# SUBMISSION DETAILS data_global _publ_contact_author_name 'Dr. Oliver Schuster' _publ_contact_author_address ; University of Fribourg Department of Chemistry Chemin du Mus\'ee 9 CH-1700 FRIBOURG ; _publ_contact_author_phone '++41 26 300 8782' _publ_contact_author_fax '++41 26 300 9739' _publ_contact_author_email 'oliver.schuster@unifr.ch' _publ_requested_journal ; Organometallics ; _publ_requested_coeditor_name ? _publ_contact_letter ? #============================================================================ # TITLE AND AUTHOR LIST _publ_section_title ; Pyridine-derived N-heterocyclic carbenes: An experimental and theoretical evaluation of the bonding in and reactivity of selected normal and abnormal complexes of Ni(II) and Pd(II) ; loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Stander-Grobler, E.' ; Department of Chemistry and Polymer Science University of Stellenbosch Private Bag XI 7602 Matieland SOUTH AFRICA ; . 'Schuster, O.' ; University of Fribourg Department of Chemistry Chemin du Mus\'ee 9 CH-1700 FRIBOURG ; . 'Heydenrych, G.' ; Fachbereich Chemie Philipps-Universit\"at Marburg Hans-Meerwein-Strasse D-35043 Marburg ; . 'Cronje, S.' ; Department of Chemistry and Polymer Science University of Stellenbosch Private Bag XI 7602 Matieland SOUTH AFRICA ; . 'Tosh, E.' ; Inorganic Chemistry Department Technische Universit\"at M\"unchen Lichtenbergstr. 4 D-85747 Garching. ; . 'Albrecht, M.' ; University of Fribourg Department of Chemistry Chemin du Mus\'ee 9 CH-1700 FRIBOURG ; . 'Frenking, G.' ; Fachbereich Chemie Philipps-Universit\"at Marburg Hans-Meerwein-Strasse D-35043 Marburg ; . 'Raubenheimer, H. G.' ; Department of Chemistry and Polymer Science University of Stellenbosch Private Bag XI 7602 Matieland SOUTH AFRICA ; . #============================================================================== data_3aBF4 _refine_special_details ; The carbene ring was found to be disordered (s.o.f.: 20%). Refinemnt of the less occupied site was supported by restraining its geometry to fit the major site using SAME. During the structure refinement 3 dichloromethane molecules were found, but could not be refined properly due to disorder. The SQUEEZE routine of Platon was used to modify the hkl-file (see end of CIF)! ; _audit_update_record ; 2009-04-05 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H37 Cl N P2 Pd, B F4' _chemical_formula_sum 'C42 H37 B Cl F4 N P2 Pd' _chemical_formula_weight 846.33 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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.897(2) _cell_length_b 13.008(3) _cell_length_c 17.193(3) _cell_angle_alpha 73.05(3) _cell_angle_beta 76.83(3) _cell_angle_gamma 65.23(3) _cell_volume 2293.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16161 _cell_measurement_theta_min 2.381 _cell_measurement_theta_max 28.243 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 0.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8138 _exptl_absorpt_correction_T_max 0.9187 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26167 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.33 _reflns_number_total 10435 _reflns_number_gt 9436 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0275P)^2^+3.4187P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10435 _refine_ls_number_parameters 500 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4094(3) 0.7873(3) 0.30978(17) 0.0188(5) Uani 0.80 1 d PD A 1 C6 C 0.3641(3) 0.9033(4) 0.3169(2) 0.0244(7) Uani 0.80 1 d PD A 1 H2 H 0.3690 0.9615 0.2692 0.029 Uiso 0.80 1 calc PR A 1 C5 C 0.3130(3) 0.9352(3) 0.3906(2) 0.0330(7) Uani 0.80 1 d P A 1 H3 H 0.2830 1.0143 0.3935 0.040 Uiso 0.80 1 calc PR A 1 C4 C 0.3057(3) 0.8504(4) 0.4607(2) 0.0363(8) Uani 0.80 1 d P A 1 H4 H 0.2717 0.8703 0.5124 0.044 Uiso 0.80 1 calc PR A 1 C3 C 0.3482(3) 0.7388(4) 0.4538(3) 0.0325(9) Uani 0.80 1 d P A 1 H5 H 0.3431 0.6803 0.5013 0.039 Uiso 0.80 1 calc PR A 1 N2 N 0.3984(2) 0.7082(2) 0.37979(15) 0.0230(5) Uani 0.80 1 d P A 1 C21 C 0.4441(3) 0.5857(4) 0.3755(2) 0.0277(7) Uani 0.80 1 d P A 1 H6A H 0.5331 0.5590 0.3548 0.042 Uiso 0.80 1 calc PR A 1 H6B H 0.3978 0.5780 0.3385 0.042 Uiso 0.80 1 calc PR A 1 H6C H 0.4319 0.5386 0.4303 0.042 Uiso 0.80 1 calc PR A 1 C01 C 0.4245(11) 0.7354(11) 0.3165(7) 0.015(3) Uiso 0.20 1 d PD A 2 C06 C 0.4351(15) 0.6306(14) 0.3723(9) 0.023(4) Uiso 0.20 1 d PD A 2 H02 H 0.4721 0.5630 0.3504 0.028 Uiso 0.20 1 calc PR A 2 C05 C 0.3994(13) 0.6142(12) 0.4530(8) 0.034(3) Uiso 0.20 1 d P A 2 H03 H 0.4146 0.5391 0.4875 0.040 Uiso 0.20 1 calc PR A 2 C04 C 0.3413(17) 0.7101(16) 0.4816(12) 0.032(4) Uiso 0.20 1 d P A 2 H04 H 0.3093 0.7028 0.5380 0.039 Uiso 0.20 1 calc PR A 2 C03 C 0.3247(15) 0.8203(16) 0.4340(10) 0.030(3) Uiso 0.20 1 d P A 2 H05 H 0.2863 0.8867 0.4573 0.036 Uiso 0.20 1 calc PR A 2 N02 N 0.3665(9) 0.8299(9) 0.3506(6) 0.0201(19) Uiso 0.20 1 d P A 2 C021 C 0.3524(14) 0.9437(12) 0.3001(9) 0.015(3) Uiso 0.20 1 d P A 2 H06A H 0.2760 1.0017 0.3210 0.023 Uiso 0.20 1 calc PR A 2 H06B H 0.3474 0.9455 0.2436 0.023 Uiso 0.20 1 calc PR A 2 H06C H 0.4244 0.9612 0.3015 0.023 Uiso 0.20 1 calc PR A 2 C211 C 0.71058(19) 0.66184(19) 0.33533(13) 0.0177(4) Uani 1 1 d . . . C216 C 0.6517(2) 0.7278(2) 0.39531(14) 0.0237(5) Uani 1 1 d . . . H12 H 0.5978 0.8067 0.3799 0.028 Uiso 1 1 calc R . . C215 C 0.6712(2) 0.6790(2) 0.47721(15) 0.0289(5) Uani 1 1 d . . . H13 H 0.6304 0.7246 0.5172 0.035 Uiso 1 1 calc R . . C214 C 0.7505(2) 0.5638(2) 0.50040(15) 0.0293(5) Uani 1 1 d . . . H14 H 0.7649 0.5309 0.5560 0.035 Uiso 1 1 calc R . . C213 C 0.8085(2) 0.4969(2) 0.44204(16) 0.0290(5) Uani 1 1 d . . . H15 H 0.8618 0.4178 0.4580 0.035 Uiso 1 1 calc R . . C212 C 0.7887(2) 0.5458(2) 0.35977(14) 0.0224(5) Uani 1 1 d . . . H16 H 0.8288 0.4996 0.3202 0.027 Uiso 1 1 calc R . . C221 C 0.81204(19) 0.62948(19) 0.17417(13) 0.0175(4) Uani 1 1 d . . . C222 C 0.8042(2) 0.5341(2) 0.15727(14) 0.0220(4) Uani 1 1 d . . . H22 H 0.7266 0.5248 0.1683 0.026 Uiso 1 1 calc R . . C223 C 0.9104(2) 0.4522(2) 0.12416(15) 0.0278(5) Uani 1 1 d . . . H23 H 0.9048 0.3872 0.1131 0.033 Uiso 1 1 calc R . . C224 C 1.0236(2) 0.4654(2) 0.10738(15) 0.0277(5) Uani 1 1 d . . . H24 H 1.0953 0.4099 0.0843 0.033 Uiso 1 1 calc R . . C225 C 1.0326(2) 0.5600(2) 0.12437(15) 0.0268(5) Uani 1 1 d . . . H25 H 1.1106 0.5685 0.1134 0.032 Uiso 1 1 calc R . . C226 C 0.9270(2) 0.6420(2) 0.15742(14) 0.0212(4) Uani 1 1 d . . . H26 H 0.9331 0.7067 0.1686 0.025 Uiso 1 1 calc R . . C231 C 0.69091(19) 0.86612(18) 0.20466(13) 0.0173(4) Uani 1 1 d . . . C232 C 0.6236(2) 0.9544(2) 0.14381(13) 0.0205(4) Uani 1 1 d . . . H32 H 0.5766 0.9384 0.1142 0.025 Uiso 1 1 calc R . . C233 C 0.6249(2) 1.0657(2) 0.12635(14) 0.0240(5) Uani 1 1 d . . . H33 H 0.5805 1.1249 0.0843 0.029 Uiso 1 1 calc R . . C234 C 0.6918(2) 1.0892(2) 0.17098(15) 0.0250(5) Uani 1 1 d . . . H34 H 0.6902 1.1656 0.1609 0.030 Uiso 1 1 calc R . . C235 C 0.7614(2) 1.0013(2) 0.23055(15) 0.0261(5) Uani 1 1 d . . . H35 H 0.8084 1.0176 0.2599 0.031 Uiso 1 1 calc R . . C236 C 0.7620(2) 0.8900(2) 0.24698(14) 0.0224(4) Uani 1 1 d . . . H36 H 0.8105 0.8301 0.2868 0.027 Uiso 1 1 calc R . . C121 C 0.31044(19) 0.67326(19) 0.10915(13) 0.0186(4) Uani 1 1 d . . . C126 C 0.2654(2) 0.7142(2) 0.03300(14) 0.0218(4) Uani 1 1 d . . . H42 H 0.2232 0.7952 0.0134 0.026 Uiso 1 1 calc R . . C125 C 0.2822(2) 0.6370(2) -0.01417(15) 0.0266(5) Uani 1 1 d . . . H43 H 0.2523 0.6654 -0.0661 0.032 Uiso 1 1 calc R . . C124 C 0.3425(2) 0.5185(2) 0.01474(16) 0.0281(5) Uani 1 1 d . . . H44 H 0.3513 0.4656 -0.0165 0.034 Uiso 1 1 calc R . . C123 C 0.3905(2) 0.4769(2) 0.09000(17) 0.0287(5) Uani 1 1 d . . . H45 H 0.4333 0.3959 0.1091 0.034 Uiso 1 1 calc R . . C122 C 0.3757(2) 0.5533(2) 0.13683(15) 0.0237(5) Uani 1 1 d . . . H46 H 0.4095 0.5248 0.1874 0.028 Uiso 1 1 calc R . . C131 C 0.2068(2) 0.91852(18) 0.11769(13) 0.0177(4) Uani 1 1 d . . . C132 C 0.2678(2) 0.9953(2) 0.08087(14) 0.0214(4) Uani 1 1 d . . . H52 H 0.3544 0.9706 0.0836 0.026 Uiso 1 1 calc R . . C133 C 0.2016(2) 1.1087(2) 0.03997(15) 0.0267(5) Uani 1 1 d . . . H53 H 0.2433 1.1608 0.0150 0.032 Uiso 1 1 calc R . . C134 C 0.0751(2) 1.1447(2) 0.03614(14) 0.0281(5) Uani 1 1 d . . . H54 H 0.0301 1.2217 0.0087 0.034 Uiso 1 1 calc R . . C135 C 0.0145(2) 1.0692(2) 0.07209(15) 0.0286(5) Uani 1 1 d . . . H55 H -0.0720 1.0945 0.0687 0.034 Uiso 1 1 calc R . . C136 C 0.0787(2) 0.9560(2) 0.11334(14) 0.0237(5) Uani 1 1 d . . . H56 H 0.0361 0.9048 0.1383 0.028 Uiso 1 1 calc R . . C111 C 0.1766(2) 0.7472(2) 0.25916(13) 0.0200(4) Uani 1 1 d . . . C112 C 0.1191(2) 0.8294(2) 0.30851(14) 0.0250(5) Uani 1 1 d . . . H62 H 0.1396 0.8961 0.2957 0.030 Uiso 1 1 calc R . . C113 C 0.0326(2) 0.8138(3) 0.37588(15) 0.0314(6) Uani 1 1 d . . . H63 H -0.0041 0.8690 0.4094 0.038 Uiso 1 1 calc R . . C114 C -0.0002(2) 0.7186(3) 0.39424(15) 0.0322(6) Uani 1 1 d . . . H64 H -0.0597 0.7085 0.4400 0.039 Uiso 1 1 calc R . . C115 C 0.0542(2) 0.6378(2) 0.34550(16) 0.0300(5) Uani 1 1 d . . . H65 H 0.0310 0.5727 0.3579 0.036 Uiso 1 1 calc R . . C116 C 0.1424(2) 0.6510(2) 0.27859(15) 0.0247(5) Uani 1 1 d . . . H66 H 0.1795 0.5946 0.2460 0.030 Uiso 1 1 calc R . . B1 B 0.6174(3) 0.3188(3) 0.3072(2) 0.0344(7) Uani 1 1 d . . . F1 F 0.48834(18) 0.36524(19) 0.32659(14) 0.0574(5) Uani 1 1 d . . . F2 F 0.6660(2) 0.20005(16) 0.33738(12) 0.0562(5) Uani 1 1 d . . . F3 F 0.6472(3) 0.3435(2) 0.22414(12) 0.0711(7) Uani 1 1 d . . . F4 F 0.67007(17) 0.36714(18) 0.34567(14) 0.0583(6) Uani 1 1 d . . . P2 P 0.67844(5) 0.72518(5) 0.22852(3) 0.01512(11) Uani 1 1 d . A . P1 P 0.29154(5) 0.77142(5) 0.17222(3) 0.01589(11) Uani 1 1 d . A . Pd1 Pd 0.484525(14) 0.749513(14) 0.199957(9) 0.01415(5) Uani 1 1 d . . . Cl1 Cl 0.56115(5) 0.74884(5) 0.06053(3) 0.02136(11) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0140(13) 0.0247(18) 0.0188(14) -0.0052(13) -0.0031(10) -0.0077(12) C6 0.0199(16) 0.030(2) 0.0223(17) -0.0030(17) -0.0043(12) -0.0089(15) C5 0.0222(15) 0.0405(19) 0.0381(18) -0.0193(15) 0.0001(13) -0.0084(14) C4 0.0230(16) 0.056(2) 0.0306(19) -0.0195(19) 0.0033(14) -0.0127(16) C3 0.0219(17) 0.051(3) 0.0248(19) 0.0001(19) -0.0023(14) -0.0200(17) N2 0.0179(11) 0.0319(15) 0.0205(12) -0.0027(10) -0.0034(9) -0.0122(11) C21 0.0285(18) 0.026(2) 0.0283(18) -0.0005(15) -0.0054(12) -0.0130(15) C211 0.0144(9) 0.0245(11) 0.0174(10) -0.0027(8) -0.0032(8) -0.0110(8) C216 0.0184(11) 0.0278(12) 0.0240(11) -0.0067(9) -0.0048(9) -0.0062(9) C215 0.0273(12) 0.0411(14) 0.0217(11) -0.0080(10) -0.0033(9) -0.0152(11) C214 0.0298(13) 0.0415(14) 0.0190(11) 0.0026(10) -0.0084(9) -0.0194(11) C213 0.0299(13) 0.0273(12) 0.0286(13) 0.0032(10) -0.0092(10) -0.0128(10) C212 0.0212(11) 0.0232(11) 0.0238(11) -0.0019(9) -0.0044(9) -0.0106(9) C221 0.0138(9) 0.0195(10) 0.0167(10) -0.0033(8) -0.0019(7) -0.0042(8) C222 0.0183(10) 0.0227(11) 0.0252(11) -0.0060(9) -0.0031(8) -0.0071(9) C223 0.0282(12) 0.0257(12) 0.0301(12) -0.0119(10) -0.0073(10) -0.0052(10) C224 0.0232(12) 0.0293(12) 0.0227(11) -0.0096(10) -0.0002(9) -0.0011(10) C225 0.0165(11) 0.0325(13) 0.0269(12) -0.0043(10) -0.0003(9) -0.0076(10) C226 0.0173(10) 0.0224(11) 0.0225(11) -0.0032(9) -0.0018(8) -0.0075(9) C231 0.0153(10) 0.0171(10) 0.0208(10) -0.0059(8) -0.0005(8) -0.0071(8) C232 0.0191(10) 0.0239(11) 0.0196(10) -0.0046(9) -0.0015(8) -0.0099(9) C233 0.0247(11) 0.0205(11) 0.0229(11) 0.0000(9) -0.0021(9) -0.0083(9) C234 0.0270(12) 0.0209(11) 0.0289(12) -0.0079(9) -0.0002(9) -0.0108(9) C235 0.0279(12) 0.0273(12) 0.0302(12) -0.0099(10) -0.0053(10) -0.0142(10) C236 0.0224(11) 0.0241(11) 0.0230(11) -0.0043(9) -0.0063(9) -0.0100(9) C121 0.0142(10) 0.0213(10) 0.0228(11) -0.0044(8) -0.0013(8) -0.0098(8) C126 0.0183(10) 0.0242(11) 0.0245(11) -0.0035(9) -0.0032(8) -0.0107(9) C125 0.0230(11) 0.0378(14) 0.0260(12) -0.0110(10) 0.0002(9) -0.0171(10) C124 0.0223(11) 0.0333(13) 0.0369(13) -0.0205(11) 0.0100(10) -0.0168(10) C123 0.0196(11) 0.0222(12) 0.0428(15) -0.0101(10) 0.0032(10) -0.0080(9) C122 0.0170(10) 0.0234(11) 0.0289(12) -0.0043(9) -0.0022(9) -0.0074(9) C131 0.0177(10) 0.0186(10) 0.0172(10) -0.0035(8) -0.0043(8) -0.0064(8) C132 0.0188(10) 0.0222(11) 0.0224(11) -0.0058(9) -0.0003(8) -0.0074(9) C133 0.0305(13) 0.0207(11) 0.0237(11) -0.0036(9) 0.0045(9) -0.0096(10) C134 0.0309(13) 0.0240(12) 0.0189(11) -0.0027(9) -0.0016(9) -0.0026(10) C135 0.0208(11) 0.0302(13) 0.0276(12) -0.0024(10) -0.0090(9) -0.0023(10) C136 0.0191(11) 0.0266(12) 0.0246(11) -0.0021(9) -0.0067(9) -0.0082(9) C111 0.0153(10) 0.0257(11) 0.0181(10) 0.0012(8) -0.0053(8) -0.0093(9) C112 0.0190(11) 0.0340(13) 0.0238(11) -0.0059(10) -0.0037(9) -0.0113(10) C113 0.0212(12) 0.0478(16) 0.0243(12) -0.0089(11) -0.0025(9) -0.0118(11) C114 0.0203(11) 0.0505(16) 0.0208(11) 0.0047(11) -0.0038(9) -0.0163(11) C115 0.0225(12) 0.0340(13) 0.0305(13) 0.0077(10) -0.0070(10) -0.0159(10) C116 0.0211(11) 0.0270(12) 0.0258(12) 0.0006(9) -0.0075(9) -0.0110(9) B1 0.0374(17) 0.0341(16) 0.0368(16) -0.0106(13) -0.0039(13) -0.0170(13) F1 0.0409(10) 0.0671(13) 0.0803(15) -0.0318(11) -0.0049(10) -0.0270(10) F2 0.0755(14) 0.0394(10) 0.0526(11) -0.0079(9) -0.0195(10) -0.0163(10) F3 0.114(2) 0.0699(14) 0.0392(11) -0.0091(10) 0.0088(12) -0.0548(15) F4 0.0362(10) 0.0638(13) 0.0931(16) -0.0481(12) -0.0087(10) -0.0156(9) P2 0.0127(2) 0.0173(3) 0.0159(2) -0.0034(2) -0.00257(19) -0.0060(2) P1 0.0133(2) 0.0181(3) 0.0167(2) -0.0019(2) -0.00320(19) -0.0070(2) Pd1 0.01186(8) 0.01682(8) 0.01430(8) -0.00249(6) -0.00246(5) -0.00612(6) Cl1 0.0179(2) 0.0303(3) 0.0176(2) -0.0076(2) -0.00081(18) -0.0099(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.358(4) . ? C1 C6 1.406(5) . ? C1 Pd1 2.002(3) . ? C6 C5 1.376(5) . ? C6 H2 0.9500 . ? C5 C4 1.391(5) . ? C5 H3 0.9500 . ? C4 C3 1.355(6) . ? C4 H4 0.9500 . ? C3 N2 1.372(5) . ? C3 H5 0.9500 . ? N2 C21 1.471(5) . ? C21 H6A 0.9800 . ? C21 H6B 0.9800 . ? C21 H6C 0.9800 . ? C01 N02 1.362(15) . ? C01 C06 