6) 0.0045(7) -0.0007(7) C22 0.0215(9) 0.0136(8) 0.0180(9) -0.0015(6) 0.0042(7) -0.0007(7) C7 0.0164(8) 0.0144(8) 0.0166(9) -0.0018(6) -0.0011(7) -0.0009(6) C1 0.0164(9) 0.0186(9) 0.0200(9) -0.0012(7) -0.0012(7) 0.0013(7) C25 0.0239(9) 0.0125(8) 0.0193(9) 0.0011(7) 0.0003(7) -0.0030(7) C21 0.0208(9) 0.0172(9) 0.0184(9) -0.0006(7) 0.0031(7) -0.0022(7) C23 0.0196(9) 0.0141(8) 0.0143(8) 0.0001(6) 0.0024(7) -0.0010(6) C8 0.0166(9) 0.0146(8) 0.0175(9) -0.0016(6) -0.0009(7) -0.0017(6) C9 0.0189(9) 0.0151(8) 0.0199(9) -0.0032(7) 0.0028(7) 0.0002(7) C20 0.0257(10) 0.0171(9) 0.0288(10) -0.0016(7) -0.0001(8) 0.0011(7) C16 0.0222(10) 0.0183(9) 0.0303(10) -0.0023(7) -0.0006(8) 0.0015(7) C10 0.0298(10) 0.0153(8) 0.0236(10) 0.0021(7) 0.0082(8) 0.0054(7) C27 0.0257(10) 0.0207(9) 0.0219(9) -0.0022(7) 0.0007(8) -0.0023(7) C31 0.0303(10) 0.0202(9) 0.0207(9) -0.0017(7) 0.0001(8) -0.0026(7) C18 0.0235(10) 0.0251(10) 0.0246(10) -0.0004(7) -0.0021(8) -0.0065(7) C5 0.0327(11) 0.0197(9) 0.0188(9) -0.0002(7) 0.0052(8) 0.0035(7) C2 0.0215(9) 0.0291(10) 0.0176(9) -0.0011(7) 0.0028(7) 0.0026(7) C17 0.0271(10) 0.0175(9) 0.0318(11) -0.0053(8) -0.0001(8) -0.0021(7) C3 0.0338(11) 0.0281(10) 0.0195(9) 0.0054(8) 0.0036(8) -0.0036(8) C15 0.0405(12) 0.0216(9) 0.0236(10) 0.0011(7) 0.0043(8) -0.0023(8) C19 0.0226(10) 0.0252(10) 0.0310(11) 0.0023(8) -0.0034(8) 0.0010(8) C4 0.0426(12) 0.0186(9) 0.0237(10) 0.0033(7) 0.0032(9) 0.0016(8) C30 0.0400(12) 0.0297(11) 0.0230(10) -0.0033(8) -0.0062(9) -0.0044(9) C29 0.0291(11) 0.0374(12) 0.0372(12) -0.0017(9) -0.0115(9) -0.0058(9) C28 0.0226(10) 0.0357(11) 0.0373(12) -0.0017(9) 0.0006(9) -0.0017(8) C14 0.0594(15) 0.0300(11) 0.0238(11) -0.0052(8) 0.0074(10) -0.0006(10) C11 0.0553(14) 0.0213(10) 0.0318(11) -0.0066(8) 0.0187(10) -0.0061(9) C13 0.0651(16) 0.0294(11) 0.0265(11) 0.0038(9) 0.0203(11) 0.0051(10) C12 0.0713(17) 0.0252(11) 0.0389(13) -0.0027(9) 0.0288(12) -0.0100(10) S1A 0.0209(3) 0.0174(3) 0.0274(4) -0.0024(2) -0.0002(3) 0.0062(2) O1A 0.0260(11) 0.0189(8) 0.0322(13) -0.0030(10) -0.0025(10) 0.0099(7) C33A 0.045(2) 0.0373(19) 0.078(3) 0.0125(18) 0.0184(19) -0.0079(15) C32A 0.074(4) 0.053(4) 0.036(2) -0.018(2) 0.000(2) 0.022(2) S1B 0.065(2) 0.0307(17) 0.079(3) -0.0276(16) -0.0425(19) 0.0351(15) O1B 0.0260(11) 0.0189(8) 0.0322(13) -0.0030(10) -0.0025(10) 0.0099(7) C33B 0.041(7) 0.077(9) 0.062(8) 0.016(7) 0.019(6) 0.043(7) C32B 0.059(12) 0.047(11) 0.112(16) -0.022(10) -0.046(11) 0.008(8) S1C 0.041(3) 0.046(3) 0.047(4) 0.011(3) 0.000(3) 0.001(3) O1C 0.0260(11) 0.0189(8) 0.0322(13) -0.0030(10) -0.0025(10) 0.0099(7) C32C 0.038(13) 0.042(14) 0.041(13) 0.016(10) 0.010(10) 0.012(11) C33C 0.061(18) 0.08(2) 0.07(2) 0.061(17) 0.039(16) 0.025(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 