1.395(15) . ? C01 Pd1 1.949(12) . ? C06 C05 1.34(2) . ? C06 H02 0.9500 . ? C05 C04 1.32(2) . ? C05 H03 0.9500 . ? C04 C03 1.38(2) . ? C04 H04 0.9500 . ? C03 N02 1.39(2) . ? C03 H05 0.9500 . ? N02 C021 1.443(15) . ? C021 H06A 0.9800 . ? C021 H06B 0.9800 . ? C021 H06C 0.9800 . ? C211 C212 1.397(3) . ? C211 C216 1.405(3) . ? C211 P2 1.836(2) . ? C216 C215 1.394(3) . ? C216 H12 0.9500 . ? C215 C214 1.390(4) . ? C215 H13 0.9500 . ? C214 C213 1.390(4) . ? C214 H14 0.9500 . ? C213 C212 1.401(3) . ? C213 H15 0.9500 . ? C212 H16 0.9500 . ? C221 C222 1.398(3) . ? C221 C226 1.400(3) . ? C221 P2 1.815(2) . ? C222 C223 1.397(3) . ? C222 H22 0.9500 . ? C223 C224 1.383(4) . ? C223 H23 0.9500 . ? C224 C225 1.395(4) . ? C224 H24 0.9500 . ? C225 C226 1.395(3) . ? C225 H25 0.9500 . ? C226 H26 0.9500 . ? C231 C232 1.402(3) . ? C231 C236 1.405(3) . ? C231 P2 1.820(2) . ? C232 C233 1.396(3) . ? C232 H32 0.9500 . ? C233 C234 1.391(3) . ? C233 H33 0.9500 . ? C234 C235 1.397(3) . ? C234 H34 0.9500 . ? C235 C236 1.388(3) . ? C235 H35 0.9500 . ? C236 H36 0.9500 . ? C121 C126 1.399(3) . ? C121 C122 1.409(3) . ? C121 P1 1.820(2) . ? C126 C125 1.393(3) . ? C126 H42 0.9500 . ? C125 C124 1.389(4) . ? C125 H43 0.9500 . ? C124 C123 1.401(4) . ? C124 H44 0.9500 . ? C123 C122 1.387(4) . ? C123 H45 0.9500 . ? C122 H46 0.9500 . ? C131 C132 1.398(3) . ? C131 C136 1.404(3) . ? C131 P1 1.824(2) . ? C132 C133 1.402(3) . ? C132 H52 0.9500 . ? C133 C134 1.388(4) . ? C133 H53 0.9500 . ? C134 C135 1.380(4) . ? C134 H54 0.9500 . ? C135 C136 1.396(3) . ? C135 H55 0.9500 . ? C136 H56 0.9500 . ? C111 C116 1.401(3) . ? C111 C112 1.408(3) . ? C111 P1 1.833(2) . ? C112 C113 1.392(3) . ? C112 H62 0.9500 . ? C113 C114 1.381(4) . ? C113 H63 0.9500 . ? C114 C115 1.387(4) . ? C114 H64 0.9500 . ? C115 C116 1.393(3) . ? C115 H65 0.9500 . ? C116 H66 0.9500 . ? B1 F3 1.366(4) . ? B1 F2 1.383(4) . ? B1 F1 1.393(4) . ? B1 F4 1.409(4) . ? P2 Pd1 2.3403(8) . ? P1 Pd1 2.3347(8) . ? Pd1 Cl1 2.3638(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C6 116.2(3) . . ? N2 C1 Pd1 124.7(3) . . ? C6 C1 Pd1 119.1(3) . . ? C5 C6 C1 122.2(4) . . ? C5 C6 H2 118.9 . . ? C1 C6 H2 118.9 . . ? C6 C5 C4 119.2(4) . . ? C6 C5 H3 120.4 . . ? C4 C5 H3 120.4 . . ? C3 C4 C5 118.6(4) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C4 C3 N2 121.5(4) . . ? C4 C3 H5 119.2 . . ? N2 C3 H5 119.2 . . ? C1 N2 C3 122.2(3) . . ? C1 N2 C21 118.3(3) . . ? C3 N2 C21 119.5(3) . . ? N02 C01 C06 113.7(12) . . ? N02 C01 Pd1 121.9(9) . . ? C06 C01 Pd1 124.3(11) . . ? C05 C06 C01 127.5(16) . . ? C05 C06 H02 116.2 . . ? C01 C06 H02 116.2 . . ? C04 C05 C06 115.4(15) . . ? C04 C05 H03 122.3 . . ? C06 C05 H03 122.3 . . ? C05 C04 C03 123.7(18) . . ? C05 C04 H04 118.1 . . ? C03 C04 H04 118.1 . . ? C04 C03 N02 117.3(16) . . ? C04 C03 H05 121.4 . . ? N02 C03 H05 121.4 . . ? C01 N02 C03 122.2(12) . . ? C01 N02 C021 119.5(11) . . ? C03 N02 C021 118.2(12) . . ? N02 C021 H06A 109.5 . . ? N02 C021 H06B 109.5 . . ? H06A C021 H06B 109.5 . . ? N02 C021 H06C 109.5 . . ? H06A C021 H06C 109.5 . . ? H06B C021 H06C 109.5 . . ? C212 C211 C216 118.4(2) . . ? C212 C211 P2 121.09(17) . . ? C216 C211 P2 120.44(17) . . ? C215 C216 C211 120.9(2) . . ? C215 C216 H12 119.5 . . ? C211 C216 H12 119.5 . . ? C214 C215 C216 120.0(2) . . ? C214 C215 H13 120.0 . . ? C216 C215 H13 120.0 . . ? C213 C214 C215 119.9(2) . . ? C213 C214 H14 120.1 . . ? C215 C214 H14 120.1 . . ? C214 C213 C212 120.1(2) . . ? C214 C213 H15 120.0 . . ? C212 C213 H15 120.0 . . ? C211 C212 C213 120.7(2) . . ? C211 C212 H16 119.6 . . ? C213 C212 H16 119.6 . . ? C222 C221 C226 119.3(2) . . ? C222 C221 P2 119.50(17) . . ? C226 C221 P2 120.77(17) . . ? C223 C222 C221 120.0(2) . . ? C223 C222 H22 120.0 . . ? C221 C222 H22 120.0 . . ? C224 C223 C222 120.4(2) . . ? C224 C223 H23 119.8 . . ? C222 C223 H23 119.8 . . ? C223 C224 C225 120.0(2) . . ? C223 C224 H24 120.0 . . ? C225 C224 H24 120.0 . . ? C226 C225 C224 119.9(2) . . ? C226 C225 H25 120.1 . . ? C224 C225 H25 120.1 . . ? C225 C226 C221 120.3(2) . . ? C225 C226 H26 119.8 . . ? C221 C226 H26 119.8 . . ? C232 C231 C236 119.3(2) . . ? C232 C231 P2 118.44(16) . . ? C236 C231 P2 122.21(17) . . ? C233 C232 C231 120.6(2) . . ? C233 C232 H32 119.7 . . ? C231 C232 H32 119.7 . . ? C234 C233 C232 119.5(2) . . ? C234 C233 H33 120.3 . . ? C232 C233 H33 120.3 . . ? C233 C234 C235 120.4(2) . . ? C233 C234 H34 119.8 . . ? C235 C234 H34 119.8 . . ? C236 C235 C234 120.2(2) . . ? C236 C235 H35 119.9 . . ? C234 C235 H35 119.9 . . ? C235 C236 C231 120.0(2) . . ? C235 C236 H36 120.0 . . ? C231 C236 H36 120.0 . . ? C126 C121 C122 119.4(2) . . ? C126 C121 P1 121.73(17) . . ? C122 C121 P1 118.86(17) . . ? C125 C126 C121 120.4(2) . . ? C125 C126 H42 119.8 . . ? C121 C126 H42 119.8 . . ? C124 C125 C126 120.0(2) . . ? C124 C125 H43 120.0 . . ? C126 C125 H43 120.0 . . ? C125 C124 C123 120.0(2) . . ? C125 C124 H44 120.0 . . ? C123 C124 H44 120.0 . . ? C122 C123 C124 120.4(2) . . ? C122 C123 H45 119.8 . . ? C124 C123 H45 119.8 . . ? C123 C122 C121 119.8(2) . . ? C123 C122 H46 120.1 . . ? C121 C122 H46 120.1 . . ? C132 C131 C136 119.4(2) . . ? C132 C131 P1 120.59(17) . . ? C136 C131 P1 120.00(17) . . ? C131 C132 C133 120.3(2) . . ? C131 C132 H52 119.9 . . ? C133 C132 H52 119.9 . . ? C134 C133 C132 119.7(2) . . ? C134 C133 H53 120.1 . . ? C132 C133 H53 120.1 . . ? C135 C134 C133 120.3(2) . . ? C135 C134 H54 119.9 . . ? C133 C134 H54 119.9 . . ? C134 C135 C136 120.8(2) . . ? C134 C135 H55 119.6 . . ? C136 C135 H55 119.6 . . ? C135 C136 C131 119.5(2) . . ? C135 C136 H56 120.2 . . ? C131 C136 H56 120.2 . . ? C116 C111 C112 118.3(2) . . ? C116 C111 P1 123.11(19) . . ? C112 C111 P1 118.57(17) . . ? C113 C112 C111 120.6(2) . . ? C113 C112 H62 119.7 . . ? C111 C112 H62 119.7 . . ? C114 C113 C112 120.4(3) . . ? C114 C113 H63 119.8 . . ? C112 C113 H63 119.8 . . ? C113 C114 C115 119.7(2) . . ? C113 C114 H64 120.2 . . ? C115 C114 H64 120.2 . . ? C114 C115 C116 120.8(2) . . ? C114 C115 H65 119.6 . . ? C116 C115 H65 119.6 . . ? C115 C116 C111 120.2(2) . . ? C115 C116 H66 119.9 . . ? C111 C116 H66 119.9 . . ? F3 B1 F2 109.8(3) . . ? F3 B1 F1 109.6(3) . . ? F2 B1 F1 111.5(3) . . ? F3 B1 F4 111.1(3) . . ? F2 B1 F4 106.7(3) . . ? F1 B1 F4 108.2(2) . . ? C221 P2 C231 108.54(10) . . ? C221 P2 C211 101.94(10) . . ? C231 P2 C211 104.88(10) . . ? C221 P2 Pd1 114.82(7) . . ? C231 P2 Pd1 109.39(8) . . ? C211 P2 Pd1 116.51(7) . . ? C121 P1 C131 107.33(10) . . ? C121 P1 C111 105.05(10) . . ? C131 P1 C111 102.44(11) . . ? C121 P1 Pd1 110.99(8) . . ? C131 P1 Pd1 112.12(8) . . ? C111 P1 Pd1 118.05(7) . . ? C01 Pd1 C1 17.5(3) . . ? C01 Pd1 P1 90.7(4) . . ? C1 Pd1 P1 91.11(8) . . ? C01 Pd1 P2 89.1(4) . . ? C1 Pd1 P2 88.86(8) . . ? P1 Pd1 P2 179.30(2) . . ? C01 Pd1 Cl1 174.9(4) . . ? C1 Pd1 Cl1 167.57(10) . . ? P1 Pd1 Cl1 88.74(3) . . ? P2 Pd1 Cl1 91.44(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C6 C5 0.9(4) . . . . ? Pd1 C1 C6 C5 -179.1(2) . . . . ? C1 C6 C5 C4 0.1(5) . . . . ? C6 C5 C4 C3 -0.8(5) . . . . ? C5 C4 C3 N2 0.4(5) . . . . ? C6 C1 N2 C3 -1.2(4) . . . . ? Pd1 C1 N2 C3 178.7(2) . . . . ? C6 C1 N2 C21 179.8(3) . . . . ? Pd1 C1 N2 C21 -0.2(4) . . . . ? C4 C3 N2 C1 0.6(5) . . . . ? C4 C3 N2 C21 179.6(3) . . . . ? N02 C01 C06 C05 -2(2) . . . . ? Pd1 C01 C06 C05 178.0(12) . . . . ? C01 C06 C05 C04 4(2) . . . . ? C06 C05 C04 C03 -4(3) . . . . ? C05 C04 C03 N02 3(3) . . . . ? C06 C01 N02 C03 1.2(17) . . . . ? Pd1 C01 N02 C03 -179.2(10) . . . . ? C06 C01 N02 C021 178.2(12) . . . . ? Pd1 C01 N02 C021 -2.2(16) . . . . ? C04 C03 N02 C01 -2(2) . . . . ? C04 C03 N02 C021 -178.7(14) . . . . ? C212 C211 C216 C215 0.5(3) . . . . ? P2 C211 C216 C215 177.20(18) . . . . ? C211 C216 C215 C214 0.3(4) . . . . ? C216 C215 C214 C213 -1.0(4) . . . . ? C215 C214 C213 C212 0.9(4) . . . . ? C216 C211 C212 C213 -0.6(3) . . . . ? P2 C211 C212 C213 -177.29(18) . . . . ? C214 C213 C212 C211 -0.1(4) . . . . ? C226 C221 C222 C223 0.1(3) . . . . ? P2 C221 C222 C223 -172.51(18) . . . . ? C221 C222 C223 C224 -0.4(4) . . . . ? C222 C223 C224 C225 0.7(4) . . . . ? C223 C224 C225 C226 -0.7(4) . . . . ? C224 C225 C226 C221 0.4(4) . . . . ? C222 C221 C226 C225 -0.1(3) . . . . ? P2 C221 C226 C225 172.41(18) . . . . ? C236 C231 C232 C233 -1.2(3) . . . . ? P2 C231 C232 C233 176.61(17) . . . . ? C231 C232 C233 C234 -1.3(3) . . . . ? C232 C233 C234 C235 2.6(4) . . . . ? C233 C234 C235 C236 -1.4(4) . . . . ? C234 C235 C236 C231 -1.1(4) . . . . ? C232 C231 C236 C235 2.4(3) . . . . ? P2 C231 C236 C235 -175.36(18) . . . . ? C122 C121 C126 C125 1.6(3) . . . . ? P1 C121 C126 C125 179.50(17) . . . . ? C121 C126 C125 C124 0.8(3) . . . . ? C126 C125 C124 C123 -2.3(3) . . . . ? C125 C124 C123 C122 1.4(4) . . . . ? C124 C123 C122 C121 1.0(3) . . . . ? C126 C121 C122 C123 -2.5(3) . . . . ? P1 C121 C122 C123 179.57(17) . . . . ? C136 C131 C132 C133 0.0(3) . . . . ? P1 C131 C132 C133 -179.18(17) . . . . ? C131 C132 C133 C134 0.0(4) . . . . ? C132 C133 C134 C135 -0.3(4) . . . . ? C133 C134 C135 C136 0.5(4) . . . . ? C134 C135 C136 C131 -0.5(4) . . . . ? C132 C131 C136 C135 0.3(3) . . . . ? P1 C131 C136 C135 179.42(18) . . . . ? C116 C111 C112 C113 1.4(3) . . . . ? P1 C111 C112 C113 -179.06(18) . . . . ? C111 C112 C113 C114 -1.4(4) . . . . ? C112 C113 C114 C115 0.5(4) . . . . ? C113 C114 C115 C116 0.6(4) . . . . ? C114 C115 C116 C111 -0.6(4) . . . . ? C112 C111 C116 C115 -0.4(3) . . . . ? P1 C111 C116 C115 -179.91(17) . . . . ? C222 C221 P2 C231 -156.74(17) . . . . ? C226 C221 P2 C231 30.7(2) . . . . ? C222 C221 P2 C211 92.91(19) . . . . ? C226 C221 P2 C211 -79.62(19) . . . . ? C222 C221 P2 Pd1 -34.0(2) . . . . ? C226 C221 P2 Pd1 153.47(16) . . . . ? C232 C231 P2 C221 98.11(18) . . . . ? C236 C231 P2 C221 -84.1(2) . . . . ? C232 C231 P2 C211 -153.54(17) . . . . ? C236 C231 P2 C211 24.2(2) . . . . ? C232 C231 P2 Pd1 -27.86(19) . . . . ? C236 C231 P2 Pd1 149.93(17) . . . . ? C212 C211 P2 C221 -22.8(2) . . . . ? C216 C211 P2 C221 160.51(18) . . . . ? C212 C211 P2 C231 -135.94(18) . . . . ? C216 C211 P2 C231 47.4(2) . . . . ? C212 C211 P2 Pd1 102.97(17) . . . . ? C216 C211 P2 Pd1 -73.69(19) . . . . ? C126 C121 P1 C131 0.9(2) . . . . ? C122 C121 P1 C131 178.78(17) . . . . ? C126 C121 P1 C111 109.38(19) . . . . ? C122 C121 P1 C111 -72.70(19) . . . . ? C126 C121 P1 Pd1 -121.96(17) . . . . ? C122 C121 P1 Pd1 55.96(18) . . . . ? C132 C131 P1 C121 -107.42(19) . . . . ? C136 C131 P1 C121 73.4(2) . . . . ? C132 C131 P1 C111 142.25(19) . . . . ? C136 C131 P1 C111 -36.9(2) . . . . ? C132 C131 P1 Pd1 14.7(2) . . . . ? C136 C131 P1 Pd1 -164.45(16) . . . . ? C116 C111 P1 C121 14.9(2) . . . . ? C112 C111 P1 C121 -164.64(17) . . . . ? C116 C111 P1 C131 126.91(19) . . . . ? C112 C111 P1 C131 -52.61(19) . . . . ? C116 C111 P1 Pd1 -109.42(18) . . . . ? C112 C111 P1 Pd1 71.06(19) . . . . ? N02 C01 Pd1 C1 2.7(6) . . . . ? C06 C01 Pd1 C1 -178(2) . . . . ? N02 C01 Pd1 P1 -88.8(9) . . . . ? C06 C01 Pd1 P1 90.7(11) . . . . ? N02 C01 Pd1 P2 91.9(9) . . . . ? C06 C01 Pd1 P2 -88.6(11) . . . . ? N02 C01 Pd1 Cl1 -172(3) . . . . ? C06 C01 Pd1 Cl1 7(5) . . . . ? N2 C1 Pd1 C01 -0.3(12) . . . . ? C6 C1 Pd1 C01 179.6(13) . . . . ? N2 C1 Pd1 P1 88.4(2) . . . . ? C6 C1 Pd1 P1 -91.6(2) . . . . ? N2 C1 Pd1 P2 -90.9(2) . . . . ? C6 C1 Pd1 P2 89.1(2) . . . . ? N2 C1 Pd1 Cl1 177.6(2) . . . . ? C6 C1 Pd1 Cl1 -2.4(5) . . . . ? C121 P1 Pd1 C01 -130.0(4) . . . . ? C131 P1 Pd1 C01 110.0(4) . . . . ? C111 P1 Pd1 C01 -8.7(4) . . . . ? C121 P1 Pd1 C1 -147.45(13) . . . . ? C131 P1 Pd1 C1 92.54(13) . . . . ? C111 P1 Pd1 C1 -26.15(14) . . . . ? C121 P1 Pd1 P2 -59.6(17) . . . . ? C131 P1 Pd1 P2 -180(100) . . . . ? C111 P1 Pd1 P2 61.7(17) . . . . ? C121 P1 Pd1 Cl1 44.98(8) . . . . ? C131 P1 Pd1 Cl1 -75.03(8) . . . . ? C111 P1 Pd1 Cl1 166.28(9) . . . . ? C221 P2 Pd1 C01 137.1(4) . . . . ? C231 P2 Pd1 C01 -100.6(4) . . . . ? C211 P2 Pd1 C01 18.1(4) . . . . ? C221 P2 Pd1 C1 154.60(13) . . . . ? C231 P2 Pd1 C1 -83.11(13) . . . . ? C211 P2 Pd1 C1 35.56(13) . . . . ? C221 P2 Pd1 P1 66.7(17) . . . . ? C231 P2 Pd1 P1 -171(13) . . . . ? C211 P2 Pd1 P1 -52.3(17) . . . . ? C221 P2 Pd1 Cl1 -37.83(8) . . . . ? C231 P2 Pd1 Cl1 84.46(8) . . . . ? C211 P2 Pd1 Cl1 -156.86(8) . . . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.919 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.075 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 0.000 0.000 0.500 513 207 ' ' _platon_squeeze_details ; ? ; #===END data_3bOTf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H37 Cl N P2 Pd, C F3 O3 S' _chemical_formula_sum 'C43 H37 Cl F3 N O3 P2 Pd S' _chemical_formula_weight 908.59 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.672(5) _cell_length_b 18.609(6) _cell_length_c 18.404(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.724(5) _cell_angle_gamma 90.00 _cell_volume 4786(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1801 _cell_measurement_theta_min 2.389 _cell_measurement_theta_max 21.350 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7272 _exptl_absorpt_correction_T_max 0.9536 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24537 _diffrn_reflns_av_R_equivalents 0.1173 _diffrn_reflns_av_sigmaI/netI 0.1984 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8709 _reflns_number_gt 3809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. During the structure refinement 2 dichloromethane molecules were found, but could not be refined properly due to disorder. The SQUEEZE routine of Platon was used to modify the hkl-file (end of file)! ; _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^)+(0.0896P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8709 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1497 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_restrained_S_all 0.831 _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 C01 C 1.0061(7) 0.6929(5) 0.3464(5) 0.042(2) Uani 1 1 d . . . C3 C 0.6443(5) 0.8012(4) 0.4378(4) 0.0188(18) Uani 1 1 d . . . C2 C 0.6564(5) 0.7869(4) 0.3662(4) 0.0207(17) Uani 1 1 d . . . H2 H 0.7140 0.7655 0.3633 0.025 Uiso 1 1 calc R . . C6 C 0.5039(5) 0.8363(4) 0.3036(5) 0.029(2) Uani 1 1 d . . . H4 H 0.4556 0.8483 0.2577 0.035 Uiso 1 1 calc R . . C5 C 0.4906(5) 0.8516(4) 0.3709(5) 0.028(2) Uani 1 1 d . . . H5 H 0.4327 0.8736 0.3722 0.033 Uiso 1 1 calc R . . C4 C 0.5615(6) 0.8352(4) 0.4391(5) 0.030(2) Uani 1 1 d . . . H6 H 0.5525 0.8476 0.4865 0.036 Uiso 1 1 calc R . . C11 C 0.5982(6) 0.7857(5) 0.2259(4) 0.031(2) Uani 1 1 d . . . H31A H 0.5513 0.7491 0.2003 0.046 Uiso 1 1 calc R . . H31B H 0.6630 0.7669 0.2342 0.046 Uiso 1 1 calc R . . H31C H 0.5891 0.8288 0.1940 0.046 Uiso 1 1 calc R . . C111 C 0.7906(5) 0.9217(4) 0.4298(4) 0.0227(19) Uani 1 1 d . . . C112 C 0.8385(6) 0.8995(4) 0.3797(5) 0.032(2) Uani 1 1 d . . . H112 H 0.8963 0.8731 0.3985 0.039 Uiso 1 1 calc R . . C113 C 0.8032(6) 0.9152(4) 0.3014(5) 0.031(2) Uani 1 1 d . . . H113 H 0.8357 0.8989 0.2670 0.038 Uiso 1 1 calc R . . C114 C 0.7193(6) 0.9555(4) 0.2753(5) 0.031(2) Uani 1 1 d . . . H114 H 0.6946 0.9670 0.2227 0.037 Uiso 1 1 calc R . . C115 C 0.6720(6) 0.9787(4) 0.3249(5) 0.028(2) Uani 1 1 d . . . H115 H 0.6158 1.0070 0.3062 0.033 Uiso 1 1 calc R . . C116 C 0.7055(6) 0.9613(4) 0.4024(5) 0.028(2) Uani 1 1 d . . . H116 H 0.6712 0.9760 0.4361 0.034 Uiso 1 1 calc R . . C121 C 0.9500(5) 0.8695(4) 0.5510(4) 0.026(2) Uani 1 1 d . . . C122 C 0.9800(6) 0.8021(5) 0.5322(4) 0.034(2) Uani 1 1 d . . . H122 H 0.9339 0.7677 0.5060 0.040 Uiso 1 1 calc R . . C123 C 1.0767(5) 0.7857(5) 0.5517(5) 0.034(2) Uani 1 1 d . . . H123 H 1.0960 0.7400 0.5387 0.041 Uiso 1 1 calc R . . C124 C 1.1459(6) 0.8352(5) 0.5899(4) 0.032(2) Uani 1 1 d . . . H124 H 1.2120 0.8237 0.6027 0.039 Uiso 1 1 calc R . . C125 C 1.1167(6) 0.9013(5) 0.6090(4) 0.033(2) Uani 1 1 d . . . H125 H 1.1631 0.9348 0.6367 0.040 Uiso 1 1 calc R . . C126 C 1.0191(6) 0.9196(4) 0.5878(4) 0.028(2) Uani 1 1 d . . . H126 H 1.0003 0.9662 0.5988 0.034 Uiso 1 1 calc R . . C131 C 0.8071(5) 0.9599(5) 0.5846(4) 0.028(2) Uani 1 1 d . . . C132 C 0.7713(5) 0.9447(5) 0.6447(5) 0.032(2) Uani 1 1 d . . . H132 H 0.7551 0.8967 0.6530 0.038 Uiso 1 1 calc R . . C133 C 0.7590(6) 0.9995(5) 0.6930(5) 0.043(3) Uani 1 1 d . . . H133 H 0.7357 0.9879 0.7344 0.052 Uiso 1 1 calc R . . C134 C 0.7798(6) 1.0689(6) 0.6818(6) 0.047(3) Uani 1 1 d . . . H134 H 0.7692 1.1059 0.7139 0.056 Uiso 1 1 calc R . . C135 C 0.8158(7) 1.0847(5) 0.6242(6) 0.047(3) Uani 1 1 d . . . H135 H 0.8325 1.1330 0.6173 0.057 Uiso 1 1 calc R . . C136 C 0.8294(6) 1.0305(4) 0.5733(5) 0.035(2) Uani 1 1 d . . . H136 H 0.8533 1.0427 0.5324 0.042 Uiso 1 1 calc R . . C211 C 0.6283(5) 0.6311(4) 0.4336(4) 0.0213(18) Uani 1 1 d . . . C212 C 0.6711(6) 0.5997(4) 0.3850(4) 0.029(2) Uani 1 1 d . . . H212 H 0.7364 0.5859 0.4037 0.035 Uiso 1 1 calc R . . C213 C 0.6203(6) 0.5878(4) 0.3083(4) 0.034(2) Uani 1 1 d . . . H213 H 0.6502 0.5662 0.2746 0.041 Uiso 1 1 calc R . . C214 C 0.5241(6) 0.6084(4) 0.2826(5) 0.036(2) Uani 1 1 d . . . H214 H 0.4891 0.6015 0.2304 0.043 Uiso 1 1 calc R . . C215 C 0.4794(6) 0.6381(4) 0.3300(5) 0.035(2) Uani 1 1 d . . . H215 H 0.4134 0.6501 0.3114 0.042 Uiso 1 1 calc R . . C216 C 0.5313(5) 0.6511(4) 0.4066(4) 0.0263(19) Uani 1 1 d . . . H216 H 0.5011 0.6731 0.4399 0.032 Uiso 1 1 calc R . . C221 C 0.8017(5) 0.6047(4) 0.5628(4) 0.0214(19) Uani 1 1 d . . . C222 C 0.8146(6) 0.5578(4) 0.6260(4) 0.028(2) Uani 1 1 d . . . H222 H 0.7664 0.5539 0.6505 0.034 Uiso 1 1 calc R . . C223 C 0.8975(6) 0.5178(5) 0.6517(5) 0.035(2) Uani 1 1 d . . . H223 H 0.9057 0.4861 0.6937 0.041 Uiso 1 1 calc R . . C224 C 0.9682(6) 0.5232(5) 0.6174(5) 0.035(2) Uani 1 1 d . . . H224 H 1.0246 0.4950 0.6348 0.042 Uiso 1 1 calc R . . C225 C 0.9561(6) 0.5708(4) 0.5566(5) 0.035(2) Uani 1 1 d . . . H225 H 1.0052 0.5753 0.5330 0.042 Uiso 1 1 calc R . . C226 C 0.8738(6) 0.6116(4) 0.5300(5) 0.0268(19) Uani 1 1 d . . . H226 H 0.8671 0.6444 0.4891 0.032 Uiso 1 1 calc R . . C231 C 0.6188(5) 0.6384(4) 0.5855(4) 0.0221(18) Uani 1 1 d . . . C232 C 0.5734(6) 0.5706(5) 0.5793(4) 0.031(2) Uani 1 1 d . . . H232 H 0.5841 0.5363 0.5445 0.038 Uiso 1 1 calc R . . C233 C 0.5148(6) 0.5526(5) 0.6215(5) 0.035(2) Uani 1 1 d . . . H233 H 0.4848 0.5068 0.6158 0.042 Uiso 1 1 calc R . . C234 C 0.4996(6) 0.6018(5) 0.6725(5) 0.042(2) Uani 1 1 d . . . H234 H 0.4593 0.5897 0.7025 0.050 Uiso 1 1 calc R . . C235 C 0.5429(6) 0.6691(5) 0.6804(5) 0.037(2) Uani 1 1 d . . . H235 H 0.5311 0.7029 0.7151 0.044 Uiso 1 1 calc R . . C236 C 0.6028(6) 0.6871(5) 0.6384(5) 0.031(2) Uani 1 1 d . . . H236 H 0.6333 0.7327 0.6453 0.037 Uiso 1 1 calc R . . P1 P 0.82274(15) 0.88687(11) 0.52602(11) 0.0249(5) Uani 1 1 d . . . P2 P 0.69527(14) 0.66113(11) 0.52922(11) 0.0234(5) Uani 1 1 d . . . Pd1 Pd 0.74615(4) 0.77946(3) 0.53521(3) 0.02179(19) Uani 1 1 d . . . Cl1 Cl 0.84714(14) 0.76018(11) 0.66136(11) 0.0319(5) Uani 1 1 d . . . F1 F 1.0422(4) 0.6565(3) 0.4126(3) 0.0487(14) Uani 1 1 d . . . F2 F 1.0534(4) 0.6704(3) 0.2997(3) 0.0622(17) Uani 1 1 d . . . F3 F 1.0365(4) 0.7618(3) 0.3661(3) 0.0481(14) Uani 1 1 d . . . S1 S 0.88042(17) 0.68613(13) 0.30905(13) 0.0372(6) Uani 1 1 d . . . O1 O 0.8474(4) 0.7118(3) 0.3706(3) 0.0378(15) Uani 1 1 d . . . O2 O 0.8667(5) 0.6112(3) 0.2921(4) 0.059(2) Uani 1 1 d . . . O3 O 0.8579(5) 0.7336(3) 0.2438(3) 0.0510(18) Uani 1 1 d . . . N1 N 0.5848(5) 0.8039(3) 0.3003(4) 0.0302(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C01 0.044(6) 0.050(6) 0.030(6) 0.006(5) 0.011(5) 0.003(5) C3 0.019(4) 0.007(4) 0.019(4) -0.003(3) -0.009(3) -0.002(3) C2 0.030(4) 0.020(4) 0.005(4) 0.002(3) -0.004(3) -0.003(3) C6 0.018(4) 0.038(5) 0.024(5) 0.003(4) -0.007(4) 0.008(4) C5 0.023(4) 0.034(5) 0.025(5) -0.009(4) 0.005(4) -0.003(4) C4 0.036(5) 0.030(5) 0.018(5) -0.013(4) 0.000(4) -0.005(4) C11 0.034(5) 0.044(5) 0.008(4) -0.004(4) -0.003(3) -0.009(4) C111 0.021(4) 0.027(5) 0.012(4) 0.004(3) -0.008(3) -0.004(3) C112 0.036(5) 0.026(5) 0.030(5) 0.008(4) 0.003(4) -0.005(4) C113 0.030(5) 0.036(5) 0.026(5) 0.007(4) 0.005(4) -0.001(4) C114 0.028(5) 0.037(5) 0.015(5) 0.008(4) -0.010(4) -0.009(4) C115 0.024(5) 0.023(5) 0.031(5) 0.010(4) 0.000(4) 0.000(4) C116 0.030(5) 0.023(5) 0.026(5) 0.005(4) 0.002(4) -0.011(4) C121 0.024(4) 0.029(5) 0.019(5) -0.001(4) -0.001(4) -0.013(4) C122 0.033(5) 0.038(6) 0.021(5) 0.001(4) -0.004(4) -0.004(4) C123 0.025(5) 0.043(6) 0.029(5) -0.005(4) 0.000(4) 0.002(4) C124 0.024(5) 0.051(6) 0.016(5) 0.010(4) -0.003(4) 0.000(4) C125 0.027(5) 0.053(6) 0.017(5) 0.008(4) 0.003(4) -0.006(4) C126 0.032(5) 0.032(5) 0.014(4) -0.003(4) -0.003(4) -0.005(4) C131 0.021(4) 0.041(6) 0.015(5) -0.001(4) -0.003(4) -0.004(4) C132 0.023(5) 0.036(5) 0.026(5) -0.008(4) -0.007(4) 0.000(4) C133 0.043(6) 0.055(7) 0.034(6) -0.020(5) 0.013(5) -0.005(5) C134 0.035(6) 0.055(7) 0.038(6) -0.015(5) -0.005(5) -0.006(5) C135 0.054(6) 0.029(6) 0.052(7) -0.015(5) 0.005(5) -0.009(5) C136 0.053(6) 0.024(5) 0.023(5) 0.000(4) 0.002(4) 0.002(4) C211 0.030(5) 0.024(5) 0.007(4) -0.002(3) 0.002(3) -0.004(4) C212 0.031(5) 0.032(5) 0.017(5) -0.003(4) -0.005(4) 0.002(4) C213 0.049(6) 0.035(5) 0.015(5) -0.014(4) 0.007(4) -0.003(4) C214 0.039(5) 0.041(6) 0.016(5) -0.004(4) -0.007(4) -0.014(4) C215 0.039(5) 0.034(5) 0.021(5) 0.005(4) -0.006(4) 0.006(4) C216 0.018(4) 0.030(5) 0.023(5) -0.004(4) -0.006(3) -0.001(3) C221 0.032(5) 0.006(4) 0.020(4) -0.008(3) -0.001(4) 0.001(3) C222 0.040(5) 0.026(5) 0.014(4) -0.004(4) 0.001(4) -0.009(4) C223 0.026(5) 0.046(6) 0.026(5) 0.005(4) -0.001(4) 0.017(4) C224 0.027(5) 0.039(6) 0.031(5) 0.000(4) -0.003(4) 0.001(4) C225 0.033(5) 0.030(5) 0.040(6) -0.009(4) 0.011(4) -0.001(4) C226 0.031(5) 0.020(5) 0.026(5) -0.001(4) 0.003(4) 0.003(4) C231 0.018(4) 0.033(5) 0.007(4) -0.004(3) -0.008(3) 0.001(3) C232 0.031(5) 0.041(6) 0.017(5) -0.002(4) -0.002(4) -0.012(4) C233 0.034(5) 0.047(6) 0.023(5) 0.014(4) 0.009(4) -0.004(4) C234 0.022(5) 0.068(7) 0.031(6) 0.016(5) 0.002(4) 0.000(5) C235 0.031(5) 0.056(7) 0.023(5) -0.005(4) 0.007(4) 0.011(5) C236 0.029(5) 0.033(5) 0.026(5) -0.001(4) 0.001(4) -0.004(4) P1 0.0272(12) 0.0265(12) 0.0118(11) 0.0003(9) -0.0076(9) -0.0034(9) P2 0.0248(11) 0.0269(12) 0.0131(11) 0.0003(9) -0.0022(9) -0.0008(9) Pd1 0.0239(3) 0.0246(3) 0.0091(3) -0.0002(3) -0.0066(2) -0.0009(3) Cl1 0.0339(12) 0.0372(13) 0.0133(10) 0.0004(9) -0.0099(9) 0.0012(9) F1 0.051(3) 0.056(4) 0.031(3) 0.013(3) 0.000(3) 0.010(3) F2 0.053(4) 0.087(5) 0.048(4) 0.000(3) 0.018(3) 0.022(3) F3 0.052(3) 0.042(4) 0.045(3) 0.003(3) 0.007(3) -0.015(3) S1 0.0433(14) 0.0378(14) 0.0253(13) -0.0035(11) 0.0025(11) 0.0047(11) O1 0.040(4) 0.044(4) 0.031(3) 0.003(3) 0.013(3) 0.005(3) O2 0.063(5) 0.035(4) 0.064(5) -0.026(3) -0.005(4) 0.007(3) O3 0.063(4) 0.059(5) 0.025(4) 0.014(3) 0.005(3) 0.015(3) N1 0.039(4) 0.028(4) 0.017(4) 0.000(3) -0.001(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C01 F2 1.328(10) . ? C01 F1 1.353(10) . ? C01 F3 1.369(10) . ? C01 S1 1.766(9) . ? C3 C4 1.376(10) . ? C3 C2 1.406(10) . ? C3 Pd1 1.996(7) . ? C2 N1 1.378(9) . ? C2 H2 0.9500 . ? C6 C5 1.341(10) . ? C6 N1 1.349(9) . ? C6 H4 0.9500 . ? C5 C4 1.399(10) . ? C5 H5 0.9500 . ? C4 H6 0.9500 . ? C11 N1 1.481(9) . ? C11 H31A 0.9800 . ? C11 H31B 0.9800 . ? C11 H31C 0.9800 . ? C111 C112 1.382(11) . ? C111 C116 1.404(10) . ? C111 P1 1.809(7) . ? C112 C113 1.406(11) . ? C112 H112 0.9500 . ? C113 C114 1.395(11) . ? C113 H113 0.9500 . ? C114 C115 1.373(11) . ? C114 H114 0.9500 . ? C115 C116 1.398(11) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C126 1.392(10) . ? C121 C122 1.407(11) . ? C121 P1 1.811(8) . ? C122 C123 1.387(11) . ? C122 H122 0.9500 . ? C123 C124 1.392(11) . ? C123 H123 0.9500 . ? C124 C125 1.384(11) . ? C124 H124 0.9500 . ? C125 C126 1.407(11) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C131 C136 1.384(11) . ? C131 C132 1.390(11) . ? C131 P1 1.792(9) . ? C132 C133 1.402(11) . ? C132 H132 0.9500 . ? C133 C134 1.357(13) . ? C133 H133 0.9500 . ? C134 C135 1.353(13) . ? C134 H134 0.9500 . ? C135 C136 1.432(12) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? C211 C212 1.371(10) . ? C211 C216 1.408(10) . ? C211 P2 1.822(7) . ? C212 C213 1.399(10) . ? C212 H212 0.9500 . ? C213 C214 1.398(11) . ? C213 H213 0.9500 . ? C214 C215 1.359(12) . ? C214 H214 0.9500 . ? C215 C216 1.404(10) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C226 1.374(11) . ? C221 C222 1.421(10) . ? C221 P2 1.826(8) . ? C222 C223 1.380(11) . ? C222 H222 0.9500 . ? C223 C224 1.373(11) . ? C223 H223 0.9500 . ? C224 C225 1.396(12) . ? C224 H224 0.9500 . ? C225 C226 1.384(11) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? C231 C236 1.401(10) . ? C231 C232 1.416(10) . ? C231 P2 1.794(8) . ? C232 C233 1.364(11) . ? C232 H232 0.9500 . ? C233 C234 1.376(12) . ? C233 H233 0.9500 . ? C234 C235 1.392(12) . ? C234 H234 0.9500 . ? C235 C236 1.375(11) . ? C235 H235 0.9500 . ? C236 H236 0.9500 . ? P1 Pd1 2.324(2) . ? P2 Pd1 2.317(2) . ? Pd1 Cl1 2.371(2) . ? S1 O2 1.431(6) . ? S1 O1 1.443(6) . ? S1 O3 1.446(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 C01 F1 106.7(7) . . ? F2 C01 F3 105.9(7) . . ? F1 C01 F3 102.9(7) . . ? F2 C01 S1 114.5(7) . . ? F1 C01 S1 113.0(6) . . ? F3 C01 S1 112.8(6) . . ? C4 C3 C2 117.9(7) . . ? C4 C3 Pd1 120.0(6) . . ? C2 C3 Pd1 122.0(5) . . ? N1 C2 C3 120.1(7) . . ? N1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C5 C6 N1 120.9(7) . . ? C5 C6 H4 119.5 . . ? N1 C6 H4 119.5 . . ? C6 C5 C4 120.3(8) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C3 C4 C5 120.2(8) . . ? C3 C4 H6 119.9 . . ? C5 C4 H6 119.9 . . ? N1 C11 H31A 109.5 . . ? N1 C11 H31B 109.5 . . ? H31A C11 H31B 109.5 . . ? N1 C11 H31C 109.5 . . ? H31A C11 H31C 109.5 . . ? H31B C11 H31C 109.5 . . ? C112 C111 C116 119.6(7) . . ? C112 C111 P1 120.8(6) . . ? C116 C111 P1 118.5(6) . . ? C111 C112 C113 121.3(8) . . ? C111 C112 H112 119.4 . . ? C113 C112 H112 119.4 . . ? C114 C113 C112 118.3(8) . . ? C114 C113 H113 120.8 . . ? C112 C113 H113 120.8 . . ? C115 C114 C113 120.8(7) . . ? C115 C114 H114 119.6 . . ? C113 C114 H114 119.6 . . ? C114 C115 C116 120.9(8) . . ? C114 C115 H115 119.6 . . ? C116 C115 H115 119.6 . . ? C115 C116 C111 119.0(8) . . ? C115 C116 H116 120.5 . . ? C111 C116 H116 120.5 . . ? C126 C121 C122 118.7(7) . . ? C126 C121 P1 123.1(6) . . ? C122 C121 P1 118.2(6) . . ? C123 C122 C121 120.3(8) . . ? C123 C122 H122 119.9 . . ? C121 C122 H122 119.9 . . ? C122 C123 C124 121.1(8) . . ? C122 C123 H123 119.4 . . ? C124 C123 H123 119.4 . . ? C125 C124 C123 118.8(8) . . ? C125 C124 H124 120.6 . . ? C123 C124 H124 120.6 . . ? C124 C125 C126 120.9(8) . . ? C124 C125 H125 119.6 . . ? C126 C125 H125 119.6 . . ? C121 C126 C125 120.1(8) . . ? C121 C126 H126 119.9 . . ? C125 C126 H126 119.9 . . ? C136 C131 C132 118.4(8) . . ? C136 C131 P1 123.3(7) . . ? C132 C131 P1 118.2(6) . . ? C131 C132 C133 120.7(9) . . ? C131 C132 H132 119.7 . . ? C133 C132 H132 119.7 . . ? C134 C133 C132 121.2(10) . . ? C134 C133 H133 119.4 . . ? C132 C133 H133 119.4 . . ? C135 C134 C133 119.0(9) . . ? C135 C134 H134 120.5 . . ? C133 C134 H134 120.5 . . ? C134 C135 C136 121.6(9) . . ? C134 C135 H135 119.2 . . ? C136 C135 H135 119.2 . . ? C131 C136 C135 119.0(9) . . ? C131 C136 H136 120.5 . . ? C135 C136 H136 120.5 . . ? C212 C211 C216 119.8(7) . . ? C212 C211 P2 122.8(6) . . ? C216 C211 P2 116.8(6) . . ? C211 C212 C213 121.1(8) . . ? C211 C212 H212 119.4 . . ? C213 C212 H212 119.4 . . ? C214 C213 C212 118.1(8) . . ? C214 C213 H213 121.0 . . ? C212 C213 H213 121.0 . . ? C215 C214 C213 121.9(8) . . ? C215 C214 H214 119.0 . . ? C213 C214 H214 119.0 . . ? C214 C215 C216 119.7(8) . . ? C214 C215 H215 120.2 . . ? C216 C215 H215 120.2 . . ? C215 C216 C211 119.4(8) . . ? C215 C216 H216 120.3 . . ? C211 C216 H216 120.3 . . ? C226 C221 C222 119.3(7) . . ? C226 C221 P2 119.4(6) . . ? C222 C221 P2 121.2(6) . . ? C223 