N1 C7 1.341(2) . ? N1 N2 1.349(2) . ? N2 C9 1.352(2) . ? N2 H2A 0.8800 . ? N4 C24 1.338(2) . ? N4 N3 1.349(2) . ? N3 C22 1.356(2) . ? N3 H3A 0.8800 . ? C6 C5 1.398(2) . ? C6 C1 1.399(2) . ? C6 C7 1.478(2) . ? C24 C23 1.409(2) . ? C24 C25 1.475(2) . ? C22 C23 1.391(2) . ? C22 C21 1.475(2) . ? C7 C8 1.424(2) . ? C1 C2 1.382(2) . ? C1 H1 0.9500 . ? C25 C27 1.396(3) . ? C25 C31 1.396(2) . ? C21 C20 1.397(3) . ? C21 C16 1.400(2) . ? C23 C8 1.480(2) . ? C8 C9 1.379(2) . ? C9 C10 1.471(2) . ? C20 C19 1.387(3) . ? C20 H20 0.9500 . ? C16 C17 1.383(3) . ? C16 H16 0.9500 . ? C10 C15 1.384(3) . ? C10 C11 1.397(3) . ? C27 C28 1.388(3) . ? C27 H27 0.9500 . ? C31 C30 1.386(3) . ? C31 H31 0.9500 . ? C18 C17 1.382(3) . ? C18 C19 1.386(3) . ? C18 H18 0.9500 . ? C5 C4 1.389(3) . ? C5 H5 0.9500 . ? C2 C3 1.388(3) . ? C2 H2 0.9500 . ? C17 H17 0.9500 . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C15 C14 1.387(3) . ? C15 H15 0.9500 . ? C19 H19 0.9500 . ? C4 H4 0.9500 . ? C30 C29 1.385(3) . ? C30 H30 0.9500 . ? C29 C28 1.385(3) . ? C29 H29 0.9500 . ? C28 H28 0.9500 . ? C14 C13 1.378(3) . ? C14 H14 0.9500 . ? C11 C12 1.387(3) . ? C11 H11 0.9500 . ? C13 C12 1.382(3) . ? C13 H13 0.9500 . ? C12 H12 0.9500 . ? S1A O1A 1.490(2) . ? S1A C33A 1.768(3) . ? S1A C32A 1.773(4) . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? S1B O1B 1.526(9) . ? S1B C32B 1.725(19) . ? S1B C33B 1.726(12) . ? C33B H33D 0.9800 . ? C33B H33E 0.9800 . ? C33B H33F 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? S1C O1C 1.461(15) . ? S1C C32C 1.79(3) . ? S1C C33C 1.82(3) . ? S1C C32C 2.04(2) 3_865 ? C32C C33C 1.03(4) 3_865 ? C32C S1C 2.04(2) 3_865 ? C33C C32C 1.03(4) 3_865 ? 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 C7 N1 N2 105.08(13) . . ? N1 N2 C9 112.88(13) . . ? N1 N2 H2A 123.6 . . ? C9 N2 H2A 123.6 . . ? C24 N4 N3 105.06(13) . . ? N4 N3 C22 112.78(14) . . ? N4 N3 H3A 123.6 . . ? C22 N3 H3A 123.6 . . ? C5 C6 C1 117.67(16) . . ? C5 C6 C7 122.23(15) . . ? C1 C6 C7 120.00(15) . . ? N4 C24 C23 111.07(15) . . ? N4 C24 C25 120.30(15) . . ? C23 C24 C25 128.61(15) . . ? N3 C22 C23 106.06(14) . . ? N3 C22 C21 121.43(15) . . ? C23 C22 C21 132.51(15) . . ? N1 C7 C8 110.43(14) . . ? N1 C7 C6 118.89(15) . . ? C8 C7 C6 130.60(15) . . ? C2 C1 C6 121.38(16) . . ? C2 C1 H1 119.3 . . ? C6 C1 H1 119.3 . . ? C27 C25 C31 119.05(16) . . ? C27 C25 C24 121.42(16) . . ? C31 C25 C24 119.52(16) . . ? C20 C21 C16 118.08(16) . . ? C20 C21 C22 120.52(15) . . ? C16 C21 C22 121.39(16) . . ? C22 C23 C24 105.03(14) . . ? C22 C23 C8 128.24(15) . . ? C24 C23 C8 126.53(15) . . ? C9 C8 C7 105.03(14) . . ? C9 C8 C23 123.54(15) . . ? C7 C8 C23 131.24(15) . . ? N2 C9 C8 106.56(15) . . ? N2 C9 C10 121.29(15) . . ? C8 C9 C10 132.14(15) . . ? C19 