C222 C221 119.7(8) . . ? C223 C222 H222 120.2 . . ? C221 C222 H222 120.2 . . ? C224 C223 C222 120.9(8) . . ? C224 C223 H223 119.5 . . ? C222 C223 H223 119.5 . . ? C223 C224 C225 119.1(8) . . ? C223 C224 H224 120.5 . . ? C225 C224 H224 120.5 . . ? C226 C225 C224 121.0(8) . . ? C226 C225 H225 119.5 . . ? C224 C225 H225 119.5 . . ? C221 C226 C225 120.0(8) . . ? C221 C226 H226 120.0 . . ? C225 C226 H226 120.0 . . ? C236 C231 C232 117.3(7) . . ? C236 C231 P2 121.0(6) . . ? C232 C231 P2 121.7(6) . . ? C233 C232 C231 122.3(8) . . ? C233 C232 H232 118.8 . . ? C231 C232 H232 118.8 . . ? C232 C233 C234 119.1(9) . . ? C232 C233 H233 120.4 . . ? C234 C233 H233 120.4 . . ? C233 C234 C235 120.3(9) . . ? C233 C234 H234 119.8 . . ? C235 C234 H234 119.8 . . ? C236 C235 C234 120.7(8) . . ? C236 C235 H235 119.6 . . ? C234 C235 H235 119.6 . . ? C235 C236 C231 120.2(8) . . ? C235 C236 H236 119.9 . . ? C231 C236 H236 119.9 . . ? C131 P1 C111 105.9(4) . . ? C131 P1 C121 107.1(4) . . ? C111 P1 C121 104.7(4) . . ? C131 P1 Pd1 117.1(3) . . ? C111 P1 Pd1 113.0(2) . . ? C121 P1 Pd1 108.2(3) . . ? C231 P2 C211 103.7(3) . . ? C231 P2 C221 106.8(4) . . ? C211 P2 C221 107.7(3) . . ? C231 P2 Pd1 116.5(3) . . ? C211 P2 Pd1 114.1(3) . . ? C221 P2 Pd1 107.5(2) . . ? C3 Pd1 P2 90.4(2) . . ? C3 Pd1 P1 90.4(2) . . ? P2 Pd1 P1 165.87(8) . . ? C3 Pd1 Cl1 170.0(2) . . ? P2 Pd1 Cl1 89.94(7) . . ? P1 Pd1 Cl1 91.69(7) . . ? O2 S1 O1 115.8(4) . . ? O2 S1 O3 115.7(4) . . ? O1 S1 O3 113.9(4) . . ? O2 S1 C01 102.5(4) . . ? O1 S1 C01 103.3(4) . . ? O3 S1 C01 103.1(4) . . ? C6 N1 C2 120.6(7) . . ? C6 N1 C11 120.7(7) . . ? C2 N1 C11 118.8(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 C3 C2 N1 -2.9(10) . . . . ? Pd1 C3 C2 N1 -178.9(5) . . . . ? N1 C6 C5 C4 1.0(12) . . . . ? C2 C3 C4 C5 2.9(11) . . . . ? Pd1 C3 C4 C5 179.0(6) . . . . ? C6 C5 C4 C3 -2.1(12) . . . . ? C116 C111 C112 C113 -0.6(11) . . . . ? P1 C111 C112 C113 167.9(6) . . . . ? C111 C112 C113 C114 1.4(12) . . . . ? C112 C113 C114 C115 -0.4(12) . . . . ? C113 C114 C115 C116 -1.4(12) . . . . ? C114 C115 C116 C111 2.3(11) . . . . ? C112 C111 C116 C115 -1.3(11) . . . . ? P1 C111 C116 C115 -170.0(6) . . . . ? C126 C121 C122 C123 1.3(12) . . . . ? P1 C121 C122 C123 -178.5(6) . . . . ? C121 C122 C123 C124 -0.1(13) . . . . ? C122 C123 C124 C125 0.6(12) . . . . ? C123 C124 C125 C126 -2.3(12) . . . . ? C122 C121 C126 C125 -3.1(11) . . . . ? P1 C121 C126 C125 176.8(6) . . . . ? C124 C125 C126 C121 3.6(12) . . . . ? C136 C131 C132 C133 -0.6(11) . . . . ? P1 C131 C132 C133 179.0(6) . . . . ? C131 C132 C133 C134 1.3(13) . . . . ? C132 C133 C134 C135 -2.0(13) . . . . ? C133 C134 C135 C136 2.2(14) . . . . ? C132 C131 C136 C135 0.7(11) . . . . ? P1 C131 C136 C135 -178.9(6) . . . . ? C134 C135 C136 C131 -1.5(13) . . . . ? C216 C211 C212 C213 0.7(12) . . . . ? P2 C211 C212 C213 -169.7(6) . . . . ? C211 C212 C213 C214 -0.3(12) . . . . ? C212 C213 C214 C215 -1.2(13) . . . . ? C213 C214 C215 C216 2.3(13) . . . . ? C214 C215 C216 C211 -1.8(12) . . . . ? C212 C211 C216 C215 0.4(12) . . . . ? P2 C211 C216 C215 171.4(6) . . . . ? C226 C221 C222 C223 -2.5(11) . . . . ? P2 C221 C222 C223 -177.7(6) . . . . ? C221 C222 C223 C224 0.6(12) . . . . ? C222 C223 C224 C225 1.0(13) . . . . ? C223 C224 C225 C226 -0.8(12) . . . . ? C222 C221 C226 C225 2.7(11) . . . . ? P2 C221 C226 C225 178.0(6) . . . . ? C224 C225 C226 C221 -1.1(12) . . . . ? C236 C231 C232 C233 1.1(11) . . . . ? P2 C231 C232 C233 -179.8(6) . . . . ? C231 C232 C233 C234 -0.6(12) . . . . ? C232 C233 C234 C235 0.5(12) . . . . ? C233 C234 C235 C236 -1.1(13) . . . . ? C234 C235 C236 C231 1.7(12) . . . . ? C232 C231 C236 C235 -1.7(11) . . . . ? P2 C231 C236 C235 179.2(6) . . . . ? C136 C131 P1 C111 -37.8(8) . . . . ? C132 C131 P1 C111 142.6(6) . . . . ? C136 C131 P1 C121 73.5(7) . . . . ? C132 C131 P1 C121 -106.1(6) . . . . ? C136 C131 P1 Pd1 -164.9(6) . . . . ? C132 C131 P1 Pd1 15.5(7) . . . . ? C112 C111 P1 C131 144.4(6) . . . . ? C116 C111 P1 C131 -47.0(7) . . . . ? C112 C111 P1 C121 31.4(7) . . . . ? C116 C111 P1 C121 -160.0(6) . . . . ? C112 C111 P1 Pd1 -86.1(6) . . . . ? C116 C111 P1 Pd1 82.5(6) . . . . ? C126 C121 P1 C131 -19.8(8) . . . . ? C122 C121 P1 C131 160.1(6) . . . . ? C126 C121 P1 C111 92.4(7) . . . . ? C122 C121 P1 C111 -87.8(7) . . . . ? C126 C121 P1 Pd1 -146.8(6) . . . . ? C122 C121 P1 Pd1 33.0(7) . . . . ? C236 C231 P2 C211 -135.3(6) . . . . ? C232 C231 P2 C211 45.6(7) . . . . ? C236 C231 P2 C221 111.0(6) . . . . ? C232 C231 P2 C221 -68.0(7) . . . . ? C236 C231 P2 Pd1 -9.1(7) . . . . ? C232 C231 P2 Pd1 171.9(5) . . . . ? C212 C211 P2 C231 -141.6(7) . . . . ? C216 C211 P2 C231 47.7(7) . . . . ? C212 C211 P2 C221 -28.6(8) . . . . ? C216 C211 P2 C221 160.7(6) . . . . ? C212 C211 P2 Pd1 90.7(7) . . . . ? C216 C211 P2 Pd1 -80.0(6) . . . . ? C226 C221 P2 C231 -179.1(6) . . . . ? C222 C221 P2 C231 -4.0(7) . . . . ? C226 C221 P2 C211 70.0(7) . . . . ? C222 C221 P2 C211 -114.9(6) . . . . ? C226 C221 P2 Pd1 -53.4(6) . . . . ? C222 C221 P2 Pd1 121.7(6) . . . . ? C4 C3 Pd1 P2 100.7(6) . . . . ? C2 C3 Pd1 P2 -83.4(6) . . . . ? C4 C3 Pd1 P1 -93.4(6) . . . . ? C2 C3 Pd1 P1 82.5(6) . . . . ? C4 C3 Pd1 Cl1 8.6(16) . . . . ? C2 C3 Pd1 Cl1 -175.6(8) . . . . ? C231 P2 Pd1 C3 -98.6(3) . . . . ? C211 P2 Pd1 C3 22.2(4) . . . . ? C221 P2 Pd1 C3 141.6(4) . . . . ? C231 P2 Pd1 P1 168.1(3) . . . . ? C211 P2 Pd1 P1 -71.1(4) . . . . ? C221 P2 Pd1 P1 48.3(4) . . . . ? C231 P2 Pd1 Cl1 71.3(3) . . . . ? C211 P2 Pd1 Cl1 -167.8(3) . . . . ? C221 P2 Pd1 Cl1 -48.4(3) . . . . ? C131 P1 Pd1 C3 102.1(4) . . . . ? C111 P1 Pd1 C3 -21.5(4) . . . . ? C121 P1 Pd1 C3 -136.9(4) . . . . ? C131 P1 Pd1 P2 -164.6(4) . . . . ? C111 P1 Pd1 P2 71.8(4) . . . . ? C121 P1 Pd1 P2 -43.6(4) . . . . ? C131 P1 Pd1 Cl1 -68.1(3) . . . . ? C111 P1 Pd1 Cl1 168.3(3) . . . . ? C121 P1 Pd1 Cl1 52.9(3) . . . . ? F2 C01 S1 O2 57.9(8) . . . . ? F1 C01 S1 O2 -64.5(8) . . . . ? F3 C01 S1 O2 179.2(6) . . . . ? F2 C01 S1 O1 178.6(6) . . . . ? F1 C01 S1 O1 56.2(8) . . . . ? F3 C01 S1 O1 -60.1(7) . . . . ? F2 C01 S1 O3 -62.6(8) . . . . ? F1 C01 S1 O3 175.0(6) . . . . ? F3 C01 S1 O3 58.7(7) . . . . ? C5 C6 N1 C2 -1.0(12) . . . . ? C5 C6 N1 C11 178.6(7) . . . . ? C3 C2 N1 C6 2.0(11) . . . . ? C3 C2 N1 C11 -177.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.336 _refine_diff_density_min -1.504 _refine_diff_density_rms 0.154 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 0.000 0.500 0.000 548 183 ' ' 2 0.500 1.000 0.500 546 184 ' ' _platon_squeeze_details ; ? ; #===END data_4bOTf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H37 Cl N Ni P2, C F3 O3 S' _chemical_formula_sum 'C43 H37 Cl F3 N Ni O3 P2 S' _chemical_formula_weight 860.90 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.6778(18) _cell_length_b 18.491(2) _cell_length_c 18.317(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.068(2) _cell_angle_gamma 90.00 _cell_volume 4698.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9600 _cell_measurement_theta_min 2.507 _cell_measurement_theta_max 26.330 _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8076 _exptl_absorpt_correction_T_max 0.9398 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23577 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8384 _reflns_number_gt 6157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. During the structure refinement 2 dichloromethane molecules were found, but could not be refined properly due to disorder. The SQUEEZE routine of Platon was used to modify the hkl-file (see end of file)! ; _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^)+(0.0617P)^2^+0.1765P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8384 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C01 C 1.0103(2) 0.30764(17) -0.15112(18) 0.0323(7) Uani 1 1 d . . . C3 C 0.6494(2) 0.19991(13) -0.05729(15) 0.0169(6) Uani 1 1 d . . . C2 C 0.6547(2) 0.21459(13) -0.13067(15) 0.0183(6) Uani 1 1 d . . . H27 H 0.7098 0.2366 -0.1349 0.022 Uiso 1 1 calc R . . C6 C 0.5011(2) 0.16610(14) -0.19287(16) 0.0242(7) Uani 1 1 d . . . H44 H 0.4518 0.1551 -0.2384 0.029 Uiso 1 1 calc R . . C5 C 0.4913(2) 0.15007(15) -0.12266(16) 0.0247(7) Uani 1 1 d . . . H42 H 0.4355 0.1279 -0.1203 0.030 Uiso 1 1 calc R . . C4 C 0.5652(2) 0.16714(14) -0.05511(16) 0.0203(6) Uani 1 1 d . . . H10 H 0.5581 0.1565 -0.0076 0.024 Uiso 1 1 calc R . . C11 C 0.5924(2) 0.21516(16) -0.27075(16) 0.0266(7) Uani 1 1 d . . . H33A H 0.6581 0.2280 -0.2637 0.040 Uiso 1 1 calc R . . H33B H 0.5511 0.2551 -0.2936 0.040 Uiso 1 1 calc R . . H33C H 0.5747 0.1738 -0.3041 0.040 Uiso 1 1 calc R . . C111 C 0.6285(2) 0.36764(13) -0.06653(15) 0.0186(6) Uani 1 1 d . . . C112 C 0.6706(2) 0.40050(14) -0.11629(16) 0.0231(6) Uani 1 1 d . . . H21 H 0.7355 0.4131 -0.0988 0.028 Uiso 1 1 calc R . . C113 C 0.6144(2) 0.41423(15) -0.19244(17) 0.0300(7) Uani 1 1 d . . . H32 H 0.6421 0.4360 -0.2259 0.036 Uiso 1 1 calc R . . C114 C 0.5184(2) 0.39599(16) -0.21863(16) 0.0317(8) Uani 1 1 d . . . H22 H 0.4817 0.4052 -0.2697 0.038 Uiso 1 1 calc R . . C115 C 0.4764(2) 0.36424(15) -0.16968(17) 0.0295(7) Uani 1 1 d . . . H48 H 0.4113 0.3523 -0.1875 0.035 Uiso 1 1 calc R . . C116 C 0.5314(2) 0.35001(14) -0.09353(16) 0.0224(6) Uani 1 1 d . . . H16 H 0.5028 0.3285 -0.0605 0.027 Uiso 1 1 calc R . . C121 C 0.8046(2) 0.39359(14) 0.06411(15) 0.0174(6) Uani 1 1 d . . . C122 C 0.8757(2) 0.38944(15) 0.02931(16) 0.0223(6) Uani 1 1 d . . . H37 H 0.8675 0.3585 -0.0124 0.027 Uiso 1 1 calc R . . C123 C 0.9590(2) 0.43103(15) 0.05608(17) 0.0252(7) Uani 1 1 d . . . H34 H 1.0056 0.4284 0.0319 0.030 Uiso 1 1 calc R . . C124 C 0.9723(2) 0.47660(15) 0.11918(16) 0.0264(7) Uani 1 1 d . . . H45 H 1.0277 0.5047 0.1372 0.032 Uiso 1 1 calc R . . C125 C 0.9026(2) 0.47978(15) 0.15488(17) 0.0268(7) Uani 1 1 d . . . H29 H 0.9118 0.5097 0.1975 0.032 Uiso 1 1 calc R . . C126 C 0.8189(2) 0.43868(15) 0.12762(15) 0.0218(6) Uani 1 1 d . . . H14 H 0.7724 0.4414 0.1519 0.026 Uiso 1 1 calc R . . C131 C 0.6224(2) 0.35726(15) 0.08629(15) 0.0207(6) Uani 1 1 d . . . C132 C 0.6056(2) 0.30673(16) 0.13621(16) 0.0268(7) Uani 1 1 d . . . H43 H 0.6339 0.2612 0.1412 0.032 Uiso 1 1 calc R . . C133 C 0.5454(3) 0.3248(2) 0.17906(19) 0.0393(8) Uani 1 1 d . . . H46 H 0.5334 0.2911 0.2124 0.047 Uiso 1 1 calc R . . C134 C 0.5042(2) 0.3924(2) 0.17196(19) 0.0387(8) Uani 1 1 d . . . H52 H 0.4650 0.4043 0.2011 0.046 Uiso 1 1 calc R . . C135 C 0.5204(2) 0.44200(18) 0.12233(17) 0.0324(7) Uani 1 1 d . . . H38 H 0.4918 0.4874 0.1175 0.039 Uiso 1 1 calc R . . C136 C 0.5792(2) 0.42477(16) 0.07930(16) 0.0255(7) Uani 1 1 d . . . H30 H 0.5898 0.4587 0.0455 0.031 Uiso 1 1 calc R . . C211 C 0.7911(2) 0.08202(13) -0.07176(15) 0.0189(6) Uani 1 1 d . . . C212 C 0.8406(2) 0.10384(14) -0.12102(16) 0.0217(6) Uani 1 1 d . . . H12 H 0.8971 0.1306 -0.1018 0.026 Uiso 1 1 calc R . . C213 C 0.8061(2) 0.08585(16) -0.19895(16) 0.0268(7) Uani 1 1 d . . . H36 H 0.8390 0.1008 -0.2319 0.032 Uiso 1 1 calc R . . C214 C 0.7226(2) 0.04563(15) -0.22729(16) 0.0263(7) Uani 1 1 d . . . H28 H 0.7000 0.0330 -0.2793 0.032 Uiso 1 1 calc R . . C215 C 0.6724(2) 0.02403(14) -0.17887(16) 0.0228(6) Uani 1 1 d . . . H31 H 0.6161 -0.0028 -0.1985 0.027 Uiso 1 1 calc R . . C216 C 0.7053(2) 0.04207(14) -0.10192(16) 0.0225(6) Uani 1 1 d . . . H20 H 0.6710 0.0279 -0.0697 0.027 Uiso 1 1 calc R . . C221 C 0.9518(2) 0.13480(14) 0.05306(15) 0.0202(6) Uani 1 1 d . . . C222 C 1.0221(2) 0.08428(16) 0.09017(16) 0.0253(7) Uani 1 1 d . . . H40 H 1.0038 0.0386 0.1016 0.030 Uiso 1 1 calc R . . C223 C 1.1181(2) 0.10132(17) 0.10999(17) 0.0309(7) Uani 1 1 d . . . H53 H 1.1644 0.0673 0.1350 0.037 Uiso 1 1 calc R . . C224 C 1.1462(2) 0.16884(18) 0.09297(16) 0.0307(7) Uani 1 1 d . . . H41 H 1.2113 0.1805 0.1071 0.037 Uiso 1 1 calc R . . C225 C 1.0776(2) 0.21879(16) 0.05506(17) 0.0294(7) Uani 1 1 d . . . H51 H 1.0964 0.2639 0.0425 0.035 Uiso 1 1 calc R . . C226 C 0.9810(2) 0.20220(15) 0.03561(16) 0.0244(6) Uani 1 1 d . . . H35 H 0.9350 0.2364 0.0106 0.029 Uiso 1 1 calc R . . C231 C 0.8048(2) 0.04326(15) 0.08417(16) 0.0227(6) Uani 1 1 d . . . C232 C 0.7658(2) 0.05678(16) 0.14193(17) 0.0287(7) Uani 1 1 d . . . H25 H 0.7479 0.1036 0.1498 0.034 Uiso 1 1 calc R . . C233 C 0.7531(2) 0.00087(18) 0.18839(19) 0.0377(8) Uani 1 1 d . . . H50 H 0.7265 0.0103 0.2270 0.045 Uiso 1 1 calc R . . C234 C 0.7798(3) -0.06825(19) 0.1772(2) 0.0427(9) Uani 1 1 d . . . H55 H 0.7714 -0.1057 0.2083 0.051 Uiso 1 1 calc R . . C235 C 0.8191(3) -0.08209(17) 0.1200(2) 0.0443(9) Uani 1 1 d . . . H56 H 0.8378 -0.1289 0.1131 0.053 Uiso 1 1 calc R . . C236 C 0.8312(2) -0.02714(16) 0.07244(19) 0.0343(8) Uani 1 1 d . . . H49 H 0.8566 -0.0371 0.0332 0.041 Uiso 1 1 calc R . . N1 N 0.58222(17) 0.19771(12) -0.19541(12) 0.0200(5) Uani 1 1 d . . . O1 O 0.86409(19) 0.38758(11) -0.21160(14) 0.0465(6) Uani 1 1 d . . . O2 O 0.85981(18) 0.26429(12) -0.25781(12) 0.0406(6) Uani 1 1 d . . . O3 O 0.84816(15) 0.28754(11) -0.13069(12) 0.0292(5) Uani 1 1 d . . . F1 F 1.04294(14) 0.34670(9) -0.08623(10) 0.0387(5) Uani 1 1 d . . . F2 F 1.04038(14) 0.23955(10) -0.13275(11) 0.0425(5) Uani 1 1 d . . . F3 F 1.05391(15) 0.33207(11) -0.19981(11) 0.0501(5) Uani 1 1 d . . . P1 P 0.69949(5) 0.33485(4) 0.02936(4) 0.01668(16) Uani 1 1 d . . . P2 P 0.82241(5) 0.11857(4) 0.02560(4) 0.01782(17) Uani 1 1 d . . . S1 S 0.87999(6) 0.31245(4) -0.19290(4) 0.02805(19) Uani 1 1 d . . . Cl1 Cl 0.84087(5) 0.23682(4) 0.15583(4) 0.02396(17) Uani 1 1 d . . . Ni1 Ni 0.74807(3) 0.220982(17) 0.035080(18) 0.01634(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C01 0.039(2) 0.0301(17) 0.0280(17) -0.0048(14) 0.0117(15) -0.0030(15) C3 0.0194(15) 0.0154(13) 0.0143(13) 0.0008(10) 0.0033(11) 0.0044(11) C2 0.0206(15) 0.0147(13) 0.0171(14) -0.0015(11) 0.0027(12) 0.0013(11) C6 0.0240(16) 0.0204(14) 0.0207(15) -0.0032(12) -0.0030(12) 0.0002(13) C5 0.0236(16) 0.0229(14) 0.0242(16) -0.0002(12) 