C20 C21 120.92(17) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C17 C16 C21 120.57(17) . . ? C17 C16 H16 119.7 . . ? C21 C16 H16 119.7 . . ? C15 C10 C11 119.06(17) . . ? C15 C10 C9 120.73(16) . . ? C11 C10 C9 120.16(16) . . ? C28 C27 C25 120.40(17) . . ? C28 C27 H27 119.8 . . ? C25 C27 H27 119.8 . . ? C30 C31 C25 120.27(18) . . ? C30 C31 H31 119.9 . . ? C25 C31 H31 119.9 . . ? C17 C18 C19 119.32(17) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C4 C5 C6 120.68(17) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C2 C3 120.48(17) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C18 C17 C16 120.82(17) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C4 C3 C2 118.85(17) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C10 C15 C14 120.30(18) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C18 C19 C20 120.27(17) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C3 C4 C5 120.91(17) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C29 C30 C31 120.21(18) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C29 C28 120.10(19) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C28 C27 119.95(19) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C13 C14 C15 120.37(19) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C12 C11 C10 120.24(19) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C14 C13 C12 119.89(19) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? O1A S1A C33A 106.27(15) . . ? O1A S1A C32A 106.22(18) . . ? C33A S1A C32A 98.0(2) . . ? O1B S1B C32B 112.3(9) . . ? O1B S1B C33B 102.6(6) . . ? C32B S1B C33B 95.7(8) . . ? S1B C33B H33D 109.5 . . ? S1B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? S1B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? S1B C32B H32D 109.5 . . ? S1B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? S1B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? O1C S1C C32C 107.7(9) . . ? O1C S1C C33C 102.0(11) . . ? C32C S1C C33C 94.6(14) . . ? O1C S1C C32C 113.3(9) . 3_865 ? C32C S1C C32C 64.5(12) . 3_865 ? C33C S1C C32C 30.4(11) . 3_865 ? C33C C32C S1C 173(3) 3_865 . ? C33C C32C S1C 63(2) 3_865 3_865 ? S1C C32C S1C 115.5(12) . 3_865 ? C32C C33C S1C 87(2) 3_865 . ? 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 C7 N1 N2 C9 -0.92(19) . . . . ? C24 N4 N3 C22 0.50(19) . . . . ? N3 N4 C24 C23 0.00(19) . . . . ? N3 N4 C24 C25 -178.58(14) . . . . ? N4 N3 C22 C23 -0.79(19) . . . . ? N4 N3 C22 C21 178.74(15) . . . . ? N2 N1 C7 C8 0.15(18) . . . . ? N2 N1 C7 C6 177.13(14) . . . . ? C5 C6 C7 N1 -170.62(16) . . . . ? C1 C6 C7 N1 5.8(2) . . . . ? C5 C6 C7 C8 5.7(3) . . . . ? C1 C6 C7 C8 -177.96(17) . . . . ? C5 C6 C1 C2 1.6(3) . . . . ? C7 C6 C1 C2 -174.93(16) . . . . ? N4 C24 C25 C27 -137.04(17) . . . . ? C23 