0.0032(13) -0.0044(13) C4 0.0239(16) 0.0199(14) 0.0174(14) -0.0009(11) 0.0070(12) -0.0010(12) C11 0.0359(18) 0.0286(16) 0.0133(14) -0.0016(12) 0.0051(13) 0.0023(14) C111 0.0269(16) 0.0132(13) 0.0134(13) -0.0016(10) 0.0036(12) 0.0024(12) C112 0.0294(17) 0.0173(14) 0.0217(15) 0.0001(11) 0.0072(13) 0.0000(13) C113 0.045(2) 0.0259(16) 0.0187(15) 0.0029(12) 0.0098(15) 0.0034(14) C114 0.046(2) 0.0306(16) 0.0105(14) -0.0010(12) -0.0025(14) 0.0036(15) C115 0.0294(18) 0.0252(15) 0.0243(16) -0.0022(13) -0.0045(13) 0.0011(13) C116 0.0252(16) 0.0207(14) 0.0192(15) 0.0005(12) 0.0045(12) 0.0041(12) C121 0.0216(15) 0.0155(13) 0.0128(13) 0.0025(11) 0.0025(11) 0.0016(11) C122 0.0265(16) 0.0192(14) 0.0199(15) 0.0026(11) 0.0057(13) 0.0003(12) C123 0.0247(16) 0.0216(15) 0.0295(17) 0.0046(12) 0.0092(13) 0.0017(13) C124 0.0227(16) 0.0231(15) 0.0264(16) 0.0005(12) -0.0015(13) -0.0036(13) C125 0.0312(18) 0.0226(15) 0.0207(15) -0.0056(12) 0.0004(13) -0.0023(13) C126 0.0219(16) 0.0244(15) 0.0183(14) 0.0005(12) 0.0058(12) 0.0006(12) C131 0.0208(15) 0.0242(14) 0.0139(14) -0.0041(11) 0.0016(12) -0.0040(12) C132 0.0321(18) 0.0284(15) 0.0197(15) -0.0022(13) 0.0080(13) -0.0074(14) C133 0.041(2) 0.050(2) 0.0291(18) 0.0005(16) 0.0158(16) -0.0101(18) C134 0.0279(18) 0.059(2) 0.0308(18) -0.0164(17) 0.0119(15) -0.0018(17) C135 0.0274(18) 0.0421(19) 0.0262(17) -0.0077(14) 0.0067(14) 0.0057(15) C136 0.0242(16) 0.0291(16) 0.0198(15) -0.0023(12) 0.0026(13) 0.0019(13) C211 0.0209(15) 0.0145(13) 0.0184(14) -0.0016(11) 0.0025(12) 0.0032(11) C212 0.0243(16) 0.0198(14) 0.0194(15) -0.0004(11) 0.0049(12) 0.0006(12) C213 0.0306(18) 0.0307(16) 0.0190(15) -0.0003(12) 0.0078(13) 0.0052(14) C214 0.0341(18) 0.0240(15) 0.0156(14) -0.0039(12) 0.0011(13) 0.0064(13) C215 0.0226(16) 0.0187(14) 0.0223(15) -0.0047(12) 0.0005(13) 0.0000(12) C216 0.0273(16) 0.0175(14) 0.0217(15) 0.0002(11) 0.0067(13) 0.0039(12) C221 0.0221(15) 0.0238(14) 0.0128(13) -0.0005(11) 0.0028(11) -0.0001(12) C222 0.0290(17) 0.0254(15) 0.0218(15) 0.0032(12) 0.0088(13) 0.0076(13) C223 0.0266(18) 0.0428(19) 0.0220(16) 0.0041(14) 0.0062(13) 0.0123(15) C224 0.0224(16) 0.053(2) 0.0163(15) -0.0062(14) 0.0051(13) 0.0000(15) C225 0.0299(18) 0.0313(16) 0.0246(16) -0.0023(13) 0.0056(14) -0.0072(14) C226 0.0239(16) 0.0277(15) 0.0179(15) 0.0013(12) 0.0017(12) 0.0023(13) C231 0.0231(16) 0.0219(14) 0.0182(15) 0.0066(11) -0.0001(12) -0.0015(12) C232 0.0300(18) 0.0273(16) 0.0276(17) 0.0050(13) 0.0076(14) -0.0013(13) C233 0.038(2) 0.042(2) 0.0323(19) 0.0118(15) 0.0100(16) -0.0052(16) C234 0.039(2) 0.038(2) 0.046(2) 0.0213(17) 0.0066(18) -0.0004(16) C235 0.050(2) 0.0217(17) 0.057(2) 0.0133(16) 0.0118(19) 0.0043(16) C236 0.042(2) 0.0238(16) 0.0358(19) 0.0043(14) 0.0107(16) 0.0034(14) N1 0.0258(13) 0.0191(11) 0.0127(11) -0.0020(9) 0.0029(10) 0.0012(10) O1 0.0548(17) 0.0255(12) 0.0521(16) 0.0143(11) 0.0076(13) 0.0006(11) O2 0.0485(15) 0.0471(14) 0.0247(12) -0.0080(10) 0.0098(11) -0.0129(12) O3 0.0315(12) 0.0332(11) 0.0251(11) 0.0016(9) 0.0122(10) -0.0003(10) F1 0.0421(11) 0.0382(10) 0.0303(10) -0.0073(8) 0.0041(9) -0.0059(9) F2 0.0437(12) 0.0374(11) 0.0454(12) -0.0030(9) 0.0131(10) 0.0104(9) F3 0.0478(13) 0.0654(14) 0.0421(12) -0.0020(10) 0.0217(10) -0.0158(11) P1 0.0208(4) 0.0160(3) 0.0119(3) -0.0009(3) 0.0035(3) -0.0004(3) P2 0.0216(4) 0.0162(3) 0.0133(3) 0.0007(3) 0.0024(3) 0.0003(3) S1 0.0348(5) 0.0241(4) 0.0231(4) 0.0033(3) 0.0066(3) -0.0021(3) Cl1 0.0282(4) 0.0244(4) 0.0130(3) -0.0012(3) -0.0019(3) 0.0000(3) Ni1 0.0202(2) 0.01541(18) 0.01023(18) -0.00044(13) 0.00070(14) -0.00003(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 C01 F3 1.335(4) . ? C01 F1 1.339(3) . ? C01 F2 1.340(4) . ? C01 S1 1.816(4) . ? C3 C4 1.390(4) . ? C3 C2 1.398(4) . ? C3 Ni1 1.874(3) . ? C2 N1 1.346(3) . ? C2 H27 0.9300 . ? C6 N1 1.341(4) . ? C6 C5 1.372(4) . ? C6 H44 0.9300 . ? C5 C4 1.389(4) . ? C5 H42 0.9300 . ? C4 H10 0.9300 . ? C11 N1 1.472(3) . ? C11 H33A 0.9600 . ? C11 H33B 0.9600 . ? C11 H33C 0.9600 . ? C111 C116 1.387(4) . ? C111 C112 1.396(4) . ? C111 P1 1.828(3) . ? C112 C113 1.392(4) . ? C112 H21 0.9300 . ? C113 C114 1.374(5) . ? C113 H32 0.9300 . ? C114 C115 1.374(4) . ? C114 H22 0.9300 . ? C115 C116 1.389(4) . ? C115 H48 0.9300 . ? C116 H16 0.9300 . ? C121 C126 1.390(4) . ? C121 C122 1.392(4) . ? C121 P1 1.823(3) . ? C122 C123 1.390(4) . ? C122 H37 0.9300 . ? C123 C124 1.391(4) . ? C123 H34 0.9300 . ? C124 C125 1.384(4) . ? C124 H45 0.9300 . ? C125 C126 1.392(4) . ? C125 H29 0.9300 . ? C126 H14 0.9300 . ? C131 C132 1.385(4) . ? C131 C136 1.387(4) . ? C131 P1 1.820(3) . ? C132 C133 1.400(4) . ? C132 H43 0.9300 . ? C133 C134 1.375(5) . ? C133 H46 0.9300 . ? C134 C135 1.366(5) . ? C134 H52 0.9300 . ? C135 C136 1.383(4) . ? C135 H38 0.9300 . ? C136 H30 0.9300 . ? C211 C212 1.390(4) . ? C211 C216 1.408(4) . ? C211 P2 1.820(3) . ? C212 C213 1.390(4) . ? C212 H12 0.9300 . ? C213 C214 1.381(4) . ? C213 H36 0.9300 . ? C214 C215 1.384(4) . ? C214 H28 0.9300 . ? C215 C216 1.373(4) . ? C215 H31 0.9300 . ? C216 H20 0.9300 . ? C221 C226 1.389(4) . ? C221 C222 1.393(4) . ? C221 P2 1.824(3) . ? C222 C223 1.371(4) . ? C222 H40 0.9300 . ? C223 C224 1.382(4) . ? C223 H53 0.9300 . ? C224 C225 1.376(4) . ? C224 H41 0.9300 . ? C225 C226 1.378(4) . ? C225 H51 0.9300 . ? C226 H35 0.9300 . ? C231 C232 1.380(4) . ? C231 C236 1.395(4) . ? C231 P2 1.827(3) . ? C232 C233 1.390(4) . ? C232 H25 0.9300 . ? C233 C234 1.371(5) . ? C233 H50 0.9300 . ? C234 C235 1.375(5) . ? C234 H55 0.9300 . ? C235 C236 1.387(4) . ? C235 H56 0.9300 . ? C236 H49 0.9300 . ? O1 S1 1.432(2) . ? O2 S1 1.437(2) . ? O3 S1 1.441(2) . ? P1 Ni1 2.2145(8) . ? P2 Ni1 2.2205(8) . ? Cl1 Ni1 2.2055(8) . ? 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 F3 C01 F1 107.5(3) . . ? F3 C01 F2 107.2(3) . . ? F1 C01 F2 106.9(3) . . ? F3 C01 S1 111.8(2) . . ? F1 C01 S1 111.7(2) . . ? F2 C01 S1 111.5(2) . . ? C4 C3 C2 116.2(2) . . ? C4 C3 Ni1 119.8(2) . . ? C2 C3 Ni1 124.0(2) . . ? N1 C2 C3 121.7(3) . . ? N1 C2 H27 119.1 . . ? C3 C2 H27 119.1 . . ? N1 C6 C5 119.5(3) . . ? N1 C6 H44 120.2 . . ? C5 C6 H44 120.2 . . ? C6 C5 C4 119.7(3) . . ? C6 C5 H42 120.1 . . ? C4 C5 H42 120.1 . . ? C5 C4 C3 121.1(3) . . ? C5 C4 H10 119.5 . . ? C3 C4 H10 119.5 . . ? N1 C11 H33A 109.5 . . ? N1 C11 H33B 109.5 . . ? H33A C11 H33B 109.5 . . ? N1 C11 H33C 109.5 . . ? H33A C11 H33C 109.5 . . ? H33B C11 H33C 109.5 . . ? C116 C111 C112 119.5(3) . . ? C116 C111 P1 117.5(2) . . ? C112 C111 P1 122.5(2) . . ? C113 C112 C111 119.3(3) . . ? C113 C112 H21 120.3 . . ? C111 C112 H21 120.3 . . ? C114 C113 C112 120.6(3) . . ? C114 C113 H32 119.7 . . ? C112 C113 H32 119.7 . . ? C113 C114 C115 120.3(3) . . ? C113 C114 H22 119.9 . . ? C115 C114 H22 119.9 . . ? C114 C115 C116 120.0(3) . . ? C114 C115 H48 120.0 . . ? C116 C115 H48 120.0 . . ? C111 C116 C115 120.3(3) . . ? C111 C116 H16 119.8 . . ? C115 C116 H16 119.8 . . ? C126 C121 C122 119.1(3) . . ? C126 C121 P1 121.9(2) . . ? C122 C121 P1 118.9(2) . . ? C123 C122 C121 120.8(3) . . ? C123 C122 H37 119.6 . . ? C121 C122 H37 119.6 . . ? C122 C123 C124 119.8(3) . . ? C122 C123 H34 120.1 . . ? C124 C123 H34 120.1 . . ? C125 C124 C123 119.5(3) . . ? C125 C124 H45 120.2 . . ? C123 C124 H45 120.2 . . ? C124 C125 C126 120.7(3) . . ? C124 C125 H29 119.7 . . ? C126 C125 H29 119.7 . . ? C121 C126 C125 120.1(3) . . ? C121 C126 H14 120.0 . . ? C125 C126 H14 120.0 . . ? C132 C131 C136 119.6(3) . . ? C132 C131 P1 120.2(2) . . ? C136 C131 P1 120.2(2) . . ? C131 C132 C133 119.3(3) . . ? C131 C132 H43 120.3 . . ? C133 C132 H43 120.3 . . ? C134 C133 C132 120.2(3) . . ? C134 C133 H46 119.9 . . ? C132 C133 H46 119.9 . . ? C135 C134 C133 120.4(3) . . ? C135 C134 H52 119.8 . . ? C133 C134 H52 119.8 . . ? C134 C135 C136 120.1(3) . . ? C134 C135 H38 120.0 . . ? C136 C135 H38 120.0 . . ? C135 C136 C131 120.4(3) . . ? C135 C136 H30 119.8 . . ? C131 C136 H30 119.8 . . ? C212 C211 C216 119.2(2) . . ? C212 C211 P2 120.7(2) . . ? C216 C211 P2 119.1(2) . . ? C213 C212 C211 120.3(3) . . ? C213 C212 H12 119.9 . . ? C211 C212 H12 119.9 . . ? C214 C213 C212 119.8(3) . . ? C214 C213 H36 120.1 . . ? C212 C213 H36 120.1 . . ? C213 C214 C215 120.5(3) . . ? C213 C214 H28 119.8 . . ? C215 C214 H28 119.8 . . ? C216 C215 C214 120.3(3) . . ? C216 C215 H31 119.8 . . ? C214 C215 H31 119.8 . . ? C215 C216 C211 120.0(3) . . ? C215 C216 H20 120.0 . . ? C211 C216 H20 120.0 . . ? C226 C221 C222 118.6(3) . . ? C226 C221 P2 117.1(2) . . ? C222 C221 P2 124.2(2) . . ? C223 C222 C221 120.5(3) . . ? C223 C222 H40 119.7 . . ? C221 C222 H40 119.7 . . ? C222 C223 C224 120.3(3) . . ? C222 C223 H53 119.9 . . ? C224 C223 H53 119.9 . . ? C225 C224 C223 119.8(3) . . ? C225 C224 H41 120.1 . . ? C223 C224 H41 120.1 . . ? C224 C225 C226 120.2(3) . . ? C224 C225 H51 119.9 . . ? C226 C225 H51 119.9 . . ? C225 C226 C221 120.6(3) . . ? C225 C226 H35 119.7 . . ? C221 C226 H35 119.7 . . ? C232 C231 C236 119.5(3) . . ? C232 C231 P2 119.0(2) . . ? C236 C231 P2 121.4(2) . . ? C231 C232 C233 120.4(3) . . ? C231 C232 H25 119.8 . . ? C233 C232 H25 119.8 . . ? C234 C233 C232 120.0(3) . . ? C234 C233 H50 120.0 . . ? C232 C233 H50 120.0 . . ? C233 C234 C235 119.9(3) . . ? C233 C234 H55 120.1 . . ? C235 C234 H55 120.1 . . ? C234 C235 C236 120.9(3) . . ? C234 C235 H56 119.5 . . ? C236 C235 H56 119.5 . . ? C235 C236 C231 119.2(3) . . ? C235 C236 H49 120.4 . . ? C231 C236 H49 120.4 . . ? C6 N1 C2 121.7(2) . . ? C6 N1 C11 119.5(2) . . ? C2 N1 C11 118.8(2) . . ? C131 P1 C121 106.14(12) . . ? C131 P1 C111 102.08(13) . . ? C121 P1 C111 106.81(12) . . ? C131 P1 Ni1 116.13(9) . . ? C121 P1 Ni1 109.11(9) . . ? C111 P1 Ni1 115.75(8) . . ? C211 P2 C221 103.76(13) . . ? C211 P2 C231 104.68(13) . . ? C221 P2 C231 107.32(13) . . ? C211 P2 Ni1 114.85(9) . . ? C221 P2 Ni1 109.40(9) . . ? C231 P2 Ni1 115.90(10) . . ? O1 S1 O2 115.47(15) . . ? O1 S1 O3 115.45(14) . . ? O2 S1 O3 115.08(13) . . ? O1 S1 C01 102.43(15) . . ? O2 S1 C01 102.85(15) . . ? O3 S1 C01 102.72(14) . . ? C3 Ni1 Cl1 167.19(9) . . ? C3 Ni1 P1 90.75(8) . . ? Cl1 Ni1 P1 90.29(3) . . ? C3 Ni1 P2 90.37(8) . . ? Cl1 Ni1 P2 91.91(3) . . ? P1 Ni1 P2 165.03(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 C3 C2 N1 -0.2(4) . . . . ? Ni1 C3 C2 N1 179.29(19) . . . . ? N1 C6 C5 C4 0.4(4) . . . . ? C6 C5 C4 C3 -0.4(4) . . . . ? C2 C3 C4 C5 0.3(4) . . . . ? Ni1 C3 C4 C5 -179.2(2) . . . . ? C116 C111 C112 C113 -0.7(4) . . . . ? P1 C111 C112 C113 170.3(2) . . . . ? C111 C112 C113 C114 0.2(4) . . . . ? C112 C113 C114 C115 0.4(4) . . . . ? C113 C114 C115 C116 -0.5(4) . . . . ? C112 C111 C116 C115 0.6(4) . . . . ? P1 C111 C116 C115 -170.9(2) . . . . ? C114 C115 C116 C111 0.0(4) . . . . ? C126 C121 C122 C123 -1.7(4) . . . . ? P1 C121 C122 C123 -177.3(2) . . . . ? C121 C122 C123 C124 1.0(4) . . . . ? C122 C123 C124 C125 0.3(4) . . . . ? C123 C124 C125 C126 -0.9(4) . . . . ? C122 C121 C126 C125 1.0(4) . . . . ? P1 C121 C126 C125 176.5(2) . . . . ? C124 C125 C126 C121 0.3(4) . . . . ? C136 C131 C132 C133 -0.3(4) . . . . ? P1 C131 C132 C133 -179.5(2) . . . . ? C131 C132 C133 C134 -0.5(5) . . . . ? C132 C133 C134 C135 0.9(5) . . . . ? C133 C134 C135 C136 -0.5(5) . . . . ? C134 C135 C136 C131 -0.2(5) . . . . ? C132 C131 C136 C135 0.6(4) . . . . ? P1 C131 C136 C135 179.9(2) . . . . ? C216 C211 C212 C213 -0.5(4) . . . . ? P2 C211 C212 C213 -168.7(2) . . . . ? C211 C212 C213 C214 -0.5(4) . . . . ? C212 C213 C214 C215 1.0(4) . . . . ? C213 C214 C215 C216 -0.3(4) . . . . ? C214 C215 C216 C211 -0.7(4) . . . . ? C212 C211 C216 C215 1.1(4) . . . . ? P2 C211 C216 C215 169.5(2) . . . . ? C226 C221 C222 C223 1.0(4) . . . . ? P2 C221 C222 C223 -178.9(2) . . . . ? C221 C222 C223 C224 -0.3(4) . . . . ? C222 C223 C224 C225 -0.9(4) . . . . ? C223 C224 C225 C226 1.4(4) . . . . ? C224 C225 C226 C221 -0.8(4) . . . . ? C222 C221 C226 C225 -0.4(4) . . . . ? P2 C221 C226 C225 179.5(2) . . . . ? C236 C231 C232 C233 0.2(5) . . . . ? P2 C231 C232 C233 -178.9(2) . . . . ? C231 C232 C233 C234 0.3(5) . . . . ? C232 C233 C234 C235 0.0(5) . . . . ? C233 C234 C235 C236 -0.8(6) . . . . ? C234 C235 C236 C231 1.4(5) . . . . ? C232 C231 C236 C235 -1.1(5) . . . . ? P2 C231 C236 C235 178.0(3) . . . . ? C5 C6 N1 C2 -0.3(4) . . . . ? C5 C6 N1 C11 -179.7(2) . . . . ? C3 C2 N1 C6 0.2(4) . . . . ? C3 C2 N1 C11 179.6(2) . . . . ? C132 C131 P1 C121 -114.5(2) . . . . ? C136 C131 P1 C121 66.2(2) . . . . ? C132 C131 P1 C111 133.8(2) . . . . ? C136 C131 P1 C111 -45.5(2) . . . . ? C132 C131 P1 Ni1 6.9(3) . . . . ? C136 C131 P1 Ni1 -172.35(19) . . . . ? C126 C121 P1 C131 6.0(3) . . . . ? C122 C121 P1 C131 -178.5(2) . . . . ? C126 C121 P1 C111 114.3(2) . . . . ? C122 C121 P1 C111 -70.2(2) . . . . ? C126 C121 P1 Ni1 -119.9(2) . . . . ? C122 C121 P1 Ni1 55.6(2) . . . . ? C116 C111 P1 C131 -46.4(2) . . . . ? C112 C111 P1 C131 142.4(2) . . . . ? C116 C111 P1 C121 -157.6(2) . . . . ? C112 C111 P1 C121 31.2(3) . . . . ? C116 C111 P1 Ni1 80.7(2) . . . . ? C112 C111 P1 Ni1 -90.5(2) . . . . ? C212 C211 P2 C221 -32.1(2) . . . . ? C216 C211 P2 C221 159.8(2) . . . . ? C212 C211 P2 C231 -144.5(2) . . . . ? C216 C211 P2 C231 47.4(2) . . . . ? C212 C211 P2 Ni1 87.3(2) . . . . ? C216 C211 P2 Ni1 -80.9(2) . . . . ? C226 C221 P2 C211 89.8(2) . . . . ? C222 C221 P2 C211 -90.3(2) . . . . ? C226 C221 P2 C231 -159.7(2) . . . . ? C222 C221 P2 C231 20.1(3) . . . . ? C226 C221 P2 Ni1 -33.2(2) . . . . ? C222 C221 P2 Ni1 146.6(2) . . . . ? C232 C231 P2 C211 -141.3(2) . . . . ? C236 C231 P2 C211 39.6(3) . . . . ? C232 C231 P2 C221 108.8(2) . . . . ? C236 C231 P2 C221 -70.2(3) . . . . ? C232 C231 P2 Ni1 -13.7(3) . . . . ? C236 C231 P2 Ni1 167.2(2) . . . . ? F3 C01 S1 O1 -57.2(2) . . . . ? F1 C01 S1 O1 63.3(2) . . . . ? F2 C01 S1 O1 -177.1(2) . . . . ? F3 C01 S1 O2 63.0(2) . . . . ? F1 C01 S1 O2 -176.6(2) . . . . ? F2 C01 S1 O2 -57.0(2) . . . . ? F3 C01 S1 O3 -177.2(2) . . . . ? F1 C01 S1 O3 -56.8(2) . . . . ? F2 C01 S1 O3 62.8(2) . . . . ? C4 C3 Ni1 Cl1 -4.2(5) . . . . ? C2 C3 Ni1 Cl1 176.3(2) . . . . ? C4 C3 Ni1 P1 -98.9(2) . . . . ? C2 C3 Ni1 P1 81.7(2) . . . . ? C4 C3 Ni1 P2 96.1(2) . . . . ? C2 C3 Ni1 P2 -83.3(2) . . . . ? C131 P1 Ni1 C3 97.50(13) . . . . ? C121 P1 Ni1 C3 -142.65(12) . . . . ? C111 P1 Ni1 C3 -22.19(13) . . . . ? C131 P1 Ni1 Cl1 -69.72(10) . . . . ? C121 P1 Ni1 Cl1 50.12(9) . . . . ? C111 P1 Ni1 Cl1 170.58(11) . . . . ? C131 P1 Ni1 P2 -168.23(13) . . . . ? C121 P1 Ni1 P2 -48.39(15) . . . . ? C111 P1 Ni1 P2 72.07(16) . . . . ? C211 P2 Ni1 C3 22.57(13) . . . . ? C221 P2 Ni1 C3 138.74(12) . . . . ? C231 P2 Ni1 C3 -99.80(13) . . . . ? C211 P2 Ni1 Cl1 -170.04(10) . . . . ? C221 P2 Ni1 Cl1 -53.87(9) . . . . ? C231 P2 Ni1 Cl1 67.59(10) . . . . ? C211 P2 Ni1 P1 -71.74(16) . . . . ? C221 P2 Ni1 P1 44.42(16) . . . . ? C231 P2 Ni1 P1 165.88(14) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.658 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.078 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 0.000 0.500 0.500 531 154 ' ' 2 0.500 0.000 0.000 528 154 ' ' _platon_squeeze_details ; ? ; #===END data_6OTf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H36 Cl2 N P2 Pd, C F3 O3 S, 2(C H2 Cl2)' _chemical_formula_sum 'C45 H40 Cl6 F3 N O3 P2 Pd S' _chemical_formula_weight 1112.88 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 17.6792(17) _cell_length_b 16.9370(17) _cell_length_c 16.3414(16) _cell_angle_alpha 90.00 _cell_angle_beta 106.954(2) _cell_angle_gamma 90.00 _cell_volume 4680.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9999 _cell_measurement_theta_min 2.196 _cell_measurement_theta_max 26.342 _exptl_crystal_description 'plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6714 _exptl_absorpt_correction_T_max 0.8397 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24156 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8523 _reflns_number_gt 7316 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^+17.9112P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8523 _refine_ls_number_parameters 560 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 C01 C 1.1222(3) 0.9301(2) 0.1238(3) 0.0213(10) Uani 1 1 d . . . C4 C 0.7517(3) 0.9544(3) 0.2636(3) 0.0221(10) Uani 1 1 d . . . C001 C 0.4908(4) 1.3390(4) 0.6735(4) 0.0433(14) Uani 1 1 d . . . H16A H 0.4815 1.2854 0.6892 0.052 Uiso 1 1 calc R . . H17A H 0.4400 1.3619 0.6432 0.052 Uiso 1 1 calc R . . C002 C 0.9885(4) 0.7499(4) 0.9493(4) 0.0467(15) Uani 1 1 d . . . H16B H 1.0224 0.7847 0.9914 0.056 Uiso 1 1 calc R . . H17B H 0.9706 0.7080 0.9796 0.056 Uiso 1 1 calc R . . C3 C 0.7389(3) 1.0264(3) 0.2217(3) 0.0251(10) Uani 1 1 d . . . H3 H 0.6943 1.0558 0.2210 0.030 Uiso 1 1 calc R . . C2 C 0.7916(3) 1.0554(3) 0.1808(3) 0.0308(12) Uani 1 1 d . . . C6 C 0.8707(3) 0.9450(4) 0.2203(3) 0.0394(14) Uani 1 1 d . . . H6 H 0.9159 0.9172 0.2198 0.047 Uiso 1 1 calc R . . C5 C 0.8207(3) 0.9139(3) 0.2611(3) 0.0307(11) Uani 1 1 d . . . H5 H 0.8321 0.8651 0.2879 0.037 Uiso 1 1 calc R . . C11 C 0.9123(4) 1.0427(5) 0.1417(4) 0.067(2) Uani 1 1 d . . . H7A H 0.9305 1.0941 0.1635 0.101 Uiso 1 1 calc R . . H7B H 0.8886 1.0458 0.0809 0.101 Uiso 1 1 calc R . . H7C H 0.9562 1.0068 0.1539 0.101 Uiso 1 1 calc R . . C111 C 0.6353(3) 0.8864(2) 0.1028(3) 0.0167(9) Uani 1 1 d . . . C112 C 0.5956(3) 0.9549(2) 0.0666(3) 0.0181(9) Uani 1 1 d . . . H13D H 0.5535 0.9732 0.0848 0.022 Uiso 1 1 calc R . . C113 C 0.6176(3) 0.9958(3) 0.0043(3) 0.0218(10) Uani 1 1 d . . . H12D H 0.5900 1.0410 -0.0195 0.026 Uiso 1 1 calc R . . C114 C 0.6804(3) 0.9699(3) -0.0229(3) 0.0269(11) Uani 1 1 d . . . H11D H 0.6955 0.9979 -0.0644 0.032 Uiso 1 1 calc R . . C115 C 0.7207(3) 0.9020(3) 0.0122(3) 0.0308(12) Uani 1 1 d . . . H10D H 0.7627 0.8841 -0.0063 0.037 Uiso 1 1 calc R . . C116 C 0.6986(3) 0.8607(3) 0.0746(3) 0.0239(10) Uani 1 1 d . . . H9D H 0.7261 0.8154 0.0981 0.029 Uiso 1 1 calc R . . C121 C 0.5082(2) 0.8418(2) 0.1720(3) 0.0162(9) Uani 1 1 d . . . C122 C 0.4701(3) 0.8927(3) 0.2137(3) 0.0207(10) Uani 1 1 d . . . H9E H 0.4994 0.9289 0.2531 0.025 Uiso 1 1 calc R . . C123 C 0.3883(3) 0.8898(3) 0.1967(3) 0.0276(11) Uani 1 1 d . . . H10E H 0.3631 0.9237 0.2251 0.033 Uiso 1 1 calc R . . C124 C 0.3447(3) 0.8367(3) 0.1379(3) 0.0308(11) Uani 1 1 d . . . H11E H 0.2901 0.8347 0.1267 0.037 Uiso 1 1 calc R . . C125 C 0.3819(3) 0.7866(3) 0.0956(3) 0.0298(11) Uani 1 1 d . . . H12E H 0.3522 0.7508 0.0558 0.036 Uiso 1 1 calc R . . C126 C 0.4630(3) 0.7891(3) 0.1119(3) 0.0228(10) Uani 1 1 d . . . H13E H 0.4877 0.7554 0.0826 0.027 Uiso 1 1 calc R . . C131 C 0.6476(2) 0.7417(2) 0.1994(3) 0.0148(9) Uani 1 1 d . . . C132 C 0.6337(3) 0.6972(3) 0.1243(3) 0.0185(9) Uani 1 1 d . . . H9F H 0.6088 0.7203 0.0717 0.022 Uiso 1 1 calc R . . C133 C 0.6568(3) 0.6190(3) 0.1282(3) 0.0221(10) Uani 1 1 d . . . H10F H 0.6473 0.5895 0.0783 0.027 Uiso 1 1 calc R . . C134 C 0.6941(3) 0.5847(3) 0.2065(3) 0.0234(10) Uani 1 1 d . . . H11F H 0.7093 0.5320 0.2089 0.028 Uiso 1 1 calc R . . C135 C 0.7086(3) 0.6278(3) 0.2804(3) 0.0246(10) Uani 1 1 d . . . H12F H 0.7340 0.6043 0.3326 0.029 Uiso 1 1 calc R . . C136 C 0.6853(3) 0.7068(2) 0.2777(3) 0.0174(9) Uani 1 1 d . . . H13F H 0.6950 0.7358 0.3280 0.021 Uiso 1 1 calc R . . C211 C 0.8202(3) 1.0507(3) 0.4280(3) 0.0202(9) Uani 1 1 d . . . C212 C 0.7931(3) 1.1257(3) 0.3967(3) 0.0238(10) Uani 1 1 d . . . H9A H 0.7425 1.1416 0.3960 0.029 Uiso 1 1 calc R . . C213 C 0.8403(3) 1.1760(3) 0.3671(3) 0.0342(12) Uani 1 1 d . . . H10A H 0.8219 1.2258 0.3471 0.041 Uiso 1 1 calc R . . C214 C 0.9147(3) 1.1525(3) 0.3671(3) 0.0367(13) Uani 1 1 d . . . H11A H 0.9461 1.1860 0.3457 0.044 Uiso 1 1 calc R . . C215 C 0.9431(3) 1.0787(4) 0.3990(3) 0.0372(13) Uani 1 1 d . . . H12A H 0.9939 1.0634 0.4003 0.045 Uiso 1 1 calc R . . C216 C 0.8951(3) 1.0277(3) 0.4292(3) 0.0277(11) Uani 1 1 d . . . H13A H 0.9139 0.9782 0.4502 0.033 Uiso 1 1 calc R . . C221 C 0.6898(2) 1.0416(2) 0.4963(3) 0.0148(9) Uani 1 1 d . . . C222 C 0.6077(2) 1.0375(2) 0.4674(3) 0.0173(9) Uani 1 1 d . . . H13B H 0.5831 1.0044 0.4220 0.021 Uiso 1 1 calc R . . C223 C 0.5623(3) 1.0828(3) 0.5063(3) 0.0216(10) Uani 1 1 d . . . H12B H 0.5074 1.0798 0.4869 0.026 Uiso 1 1 calc R . . C224 C 0.5981(3) 1.1322(3) 0.5735(3) 0.0234(10) Uani 1 1 d . . . H11B H 0.5676 1.1616 0.6001 0.028 Uiso 1 1 calc R . . C225 C 0.6797(3) 1.1379(3) 0.6010(3) 0.0213(10) Uani 1 1 d . . . H10B H 0.7039 1.1714 0.6461 0.026 Uiso 1 1 calc R . . C226 C 0.7254(3) 1.0942(2) 0.5622(3) 0.0186(9) Uani 1 1 d . . . H9B H 0.7801 1.0997 0.5799 0.022 Uiso 1 1 calc R . . C231 C 0.8061(2) 0.9126(2) 0.5284(3) 0.0141(8) Uani 1 1 d . . . C232 C 0.8124(3) 0.8332(3) 0.5069(3) 0.0207(9) Uani 1 1 d . . . H13C H 0.7883 0.8160 0.4514 0.025 Uiso 1 1 calc R . . C233 C 0.8542(3) 0.7805(3) 0.5678(3) 0.0231(10) Uani 1 1 d . . . H12C H 0.8594 0.7283 0.5523 0.028 Uiso 1 1 calc R . . C234 C 0.8884(3) 0.8041(3) 0.6514(3) 0.0213(10) Uani 1 1 d . . . H11C H 0.9145 0.7678 0.6926 0.026 Uiso 1 1 calc R . . C235 C 0.8832(3) 0.8824(3) 0.6727(3) 0.0235(10) Uani 1 1 d . . . H10C H 0.9070 0.8991 0.7285 0.028 Uiso 1 1 calc R . . C236 C 0.8431(3) 0.9362(3) 0.6121(3) 0.0194(9) Uani 1 1 d . . . H9C H 0.8409 0.9889 0.6274 0.023 Uiso 1 1 calc R . . N1 N 0.8560(3) 1.0154(3) 0.1807(3) 0.0395(11) Uani 1 1 d . . . O1 O 1.1455(3) 0.8303(2) 0.2441(2) 0.0460(10) Uani 1 1 d . . . O2 O 1.0663(2) 0.9444(2) 0.2480(2) 0.0414(9) Uani 1 1 d . . . O3 O 1.0144(2) 0.8407(2) 0.1480(2) 0.0421(10) Uani 1 1 d . . . F1 F 1.1888(2) 0.9671(2) 0.1571(3) 0.0657(11) Uani 1 1 d . . . F2 F 1.13730(19) 0.87617(19) 0.0661(2) 0.0408(7) Uani 1 1 d . . . F3 F 1.0700(2) 0.9802(2) 0.0732(3) 0.0615(11) Uani 1 1 d . . . P1 P 0.61591(6) 0.84393(6) 0.19716(6) 0.0134(2) Uani 1 1 d . . . P2 P 0.74944(6) 0.98011(6) 0.44689(6) 0.0129(2) Uani 1 1 d . . . S1 S 1.08306(8) 0.88043(8) 0.19892(8) 0.0310(3) Uani 1 1 d . . . Pd1 Pd 0.679919(18) 0.909942(18) 0.324114(19) 0.01176(10) Uani 1 1 d . . . Cl01 Cl 0.55096(10) 1.33674(8) 0.60575(10) 0.0452(4) Uani 1 1 d . . . Cl1 Cl 0.60385(6) 0.84237(6) 0.40059(6) 0.0173(2) Uani 1 1 d . . . Cl02 Cl 0.53336(12) 1.39416(9) 0.76710(10) 0.0573(5) Uani 1 1 d . . . Cl03 Cl 0.90565(12) 0.80371(11) 0.88684(11) 0.0662(5) Uani 1 1 d . . . Cl04 Cl 1.04060(17) 0.7106(2) 0.88787(14) 0.1364(14) Uani 1 1 d . . . Cl21 Cl 0.77496(9) 1.14488(9) 0.12994(10) 0.0455(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C01 0.014(2) 0.012(2) 0.039(3) 0.0019(19) 0.011(2) -0.0053(17) C4 0.023(2) 0.031(3) 0.012(2) -0.0026(19) 0.0037(18) -0.005(2) C001 0.056(4) 0.043(3) 0.037(3) -0.014(3) 0.023(3) -0.014(3) C002 0.053(4) 0.056(4) 0.029(3) 0.001(3) 0.009(3) 0.000(3) C3 0.026(3) 0.029(3) 0.021(2) -0.003(2) 0.009(2) -0.003(2) C2 0.033(3) 0.044(3) 0.017(2) 0.001(2) 0.011(2) -0.009(2) C6 0.031(3) 0.059(4) 0.031(3) 0.011(3) 0.013(2) 0.016(3) C5 0.030(3) 0.038(3) 0.026(3) 0.004(2) 0.012(2) 0.007(2) C11 0.029(3) 0.125(7) 0.056(4) 0.006(4) 0.024(3) 0.030(4) C111 0.019(2) 0.018(2) 0.014(2) -0.0019(17) 0.0053(17) 0.0006(17) C112 0.017(2) 0.018(2) 0.019(2) -0.0012(18) 0.0038(18) 0.0030(18) C113 0.025(2) 0.022(2) 0.016(2) 0.0062(18) 0.0025(18) 0.0046(19) C114 0.035(3) 0.032(3) 0.017(2) 0.007(2) 0.014(2) 0.008(2) C115 0.035(3) 0.039(3) 0.025(3) 0.009(2) 0.020(2) 0.018(2) C116 0.031(3) 0.026(2) 0.016(2) 0.0069(19) 0.009(2) 0.013(2) C121 0.019(2) 0.015(2) 0.014(2) 0.0050(17) 0.0049(17) 0.0038(18) C122 0.025(2) 0.024(2) 0.012(2) -0.0016(18) 0.0043(18) 0.0072(19) C123 0.026(3) 0.038(3) 0.021(2) 0.006(2) 0.010(2) 0.017(2) C124 0.023(3) 0.035(3) 0.034(3) 0.012(2) 0.008(2) 0.004(2) C125 0.022(3) 0.025(3) 0.037(3) -0.005(2) 0.001(2) -0.005(2) C126 0.023(2) 0.017(2) 0.028(3) -0.0042(19) 0.006(2) 0.0035(19) C131 0.017(2) 0.012(2) 0.017(2) -0.0005(16) 0.0061(17) 0.0013(17) C132 0.018(2) 0.022(2) 0.013(2) -0.0013(17) 0.0020(17) 0.0040(18) C133 0.022(2) 0.025(2) 0.020(2) -0.0090(19) 0.0079(19) -0.0018(19) C134 0.029(3) 0.013(2) 0.032(3) -0.0008(19) 0.015(2) 0.0026(19) C135 0.030(3) 0.024(2) 0.020(2) 0.0065(19) 0.006(2) 0.007(2) C136 0.024(2) 0.016(2) 0.013(2) -0.0020(17) 0.0073(18) 0.0012(18) C211 0.019(2) 0.026(2) 0.016(2) -0.0013(18) 0.0056(18) -0.0089(19) C212 0.031(3) 0.019(2) 0.023(2) -0.0036(19) 0.011(2) -0.006(2) C213 0.047(3) 0.029(3) 0.032(3) -0.002(2) 0.019(3) -0.009(2) C214 0.040(3) 0.040(3) 0.031(3) 0.003(2) 0.012(2) -0.021(3) C215 0.019(3) 0.059(4) 0.032(3) 0.007(3) 0.006(2) -0.004(2) C216 0.023(2) 0.038(3) 0.020(2) 0.009(2) 0.004(2) -0.004(2) C221 0.021(2) 0.012(2) 0.014(2) 0.0039(16) 0.0093(17) 0.0008(17) C222 0.019(2) 0.012(2) 0.020(2) 0.0034(17) 0.0047(18) 0.0018(17) C223 0.016(2) 0.019(2) 0.030(3) 0.0068(19) 0.0080(19) 0.0038(18) C224 0.028(3) 0.017(2) 0.030(3) 0.003(2) 0.016(2) 0.008(2) C225 0.030(3) 0.015(2) 0.018(2) 0.0007(18) 0.0056(19) 0.0062(19) C226 0.022(2) 0.015(2) 0.018(2) 0.0001(18) 0.0041(18) 0.0011(18) C231 0.013(2) 0.016(2) 0.015(2) 0.0014(17) 0.0064(16) -0.0010(17) C232 0.021(2) 0.022(2) 0.018(2) -0.0058(18) 0.0041(18) 0.0000(19) C233 0.024(2) 0.014(2) 0.031(3) 0.0001(19) 0.008(2) 0.0029(19) C234 0.022(2) 0.023(2) 0.020(2) 0.0057(19) 0.0067(19) 0.0039(19) C235 0.025(2) 0.028(2) 0.015(2) 0.0004(19) 0.0028(19) -0.001(2) C236 0.025(2) 0.015(2) 0.017(2) -0.0015(17) 0.0042(18) -0.0006(18) N1 0.035(3) 0.054(3) 0.032(2) 0.015(2) 0.013(2) 0.004(2) O1 0.060(3) 0.042(2) 0.029(2) -0.0024(18) 0.0016(19) 0.016(2) O2 0.037(2) 0.045(2) 0.043(2) -0.0209(19) 0.0113(18) -0.0012(18) O3 0.039(2) 0.041(2) 0.044(2) -0.0087(18) 0.0081(18) -0.0211(18) F1 0.052(2) 0.061(2) 0.094(3) -0.026(2) 0.035(2) -0.031(2) F2 0.0425(18) 0.0458(18) 0.0358(17) -0.0002(15) 0.0143(14) 0.0048(15) F3 0.068(3) 0.051(2) 0.074(3) 0.029(2) 0.033(2) 0.0200(19) P1 0.0165(5) 0.0144(5) 0.0092(5) -0.0001(4) 0.0037(4) 0.0030(4) P2 0.0138(5) 0.0144(5) 0.0109(5) 0.0001(4) 0.0042(4) -0.0013(4) S1 0.0330(7) 0.0299(6) 0.0275(7) -0.0064(5) 0.0050(5) -0.0046(5) Pd1 0.01348(16) 0.01350(16) 0.00874(16) -0.00081(12) 0.00392(12) 0.00075(13) Cl01 0.0728(10) 0.0271(7) 0.0498(8) -0.0033(6) 0.0400(8) -0.0043(7) Cl1 0.0226(5) 0.0179(5) 0.0127(5) -0.0019(4) 0.0073(4) -0.0052(4) Cl02 0.0962(13) 0.0383(8) 0.0392(8) -0.0146(7) 0.0225(9) -0.0062(8) Cl03 0.0918(14) 0.0689(11) 0.0422(9) 0.0299(8) 0.0264(9) 0.0243(10) Cl04 0.122(2) 0.243(4) 0.0466(12) 0.0052(17) 0.0284(13) 0.103(2) Cl21 0.0446(8) 0.0465(8) 0.0486(8) 0.0183(7) 0.0188(7) -0.0017(7) _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 C01 F1 1.305(5) . ? C01 F3 1.345(6) . ? C01 F2 1.392(5) . ? C01 S1 1.786(5) . ? C4 C3 1.384(7) . ? C4 C5 1.409(7) . ? C4 Pd1 1.972(4) . ? C001 Cl01 1.746(6) . ? C001 Cl02 1.763(6) . ? C001 H16A 0.9700 . ? C001 H17A 0.9700 . ? C002 Cl04 1.684(6) . ? C002 Cl03 1.774(6) . ? C002 H16B 0.9700 . ? C002 H17B 0.9700 . ? C3 C2 1.385(7) . ? C3 H3 0.9300 . ? C2 N1 1.326(7) . ? C2 Cl21 1.712(6) . ? C6 N1 1.345(7) . ? C6 C5 1.360(7) . ? C6 H6 0.9300 . ? C5 H5 0.9300 . ? C11 N1 1.407(8) . ? C11 H7A 0.9600 . ? C11 H7B 0.9600 . ? C11 H7C 0.9600 . ? C111 C112 1.396(6) . ? C111 C116 1.396(6) . ? C111 P1 1.823(4) . ? C112 C113 1.376(6) . ? C112 H13D 0.9300 . ? C113 C114 1.382(6) . ? C113 H12D 0.9300 . ? C114 C115 1.386(7) . ? C114 H11D 0.9300 . ? C115 C116 1.384(6) . ? C115 H10D 0.9300 . ? C116 H9D 0.9300 . ? C121 C122 1.388(6) . ? C121 C126 1.394(6) . ? C121 P1 1.828(4) . ? C122 C123 1.392(7) . ? C122 H9E 0.9300 . ? C123 C124 1.376(7) . ? C123 H10E 0.9300 . ? C124 C125 1.377(7) . ? C124 H11E 0.9300 . ? C125 C126 1.381(7) . ? C125 H12E 0.9300 . ? C126 H13E 0.9300 . ? C131 C136 1.392(6) . ? C131 C132 1.399(6) . ? C131 P1 1.817(4) . ? C132 C133 1.381(6) . ? C132 H9F 0.9300 . ? C133 C134 1.385(7) . ? C133 H10F 0.9300 . ? C134 C135 1.369(7) . ? C134 H11F 0.9300 . ? C135 C136 1.397(6) . ? C135 H12F 0.9300 . ? C136 H13F 0.9300 . ? C211 C216 1.374(7) . ? C211 C212 1.401(7) . ? C211 P2 1.821(4) . ? C212 C213 1.376(7) . ? C212 H9A 0.9300 . ? C213 C214 1.375(8) . ? C213 H10A 0.9300 . ? C214 C215 1.390(8) . ? C214 H11A 0.9300 . ? C215 C216 1.398(7) . ? C215 H12A 0.9300 . ? C216 H13A 0.9300 . ? C221 C222 1.392(6) . ? C221 C226 1.397(6) . ? C221 P2 1.829(4) . ? C222 C223 1.392(6) . ? C222 H13B 0.9300 . ? C223 C224 1.378(7) . ? C223 H12B 0.9300 . ? C224 C225 1.383(7) . ? C224 H11B 0.9300 . ? C225 C226 1.380(6) . ? C225 H10B 0.9300 . ? C226 H9B 0.9300 . ? C231 C236 1.392(6) . ? C231 C232 1.403(6) . ? C231 P2 1.818(4) . ? C232 C233 1.380(6) . ? C232 H13C 0.9300 . ? C233 C234 1.382(7) . ? C233 H12C 0.9300 . ? C234 C235 1.382(6) . ? C234 H11C 0.9300 . ? C235 C236 1.379(6) . ? C235 H10C 0.9300 . ? C236 H9C 0.9300 . ? O1 S1 1.418(4) . ? O2 S1 1.430(4) . ? O3 S1 1.424(4) . ? P1 Pd1 2.3378(11) . ? P2 Pd1 2.3473(11) . ? Pd1 Cl1 2.3791(10) . ? 