C24 C25 C27 44.7(3) . . . . ? N4 C24 C25 C31 41.8(2) . . . . ? C23 C24 C25 C31 -136.52(18) . . . . ? N3 C22 C21 C20 12.1(3) . . . . ? C23 C22 C21 C20 -168.55(18) . . . . ? N3 C22 C21 C16 -167.49(16) . . . . ? C23 C22 C21 C16 11.9(3) . . . . ? N3 C22 C23 C24 0.72(18) . . . . ? C21 C22 C23 C24 -178.72(17) . . . . ? N3 C22 C23 C8 175.65(16) . . . . ? C21 C22 C23 C8 -3.8(3) . . . . ? N4 C24 C23 C22 -0.46(19) . . . . ? C25 C24 C23 C22 177.97(16) . . . . ? N4 C24 C23 C8 -175.51(15) . . . . ? C25 C24 C23 C8 2.9(3) . . . . ? N1 C7 C8 C9 0.62(19) . . . . ? C6 C7 C8 C9 -175.90(17) . . . . ? N1 C7 C8 C23 -174.37(16) . . . . ? C6 C7 C8 C23 9.1(3) . . . . ? C22 C23 C8 C9 -87.2(2) . . . . ? C24 C23 C8 C9 86.7(2) . . . . ? C22 C23 C8 C7 87.0(2) . . . . ? C24 C23 C8 C7 -99.1(2) . . . . ? N1 N2 C9 C8 1.32(19) . . . . ? N1 N2 C9 C10 -177.83(15) . . . . ? C7 C8 C9 N2 -1.12(18) . . . . ? C23 C8 C9 N2 174.36(15) . . . . ? C7 C8 C9 C10 177.90(18) . . . . ? C23 C8 C9 C10 -6.6(3) . . . . ? C16 C21 C20 C19 -0.5(3) . . . . ? C22 C21 C20 C19 179.89(17) . . . . ? C20 C21 C16 C17 1.1(3) . . . . ? C22 C21 C16 C17 -179.36(17) . . . . ? N2 C9 C10 C15 125.64(19) . . . . ? C8 C9 C10 C15 -53.3(3) . . . . ? N2 C9 C10 C11 -51.8(3) . . . . ? C8 C9 C10 C11 129.3(2) . . . . ? C31 C25 C27 C28 -1.3(3) . . . . ? C24 C25 C27 C28 177.55(16) . . . . ? C27 C25 C31 C30 0.4(3) . . . . ? C24 C25 C31 C30 -178.48(16) . . . . ? C1 C6 C5 C4 -1.8(3) . . . . ? C7 C6 C5 C4 174.68(17) . . . . ? C6 C1 C2 C3 -0.1(3) . . . . ? C19 C18 C17 C16 -0.4(3) . . . . ? C21 C16 C17 C18 -0.6(3) . . . . ? C1 C2 C3 C4 -1.3(3) . . . . ? C11 C10 C15 C14 2.6(3) . . . . ? C9 C10 C15 C14 -174.85(18) . . . . ? C17 C18 C19 C20 0.9(3) . . . . ? C21 C20 C19 C18 -0.4(3) . . . . ? C2 C3 C4 C5 1.1(3) . . . . ? C6 C5 C4 C3 0.4(3) . . . . ? C25 C31 C30 C29 0.7(3) . . . . ? C31 C30 C29 C28 -0.8(3) . . . . ? C30 C29 C28 C27 -0.1(3) . . . . ? C25 C27 C28 C29 1.1(3) . . . . ? C10 C15 C14 C13 -0.1(3) . . . . ? C15 C10 C11 C12 -2.8(3) . . . . ? C9 C10 C11 C12 174.7(2) . . . . ? C15 C14 C13 C12 -2.2(4) . . . . ? C14 C13 C12 C11 2.0(4) . . . . ? C10 C11 C12 C13 0.5(4) . . . . ? O1C S1C C32C C33C -178(100) . . . 3_865 ? C33C S1C C32C C33C 77(24) . . . 3_865 ? C32C S1C C32C C33C 74(23) 3_865 . . 3_865 ? O1C S1C C32C S1C 107.9(12) . . . 3_865 ? C33C S1C C32C S1C 3.7(16) . . . 3_865 ? C32C S1C C32C S1C 0.000(1) 3_865 . . 3_865 ? O1C S1C C33C C32C -116(2) . . . 3_865 ? C32C S1C C33C C32C -7(3) . . . 3_865 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O1B 0.88 1.78 2.614(8) 157.2 1_455 N3 H3A O1A 0.88 1.99 2.845(2) 163.4 1_455 N2 H2A N4 0.88 2.05 2.932(2) 176.4 2_645 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.570 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.046