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 F1 C01 F3 109.1(4) . . ? F1 C01 F2 105.6(4) . . ? F3 C01 F2 103.3(4) . . ? F1 C01 S1 115.1(4) . . ? F3 C01 S1 112.7(3) . . ? F2 C01 S1 110.2(3) . . ? C3 C4 C5 115.6(4) . . ? C3 C4 Pd1 123.3(4) . . ? C5 C4 Pd1 121.1(4) . . ? Cl01 C001 Cl02 112.1(3) . . ? Cl01 C001 H16A 109.2 . . ? Cl02 C001 H16A 109.2 . . ? Cl01 C001 H17A 109.2 . . ? Cl02 C001 H17A 109.2 . . ? H16A C001 H17A 107.9 . . ? Cl04 C002 Cl03 111.3(3) . . ? Cl04 C002 H16B 109.4 . . ? Cl03 C002 H16B 109.4 . . ? Cl04 C002 H17B 109.4 . . ? Cl03 C002 H17B 109.4 . . ? H16B C002 H17B 108.0 . . ? C4 C3 C2 121.0(5) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? N1 C2 C3 121.2(5) . . ? N1 C2 Cl21 118.6(4) . . ? C3 C2 Cl21 120.2(4) . . ? N1 C6 C5 121.1(5) . . ? N1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C5 C4 121.2(5) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? N1 C11 H7A 109.5 . . ? N1 C11 H7B 109.5 . . ? H7A C11 H7B 109.5 . . ? N1 C11 H7C 109.5 . . ? H7A C11 H7C 109.5 . . ? H7B C11 H7C 109.5 . . ? C112 C111 C116 118.2(4) . . ? C112 C111 P1 119.4(3) . . ? C116 C111 P1 121.5(3) . . ? C113 C112 C111 121.0(4) . . ? C113 C112 H13D 119.5 . . ? C111 C112 H13D 119.5 . . ? C112 C113 C114 120.3(4) . . ? C112 C113 H12D 119.8 . . ? C114 C113 H12D 119.8 . . ? C113 C114 C115 119.7(4) . . ? C113 C114 H11D 120.2 . . ? C115 C114 H11D 120.2 . . ? C116 C115 C114 120.1(4) . . ? C116 C115 H10D 120.0 . . ? C114 C115 H10D 120.0 . . ? C115 C116 C111 120.8(4) . . ? C115 C116 H9D 119.6 . . ? C111 C116 H9D 119.6 . . ? C122 C121 C126 118.9(4) . . ? C122 C121 P1 120.0(3) . . ? C126 C121 P1 121.1(3) . . ? C121 C122 C123 120.3(4) . . ? C121 C122 H9E 119.8 . . ? C123 C122 H9E 119.8 . . ? C124 C123 C122 120.0(4) . . ? C124 C123 H10E 120.0 . . ? C122 C123 H10E 120.0 . . ? C123 C124 C125 120.1(5) . . ? C123 C124 H11E 119.9 . . ? C125 C124 H11E 119.9 . . ? C124 C125 C126 120.4(5) . . ? C124 C125 H12E 119.8 . . ? C126 C125 H12E 119.8 . . ? C125 C126 C121 120.3(4) . . ? C125 C126 H13E 119.9 . . ? C121 C126 H13E 119.9 . . ? C136 C131 C132 119.5(4) . . ? C136 C131 P1 119.0(3) . . ? C132 C131 P1 121.5(3) . . ? C133 C132 C131 120.1(4) . . ? C133 C132 H9F 119.9 . . ? C131 C132 H9F 119.9 . . ? C132 C133 C134 120.0(4) . . ? C132 C133 H10F 120.0 . . ? C134 C133 H10F 120.0 . . ? C135 C134 C133 120.4(4) . . ? C135 C134 H11F 119.8 . . ? C133 C134 H11F 119.8 . . ? C134 C135 C136 120.4(4) . . ? C134 C135 H12F 119.8 . . ? C136 C135 H12F 119.8 . . ? C131 C136 C135 119.5(4) . . ? C131 C136 H13F 120.2 . . ? C135 C136 H13F 120.2 . . ? C216 C211 C212 119.2(4) . . ? C216 C211 P2 121.2(4) . . ? C212 C211 P2 118.5(3) . . ? C213 C212 C211 120.7(5) . . ? C213 C212 H9A 119.6 . . ? C211 C212 H9A 119.6 . . ? C214 C213 C212 120.0(5) . . ? C214 C213 H10A 120.0 . . ? C212 C213 H10A 120.0 . . ? C213 C214 C215 120.0(5) . . ? C213 C214 H11A 120.0 . . ? C215 C214 H11A 120.0 . . ? C214 C215 C216 120.0(5) . . ? C214 C215 H12A 120.0 . . ? C216 C215 H12A 120.0 . . ? C211 C216 C215 120.0(5) . . ? C211 C216 H13A 120.0 . . ? C215 C216 H13A 120.0 . . ? C222 C221 C226 119.0(4) . . ? C222 C221 P2 120.0(3) . . ? C226 C221 P2 121.0(3) . . ? C221 C222 C223 120.1(4) . . ? C221 C222 H13B 120.0 . . ? C223 C222 H13B 120.0 . . ? C224 C223 C222 120.4(4) . . ? C224 C223 H12B 119.8 . . ? C222 C223 H12B 119.8 . . ? C223 C224 C225 119.7(4) . . ? C223 C224 H11B 120.2 . . ? C225 C224 H11B 120.2 . . ? C226 C225 C224 120.6(4) . . ? C226 C225 H10B 119.7 . . ? C224 C225 H10B 119.7 . . ? C225 C226 C221 120.2(4) . . ? C225 C226 H9B 119.9 . . ? C221 C226 H9B 119.9 . . ? C236 C231 C232 118.2(4) . . ? C236 C231 P2 122.7(3) . . ? C232 C231 P2 119.1(3) . . ? C233 C232 C231 120.4(4) . . ? C233 C232 H13C 119.8 . . ? C231 C232 H13C 119.8 . . ? C232 C233 C234 120.9(4) . . ? C232 C233 H12C 119.6 . . ? C234 C233 H12C 119.6 . . ? C233 C234 C235 119.0(4) . . ? C233 C234 H11C 120.5 . . ? C235 C234 H11C 120.5 . . ? C236 C235 C234 120.7(4) . . ? C236 C235 H10C 119.6 . . ? C234 C235 H10C 119.6 . . ? C235 C236 C231 120.8(4) . . ? C235 C236 H9C 119.6 . . ? C231 C236 H9C 119.6 . . ? C2 N1 C6 119.9(5) . . ? C2 N1 C11 123.6(5) . . ? C6 N1 C11 116.5(5) . . ? C131 P1 C111 105.04(19) . . ? C131 P1 C121 106.32(19) . . ? C111 P1 C121 104.99(19) . . ? C131 P1 Pd1 111.80(14) . . ? C111 P1 Pd1 113.58(14) . . ? C121 P1 Pd1 114.34(14) . . ? C231 P2 C211 106.1(2) . . ? C231 P2 C221 107.45(18) . . ? C211 P2 C221 102.4(2) . . ? C231 P2 Pd1 110.33(14) . . ? C211 P2 Pd1 113.68(14) . . ? C221 P2 Pd1 116.12(14) . . ? O1 S1 O3 115.1(3) . . ? O1 S1 O2 114.7(2) . . ? O3 S1 O2 113.9(2) . . ? O1 S1 C01 103.9(2) . . ? O3 S1 C01 104.8(2) . . ? O2 S1 C01 102.4(2) . . ? C4 Pd1 P1 87.35(13) . . ? C4 Pd1 P2 88.96(13) . . ? P1 Pd1 P2 176.30(4) . . ? C4 Pd1 Cl1 172.88(14) . . ? P1 Pd1 Cl1 91.98(4) . . ? P2 Pd1 Cl1 91.71(4) . . ? 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 C5 C4 C3 C2 -0.2(7) . . . . ? Pd1 C4 C3 C2 179.4(4) . . . . ? C4 C3 C2 N1 -0.2(7) . . . . ? C4 C3 C2 Cl21 -179.6(4) . . . . ? N1 C6 C5 C4 -0.2(8) . . . . ? C3 C4 C5 C6 0.4(7) . . . . ? Pd1 C4 C5 C6 -179.2(4) . . . . ? C116 C111 C112 C113 0.5(6) . . . . ? P1 C111 C112 C113 169.4(3) . . . . ? C111 C112 C113 C114 -0.7(7) . . . . ? C112 C113 C114 C115 0.7(7) . . . . ? C113 C114 C115 C116 -0.6(8) . . . . ? C114 C115 C116 C111 0.4(8) . . . . ? C112 C111 C116 C115 -0.4(7) . . . . ? P1 C111 C116 C115 -169.1(4) . . . . ? C126 C121 C122 C123 1.3(6) . . . . ? P1 C121 C122 C123 -178.1(3) . . . . ? C121 C122 C123 C124 -0.5(7) . . . . ? C122 C123 C124 C125 -0.2(7) . . . . ? C123 C124 C125 C126 0.1(8) . . . . ? C124 C125 C126 C121 0.7(7) . . . . ? C122 C121 C126 C125 -1.4(7) . . . . ? P1 C121 C126 C125 178.0(4) . . . . ? C136 C131 C132 C133 0.4(6) . . . . ? P1 C131 C132 C133 -178.4(3) . . . . ? C131 C132 C133 C134 -0.2(7) . . . . ? C132 C133 C134 C135 -0.2(7) . . . . ? C133 C134 C135 C136 0.5(7) . . . . ? C132 C131 C136 C135 -0.1(6) . . . . ? P1 C131 C136 C135 178.7(3) . . . . ? C134 C135 C136 C131 -0.4(7) . . . . ? C216 C211 C212 C213 0.4(7) . . . . ? P2 C211 C212 C213 -168.4(4) . . . . ? C211 C212 C213 C214 0.7(7) . . . . ? C212 C213 C214 C215 -1.6(8) . . . . ? C213 C214 C215 C216 1.5(8) . . . . ? C212 C211 C216 C215 -0.5(7) . . . . ? P2 C211 C216 C215 168.0(4) . . . . ? C214 C215 C216 C211 -0.5(8) . . . . ? C226 C221 C222 C223 -2.7(6) . . . . ? P2 C221 C222 C223 178.4(3) . . . . ? C221 C222 C223 C224 0.2(6) . . . . ? C222 C223 C224 C225 1.4(7) . . . . ? C223 C224 C225 C226 -0.4(7) . . . . ? C224 C225 C226 C221 -2.2(7) . . . . ? C222 C221 C226 C225 3.7(6) . . . . ? P2 C221 C226 C225 -177.5(3) . . . . ? C236 C231 C232 C233 0.2(6) . . . . ? P2 C231 C232 C233 -179.1(3) . . . . ? C231 C232 C233 C234 2.0(7) . . . . ? C232 C233 C234 C235 -2.8(7) . . . . ? C233 C234 C235 C236 1.3(7) . . . . ? C234 C235 C236 C231 0.9(7) . . . . ? C232 C231 C236 C235 -1.6(6) . . . . ? P2 C231 C236 C235 177.7(3) . . . . ? C3 C2 N1 C6 0.4(8) . . . . ? Cl21 C2 N1 C6 179.9(4) . . . . ? C3 C2 N1 C11 -178.8(6) . . . . ? Cl21 C2 N1 C11 0.7(8) . . . . ? C5 C6 N1 C2 -0.3(8) . . . . ? C5 C6 N1 C11 179.0(6) . . . . ? C136 C131 P1 C111 141.7(3) . . . . ? C132 C131 P1 C111 -39.5(4) . . . . ? C136 C131 P1 C121 -107.3(4) . . . . ? C132 C131 P1 C121 71.5(4) . . . . ? C136 C131 P1 Pd1 18.1(4) . . . . ? C132 C131 P1 Pd1 -163.1(3) . . . . ? C112 C111 P1 C131 159.4(3) . . . . ? C116 C111 P1 C131 -32.1(4) . . . . ? C112 C111 P1 C121 47.5(4) . . . . ? C116 C111 P1 C121 -144.0(4) . . . . ? C112 C111 P1 Pd1 -78.1(4) . . . . ? C116 C111 P1 Pd1 90.4(4) . . . . ? C122 C121 P1 C131 139.6(3) . . . . ? C126 C121 P1 C131 -39.8(4) . . . . ? C122 C121 P1 C111 -109.4(4) . . . . ? C126 C121 P1 C111 71.2(4) . . . . ? C122 C121 P1 Pd1 15.7(4) . . . . ? C126 C121 P1 Pd1 -163.7(3) . . . . ? C236 C231 P2 C211 66.6(4) . . . . ? C232 C231 P2 C211 -114.1(3) . . . . ? C236 C231 P2 C221 -42.4(4) . . . . ? C232 C231 P2 C221 136.9(3) . . . . ? C236 C231 P2 Pd1 -169.8(3) . . . . ? C232 C231 P2 Pd1 9.4(4) . . . . ? C216 C211 P2 C231 37.0(4) . . . . ? C212 C211 P2 C231 -154.4(3) . . . . ? C216 C211 P2 C221 149.6(4) . . . . ? C212 C211 P2 C221 -41.9(4) . . . . ? C216 C211 P2 Pd1 -84.4(4) . . . . ? C212 C211 P2 Pd1 84.1(4) . . . . ? C222 C221 P2 C231 -116.2(3) . . . . ? C226 C221 P2 C231 64.9(4) . . . . ? C222 C221 P2 C211 132.2(3) . . . . ? C226 C221 P2 C211 -46.6(4) . . . . ? C222 C221 P2 Pd1 7.8(4) . . . . ? C226 C221 P2 Pd1 -171.0(3) . . . . ? F1 C01 S1 O1 -55.1(4) . . . . ? F3 C01 S1 O1 179.0(3) . . . . ? F2 C01 S1 O1 64.2(4) . . . . ? F1 C01 S1 O3 -176.2(4) . . . . ? F3 C01 S1 O3 57.9(4) . . . . ? F2 C01 S1 O3 -57.0(4) . . . . ? F1 C01 S1 O2 64.6(4) . . . . ? F3 C01 S1 O2 -61.3(4) . . . . ? F2 C01 S1 O2 -176.1(3) . . . . ? C3 C4 Pd1 P1 92.8(4) . . . . ? C5 C4 Pd1 P1 -87.6(4) . . . . ? C3 C4 Pd1 P2 -87.0(4) . . . . ? C5 C4 Pd1 P2 92.6(4) . . . . ? C3 C4 Pd1 Cl1 177.5(8) . . . . ? C5 C4 Pd1 Cl1 -2.9(13) . . . . ? C131 P1 Pd1 C4 99.4(2) . . . . ? C111 P1 Pd1 C4 -19.3(2) . . . . ? C121 P1 Pd1 C4 -139.8(2) . . . . ? C131 P1 Pd1 P2 102.7(6) . . . . ? C111 P1 Pd1 P2 -16.0(7) . . . . ? C121 P1 Pd1 P2 -136.4(6) . . . . ? C131 P1 Pd1 Cl1 -73.54(15) . . . . ? C111 P1 Pd1 Cl1 167.81(15) . . . . ? C121 P1 Pd1 Cl1 47.33(15) . . . . ? C231 P2 Pd1 C4 -109.69(19) . . . . ? C211 P2 Pd1 C4 9.4(2) . . . . ? C221 P2 Pd1 C4 127.8(2) . . . . ? C231 P2 Pd1 P1 -113.0(6) . . . . ? C211 P2 Pd1 P1 6.0(7) . . . . ? C221 P2 Pd1 P1 124.4(6) . . . . ? C231 P2 Pd1 Cl1 63.22(14) . . . . ? C211 P2 Pd1 Cl1 -177.73(17) . . . . ? C221 P2 Pd1 Cl1 -59.31(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.668 _refine_diff_density_min -1.558 _refine_diff_density_rms 0.108 #===END data_7OTf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H36 Cl2 N Ni P2, C F3 O3 S, C H2 Cl2 ' _chemical_formula_sum 'C44 H38 Cl4 F3 N Ni O3 P2 S' _chemical_formula_weight 980.26 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.5898(7) _cell_length_b 21.8258(14) _cell_length_c 19.7422(13) _cell_angle_alpha 90.00 _cell_angle_beta 104.7130(10) _cell_angle_gamma 90.00 _cell_volume 4413.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9536 _cell_measurement_theta_min 2.196 _cell_measurement_theta_max 26,342 _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7905 _exptl_absorpt_correction_T_max 0.9194 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23126 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8048 _reflns_number_gt 7147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0480P)^2^+3.1369P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8048 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 C001 C 0.9186(3) 0.32532(14) 0.86227(18) 0.0433(8) Uani 1 1 d . . . H77A H 0.9910 0.3546 0.8645 0.052 Uiso 1 1 calc R . . H77B H 0.9461 0.2848 0.8486 0.052 Uiso 1 1 calc R . . Cl01 Cl 0.88553(9) 0.31991(4) 0.94595(4) 0.0497(2) Uani 1 1 d . . . Cl02 Cl 0.77856(7) 0.35023(4) 0.79877(4) 0.04139(18) Uani 1 1 d . . . C4 C 0.4985(2) 0.17559(9) 0.80549(12) 0.0161(5) Uani 1 1 d . . . C01 C 1.1076(2) 0.07882(12) 0.95029(14) 0.0277(6) Uani 1 1 d . . . C3 C 0.4658(2) 0.15892(10) 0.86732(12) 0.0168(5) Uani 1 1 d . . . H002 H 0.3784 0.1484 0.8663 0.020 Uiso 1 1 calc R . . C2 C 0.5605(2) 0.15786(10) 0.92938(12) 0.0198(5) Uani 1 1 d . . . C6 C 0.7211(2) 0.18671(10) 0.87373(13) 0.0212(5) Uani 1 1 d . . . H020 H 0.8099 0.1954 0.8758 0.025 Uiso 1 1 calc R . . C5 C 0.6306(2) 0.18993(10) 0.81122(13) 0.0194(5) Uani 1 1 d . . . H028 H 0.6568 0.2021 0.7706 0.023 Uiso 1 1 calc R . . C11 C 0.7889(3) 0.16885(12) 0.99999(13) 0.0299(6) Uani 1 1 d . . . H03A H 0.8740 0.1784 0.9915 0.045 Uiso 1 1 calc R . . H03B H 0.7914 0.1277 1.0201 0.045 Uiso 1 1 calc R . . H03C H 0.7688 0.1988 1.0327 0.045 Uiso 1 1 calc R . . C111 C 0.3563(2) 0.28969(10) 0.83907(12) 0.0172(5) Uani 1 1 d . . . C112 C 0.2690(2) 0.27228(10) 0.87787(13) 0.0212(5) Uani 1 1 d . . . H011 H 0.1848 0.2574 0.8546 0.025 Uiso 1 1 calc R . . C113 C 0.3051(2) 0.27666(11) 0.95066(13) 0.0245(5) Uani 1 1 d . . . H029 H 0.2451 0.2648 0.9768 0.029 Uiso 1 1 calc R . . C114 C 0.4273(3) 0.29810(11) 0.98528(13) 0.0257(5) Uani 1 1 d . . . H016 H 0.4515 0.3008 1.0349 0.031 Uiso 1 1 calc R . . C115 C 0.5147(2) 0.31569(10) 0.94684(13) 0.0235(5) Uani 1 1 d . . . H009 H 0.5988 0.3305 0.9703 0.028 Uiso 1 1 calc R . . C116 C 0.4796(2) 0.31172(10) 0.87452(13) 0.0202(5) Uani 1 1 d . . . H010 H 0.5397 0.3241 0.8487 0.024 Uiso 1 1 calc R . . C121 C 0.1452(2) 0.27966(11) 0.71335(12) 0.0204(5) Uani 1 1 d . . . C122 C 0.0710(2) 0.22743(12) 0.71708(14) 0.0262(5) Uani 1 1 d . . . H030 H 0.1136 0.1909 0.7370 0.031 Uiso 1 1 calc R . . C123 C -0.0636(3) 0.22804(13) 0.69218(14) 0.0318(6) Uani 1 1 d . . . H033 H -0.1132 0.1923 0.6950 0.038 Uiso 1 1 calc R . . C124 C -0.1252(3) 0.28152(14) 0.66314(14) 0.0359(7) Uani 1 1 d . . . H036 H -0.2174 0.2821 0.6453 0.043 Uiso 1 1 calc R . . C125 C -0.0538(3) 0.33355(14) 0.66006(15) 0.0357(7) Uani 1 1 d . . . H037 H -0.0972 0.3701 0.6408 0.043 Uiso 1 1 calc R . . C126 C 0.0819(2) 0.33308(12) 0.68502(13) 0.0274(6) Uani 1 1 d . . . H038 H 0.1308 0.3691 0.6826 0.033 Uiso 1 1 calc R . . C131 C 0.4004(2) 0.33436(11) 0.71028(12) 0.0193(5) Uani 1 1 d . . . C132 C 0.4777(2) 0.32043(11) 0.66475(12) 0.0216(5) Uani 1 1 d . . . H001 H 0.4854 0.2792 0.6508 0.026 Uiso 1 1 calc R . . C133 C 0.5433(2) 0.36675(12) 0.63987(13) 0.0270(6) Uani 1 1 d . . . H008 H 0.5958 0.3571 0.6088 0.032 Uiso 1 1 calc R . . C134 C 0.5329(2) 0.42684(12) 0.65984(14) 0.0287(6) Uani 1 1 d . . . H012 H 0.5785 0.4583 0.6427 0.034 Uiso 1 1 calc R . . C135 C 0.4559(3) 0.44116(12) 0.70489(14) 0.0290(6) Uani 1 1 d . . . H043 H 0.4479 0.4826 0.7181 0.035 Uiso 1 1 calc R . . C136 C 0.3908(2) 0.39522(11) 0.73077(13) 0.0242(5) Uani 1 1 d . . . H026 H 0.3395 0.4050 0.7624 0.029 Uiso 1 1 calc R . . C211 C 0.4868(2) 0.03868(10) 0.78336(12) 0.0168(5) Uani 1 1 d . . . C212 C 0.3982(2) 0.01554(10) 0.81856(12) 0.0193(5) Uani 1 1 d . . . H007 H 0.3074 0.0156 0.7963 0.023 Uiso 1 1 calc R . . C213 C 0.4420(2) -0.00738(10) 0.88570(13) 0.0221(5) Uani 1 1 d . . . H022 H 0.3811 -0.0234 0.9091 0.027 Uiso 1 1 calc R . . C214 C 0.5741(2) -0.00725(11) 0.91919(13) 0.0230(5) Uani 1 1 d . . . H013 H 0.6036 -0.0224 0.9656 0.028 Uiso 1 1 calc R . . C215 C 0.6631(2) 0.01529(10) 0.88421(13) 0.0218(5) Uani 1 1 d . . . H014 H 0.7538 0.0151 0.9068 0.026 Uiso 1 1 calc R . . C216 C 0.6203(2) 0.03807(10) 0.81660(12) 0.0187(5) Uani 1 1 d . . . H017 H 0.6816 0.0532 0.7929 0.022 Uiso 1 1 calc R . . C221 C 0.2758(2) 0.03987(10) 0.65904(12) 0.0188(5) Uani 1 1 d . . . C222 C 0.2774(2) -0.01330(12) 0.61995(13) 0.0273(6) Uani 1 1 d . . . H021 H 0.3575 -0.0282 0.6130 0.033 Uiso 1 1 calc R . . C223 C 0.1621(3) -0.04446(12) 0.59118(13) 0.0291(6) Uani 1 1 d . . . H023 H 0.1636 -0.0808 0.5649 0.035 Uiso 1 1 calc R . . C224 C 0.0453(2) -0.02295(12) 0.60054(13) 0.0288(6) Uani 1 1 d . . . H025 H -0.0337 -0.0438 0.5797 0.035 Uiso 1 1 calc R . . C225 C 0.0432(3) 0.02896(12) 0.64022(16) 0.0350(7) Uani 1 1 d . . . H040 H -0.0369 0.0432 0.6478 0.042 Uiso 1 1 calc R . . C226 C 0.1582(2) 0.06037(12) 0.66906(15) 0.0298(6) Uani 1 1 d . . . H031 H 0.1562 0.0963 0.6959 0.036 Uiso 1 1 calc R . . C231 C 0.5416(2) 0.06613(12) 0.65057(12) 0.0234(5) Uani 1 1 d . . . C232 C 0.6038(2) 0.00976(12) 0.65321(14) 0.0286(6) Uani 1 1 d . . . H035 H 0.5906 -0.0207 0.6851 0.034 Uiso 1 1 calc R . . C233 C 0.6849(3) -0.00230(15) 0.60975(15) 0.0366(7) Uani 1 1 d . . . H041 H 0.7261 -0.0411 0.6114 0.044 Uiso 1 1 calc R . . C234 C 0.7058(3) 0.04188(17) 0.56436(15) 0.0453(8) Uani 1 1 d . . . H042 H 0.7605 0.0333 0.5341 0.054 Uiso 1 1 calc R . . C235 C 0.6476(3) 0.09872(18) 0.56235(17) 0.0547(10) Uani 1 1 d . . . H039 H 0.6645 0.1295 0.5318 0.066 Uiso 1 1 calc R . . C236 C 0.5643(3) 0.11088(14) 0.60502(15) 0.0374(7) Uani 1 1 d . . . H032 H 0.5230 0.1497 0.6030 0.045 Uiso 1 1 calc R . . N1 N 0.68719(18) 0.17129(9) 0.93319(10) 0.0208(4) Uani 1 1 d . . . O1 O 1.02374(16) 0.17962(8) 0.88807(10) 0.0295(4) Uani 1 1 d . . . O2 O 0.93347(17) 0.08429(8) 0.83252(10) 0.0320(4) Uani 1 1 d . . . O3 O 1.15664(17) 0.11344(8) 0.83502(9) 0.0300(4) Uani 1 1 d . . . F1 F 1.20314(16) 0.11002(8) 0.99348(8) 0.0412(4) Uani 1 1 d . . . F2 F 1.15308(15) 0.02312(7) 0.94202(8) 0.0334(4) Uani 1 1 d . . . F3 F 1.01186(16) 0.07177(8) 0.98279(9) 0.0416(4) Uani 1 1 d . . . P1 P 0.32189(6) 0.27215(3) 0.74560(3) 0.01665(13) Uani 1 1 d . . . P2 P 0.42429(6) 0.08129(3) 0.70205(3) 0.01671(13) Uani 1 1 d . . . S1 S 1.04826(6) 0.11841(3) 0.86634(3) 0.02219(14) Uani 1 1 d . . . Cl1 Cl 0.27252(6) 0.19134(3) 0.60716(3) 0.02405(14) Uani 1 1 d . . . Cl21 Cl 0.52237(6) 0.13987(3) 1.00631(3) 0.02770(15) Uani 1 1 d . . . Ni1 Ni 0.38257(3) 0.179733(13) 0.717695(15) 0.01624(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C001 0.0297(15) 0.0378(17) 0.061(2) 0.0041(15) 0.0090(15) -0.0025(12) Cl01 0.0618(5) 0.0389(4) 0.0380(4) -0.0037(3) -0.0066(4) -0.0046(3) Cl02 0.0374(4) 0.0551(5) 0.0321(4) -0.0008(3) 0.0097(3) -0.0043(3) C4 0.0190(11) 0.0112(10) 0.0162(11) -0.0013(9) 0.0008(9) 0.0013(8) C01 0.0270(13) 0.0293(14) 0.0274(14) -0.0031(11) 0.0080(11) 0.0003(10) C3 0.0150(11) 0.0144(11) 0.0196(12) 0.0000(9) 0.0020(9) 0.0031(8) C2 0.0242(12) 0.0145(11) 0.0211(12) 0.0015(9) 0.0068(10) 0.0031(9) C6 0.0172(11) 0.0189(12) 0.0272(13) -0.0043(10) 0.0055(10) 0.0000(9) C5 0.0192(11) 0.0166(11) 0.0227(12) -0.0014(9) 0.0056(10) -0.0010(9) C11 0.0269(13) 0.0320(14) 0.0237(13) -0.0034(11) -0.0069(11) 0.0034(11) C111 0.0195(11) 0.0151(11) 0.0161(11) 0.0024(9) 0.0026(9) 0.0043(9) C112 0.0217(12) 0.0178(12) 0.0244(13) 0.0013(10) 0.0065(10) 0.0024(9) C113 0.0313(14) 0.0221(13) 0.0232(13) 0.0034(10) 0.0123(11) 0.0033(10) C114 0.0361(14) 0.0234(13) 0.0160(12) 0.0014(10) 0.0034(11) 0.0058(11) C115 0.0251(13) 0.0185(12) 0.0229(13) -0.0001(10) -0.0010(10) 0.0029(9) C116 0.0236(12) 0.0153(11) 0.0225(12) 0.0025(9) 0.0071(10) 0.0015(9) C121 0.0201(12) 0.0244(12) 0.0155(11) 0.0013(9) 0.0022(9) 0.0026(9) C122 0.0233(13) 0.0253(13) 0.0295(14) -0.0015(11) 0.0059(11) 0.0017(10) C123 0.0241(13) 0.0383(16) 0.0335(15) -0.0058(12) 0.0079(12) -0.0024(11) C124 0.0191(13) 0.0570(19) 0.0303(15) 0.0028(13) 0.0041(11) 0.0045(12) C125 0.0297(14) 0.0441(17) 0.0341(16) 0.0163(13) 0.0098(12) 0.0162(12) C126 0.0260(13) 0.0304(14) 0.0266(14) 0.0091(11) 0.0083(11) 0.0065(11) C131 0.0208(12) 0.0210(12) 0.0148(11) 0.0047(9) 0.0019(9) -0.0008(9) C132 0.0214(12) 0.0217(12) 0.0201(12) 0.0038(10) 0.0023(10) 0.0024(9) C133 0.0236(13) 0.0350(15) 0.0238(13) 0.0080(11) 0.0084(11) 0.0043(10) C134 0.0274(13) 0.0291(14) 0.0292(14) 0.0127(11) 0.0063(11) -0.0031(11) C135 0.0362(15) 0.0200(13) 0.0306(14) 0.0026(11) 0.0078(12) -0.0013(11) C136 0.0302(13) 0.0224(13) 0.0216(12) 0.0021(10) 0.0095(11) 0.0010(10) C211 0.0184(11) 0.0133(11) 0.0185(11) -0.0013(9) 0.0046(9) 0.0012(8) C212 0.0193(11) 0.0157(11) 0.0231(12) -0.0038(9) 0.0055(10) -0.0012(9) C213 0.0264(13) 0.0172(12) 0.0247(13) 0.0021(10) 0.0102(10) -0.0004(9) C214 0.0301(13) 0.0173(12) 0.0212(13) 0.0023(10) 0.0055(10) 0.0036(10) C215 0.0191(11) 0.0189(12) 0.0250(13) -0.0013(10) 0.0007(10) 0.0048(9) C216 0.0186(11) 0.0146(11) 0.0233(12) -0.0021(9) 0.0063(10) 0.0008(9) C221 0.0211(12) 0.0184(12) 0.0155(11) 0.0003(9) 0.0019(9) -0.0035(9) C222 0.0275(13) 0.0291(14) 0.0280(14) -0.0054(11) 0.0121(11) -0.0044(10) C223 0.0373(15) 0.0271(14) 0.0253(14) -0.0099(11) 0.0121(12) -0.0117(11) C224 0.0244(13) 0.0290(14) 0.0280(14) 0.0016(11) -0.0025(11) -0.0081(10) C225 0.0217(13) 0.0304(15) 0.0502(18) -0.0031(13) 0.0037(12) 0.0016(11) C226 0.0234(13) 0.0253(13) 0.0394(16) -0.0077(12) 0.0052(12) -0.0011(10) C231 0.0158(11) 0.0382(15) 0.0165(12) -0.0030(10) 0.0046(9) -0.0056(10) C232 0.0257(13) 0.0336(15) 0.0289(14) -0.0054(11) 0.0116(11) -0.0025(11) C233 0.0259(14) 0.0527(18) 0.0330(16) -0.0067(14) 0.0104(12) 0.0042(12) C234 0.0254(15) 0.086(2) 0.0273(15) 0.0095(16) 0.0107(12) 0.0163(15) C235 0.0363(17) 0.091(3) 0.0434(19) 0.0394(19) 0.0231(15) 0.0206(17) C236 0.0269(14) 0.0519(18) 0.0349(16) 0.0190(14) 0.0104(12) 0.0090(12) N1 0.0189(10) 0.0197(10) 0.0204(11) -0.0031(8) -0.0015(8) 0.0017(8) O1 0.0222(9) 0.0223(9) 0.0461(12) -0.0006(8) 0.0123(8) 0.0005(7) O2 0.0221(9) 0.0314(10) 0.0383(11) -0.0020(8) -0.0002(8) -0.0018(7) O3 0.0246(9) 0.0356(10) 0.0327(10) 0.0051(8) 0.0125(8) 0.0049(7) F1 0.0393(9) 0.0421(10) 0.0350(9) -0.0084(7) -0.0035(7) -0.0023(7) F2 0.0377(8) 0.0276(8) 0.0336(9) 0.0022(7) 0.0069(7) 0.0075(6) F3 0.0468(10) 0.0469(10) 0.0395(10) 0.0033(8) 0.0266(8) 0.0018(8) P1 0.0177(3) 0.0161(3) 0.0154(3) 0.0028(2) 0.0028(2) 0.0009(2) P2 0.0170(3) 0.0174(3) 0.0155(3) -0.0005(2) 0.0037(2) -0.0013(2) S1 0.0165(3) 0.0222(3) 0.0284(3) 0.0005(2) 0.0066(2) 0.0008(2) Cl1 0.0278(3) 0.0257(3) 0.0151(3) 0.0015(2) -0.0011(2) 0.0024(2) Cl21 0.0360(3) 0.0292(3) 0.0181(3) 0.0054(2) 0.0073(3) 0.0032(3) Ni1 0.01749(16) 0.01605(16) 0.01370(16) 0.00135(11) 0.00123(12) -0.00015(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C001 Cl02 1.767(3) . ? C001 Cl01 1.777(3) . ? C001 H77A 0.9900 . ? C001 H77B 0.9900 . ? C4 C3 1.399(3) . ? C4 C5 1.409(3) . ? C4 Ni1 1.855(2) . ? C01 F1 1.333(3) . ? C01 F2 1.333(3) . ? C01 F3 1.339(3) . ? C01 S1 1.833(3) . ? C3 C2 1.372(3) . ? C3 H002 0.9500 . ? C2 N1 1.356(3) . ? C2 Cl21 1.713(2) . ? C6 N1 1.355(3) . ? C6 C5 1.359(3) . ? C6 H020 0.9500 . ? C5 H028 0.9500 . ? C11 N1 1.477(3) . ? C11 H03A 0.9800 . ? C11 H03B 0.9800 . ? C11 H03C 0.9800 . ? C111 C112 1.395(3) . ? C111 C116 1.401(3) . ? C111 P1 1.829(2) . ? C112 C113 1.393(3) . ? C112 H011 0.9500 . ? C113 C114 1.383(4) . ? C113 H029 0.9500 . ? C114 C115 1.391(4) . ? C114 H016 0.9500 . ? C115 C116 1.384(3) . ? C115 H009 0.9500 . ? C116 H010 0.9500 . ? C121 C126 1.389(3) . ? C121 C122 1.397(3) . ? C121 P1 1.825(2) . ? C122 C123 1.386(4) . ? C122 H030 0.9500 . ? C123 C124 1.388(4) . ? C123 H033 0.9500 . ? C124 C125 1.374(4) . ? C124 H036 0.9500 . ? C125 C126 1.396(4) . ? C125 H037 0.9500 . ? C126 H038 0.9500 . ? C131 C132 1.395(3) . ? C131 C136 1.400(3) . ? C131 P1 1.821(2) . ? C132 C133 1.385(3) . ? C132 H001 0.9500 . ? C133 C134 1.382(4) . ? C133 H008 0.9500 . ? C134 C135 1.386(4) . ? C134 H012 0.9500 . ? C135 C136 1.387(4) . ? C135 H043 0.9500 . ? C136 H026 0.9500 . ? C211 C212 1.397(3) . ? C211 C216 1.399(3) . ? C211 P2 1.828(2) . ? C212 C213 1.382(3) . ? C212 H007 0.9500 . ? C213 C214 1.387(3) . ? C213 H022 0.9500 . ? C214 C215 1.392(3) . ? C214 H013 0.9500 . ? C215 C216 1.388(3) . ? C215 H014 0.9500 . ? C216 H017 0.9500 . ? C221 C226 1.384(3) . ? C221 C222 1.396(3) . ? C221 P2 1.825(2) . ? C222 C223 1.387(3) . ? C222 H021 0.9500 . ? C223 C224 1.378(4) . ? C223 H023 0.9500 . ? C224 C225 1.381(4) . ? C224 H025 0.9500 . ? C225 C226 1.387(4) . ? C225 H040 0.9500 . ? C226 H031 0.9500 . ? C231 C236 1.389(4) . ? C231 C232 1.390(4) . ? C231 P2 1.824(2) . ? C232 C233 1.384(4) . ? C232 H035 0.9500 . ? C233 C234 1.372(4) . ? C233 H041 0.9500 . ? C234 C235 1.381(5) . ? C234 H042 0.9500 . ? C235 C236 1.392(4) . ? C235 H039 0.9500 . ? C236 H032 0.9500 . ? O1 S1 1.4465(18) . ? O2 S1 1.4373(18) . ? O3 S1 1.4394(18) . ? P1 Ni1 2.2282(6) . ? P2 Ni1 2.2307(7) . ? Cl1 Ni1 2.2119(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl02 C001 Cl01 110.62(17) . . ? Cl02 C001 H77A 109.5 . . ? Cl01 C001 H77A 109.5 . . ? Cl02 C001 H77B 109.5 . . ? Cl01 C001 H77B 109.5 . . ? H77A C001 H77B 108.1 . . ? C3 C4 C5 116.6(2) . . ? C3 C4 Ni1 125.18(17) . . ? C5 C4 Ni1 118.19(17) . . ? F1 C01 F2 107.8(2) . . ? F1 C01 F3 107.2(2) . . ? F2 C01 F3 107.2(2) . . ? F1 C01 S1 111.58(18) . . ? F2 C01 S1 111.77(18) . . ? F3 C01 S1 111.10(18) . . ? C2 C3 C4 119.8(2) . . ? C2 C3 H002 120.1 . . ? C4 C3 H002 120.1 . . ? N1 C2 C3 122.3(2) . . ? N1 C2 Cl21 116.92(18) . . ? C3 C2 Cl21 120.79(18) . . ? N1 C6 C5 121.2(2) . . ? N1 C6 H020 119.4 . . ? C5 C6 H020 119.4 . . ? C6 C5 C4 121.2(2) . . ? C6 C5 H028 119.4 . . ? C4 C5 H028 119.4 . . ? N1 C11 H03A 109.5 . . ? N1 C11 H03B 109.5 . . ? H03A C11 H03B 109.5 . . ? N1 C11 H03C 109.5 . . ? H03A C11 H03C 109.5 . . ? H03B C11 H03C 109.5 . . ? C112 C111 C116 118.9(2) . . ? C112 C111 P1 120.49(17) . . ? C116 C111 P1 119.83(17) . . ? C113 C112 C111 120.1(2) . . ? C113 C112 H011 120.0 . . ? C111 C112 H011 120.0 . . ? C114 C113 C112 120.7(2) . . ? C114 C113 H029 119.7 . . ? C112 C113 H029 119.7 . . ? C113 C114 C115 119.5(2) . . ? C113 C114 H016 120.2 . . ? C115 C114 H016 120.2 . . ? C116 C115 C114 120.3(2) . . ? C116 C115 H009 119.9 . . ? C114 C115 H009 119.9 . . ? C115 C116 C111 120.6(2) . . ? C115 C116 H010 119.7 . . ? C111 C116 H010 119.7 . . ? C126 C121 C122 119.1(2) . . ? C126 C121 P1 124.24(19) . . ? C122 C121 P1 116.66(18) . . ? C123 C122 C121 121.0(2) . . ? C123 C122 H030 119.5 . . ? C121 C122 H030 119.5 . . ? C122 C123 C124 119.2(3) . . ? C122 C123 H033 120.4 . . ? C124 C123 H033 120.4 . . ? C125 C124 C123 120.5(2) . . ? C125 C124 H036 119.8 . . ? C123 C124 H036 119.8 . . ? C124 C125 C126 120.5(3) . . ? C124 C125 H037 119.8 . . ? C126 C125 H037 119.8 . . ? C121 C126 C125 119.7(2) . . ? C121 C126 H038 120.1 . . ? C125 C126 H038 120.1 . . ? C132 C131 C136 119.4(2) . . ? C132 C131 P1 118.96(18) . . ? C136 C131 P1 121.53(18) . . ? C133 C132 C131 119.9(2) . . ? C133 C132 H001 120.0 . . ? C131 C132 H001 120.0 . . ? C134 C133 C132 120.5(2) . . ? C134 C133 H008 119.7 . . ? C132 C133 H008 119.7 . . ? C133 C134 C135 120.0(2) . . ? C133 C134 H012 120.0 . . ? C135 C134 H012 120.0 . . ? C134 C135 C136 120.2(2) . . ? C134 C135 H043 119.9 . . ? C136 C135 H043 119.9 . . ? C135 C136 C131 120.0(2) . . ? C135 C136 H026 120.0 . . ? C131 C136 H026 120.0 . . ? C212 C211 C216 119.3(2) . . ? C212 C211 P2 118.78(17) . . ? C216 C211 P2 120.96(17) . . ? C213 C212 C211 120.2(2) . . ? C213 C212 H007 119.9 . . ? C211 C212 H007 119.9 . . ? C212 C213 C214 120.6(2) . . ? C212 C213 H022 119.7 . . ? C214 C213 H022 119.7 . . ? C213 C214 C215 119.5(2) . . ? C213 C214 H013 120.3 . . ? C215 C214 H013 120.3 . . ? C216 C215 C214 120.4(2) . . ? C216 C215 H014 119.8 . . ? C214 C215 H014 119.8 . . ? C215 C216 C211 119.9(2) . . ? C215 C216 H017 120.0 . . ? C211 C216 H017 120.0 . . ? C226 C221 C222 119.0(2) . . ? C226 C221 P2 118.26(18) . . ? C222 C221 P2 122.61(18) . . ? C223 C222 C221 120.1(2) . . ? C223 C222 H021 120.0 . . ? C221 C222 H021 120.0 . . ? C224 C223 C222 120.3(2) . . ? C224 C223 H023 119.8 . . ? C222 C223 H023 119.8 . . ? C223 C224 C225 120.0(2) . . ? C223 C224 H025 120.0 . . ? C225 C224 H025 120.0 . . ? C224 C225 C226 120.0(2) . . ? C224 C225 H040 120.0 . . ? C226 C225 H040 120.0 . . ? C221 C226 C225 120.6(2) . . ? C221 C226 H031 119.7 . . ? C225 C226 H031 119.7 . . ? C236 C231 C232 119.2(2) . . ? C236 C231 P2 119.2(2) . . ? C232 C231 P2 121.54(19) . . ? C233 C232 C231 120.5(3) . . ? C233 C232 H035 119.7 . . ? C231 C232 H035 119.7 . . ? C234 C233 C232 119.9(3) . . ? C234 C233 H041 120.0 . . ? C232 C233 H041 120.0 . . ? C233 C234 C235 120.4(3) . . ? C233 C234 H042 119.8 . . ? C235 C234 H042 119.8 . . ? C234 C235 C236 120.0(3) . . ? C234 C235 H039 120.0 . . ? C236 C235 H039 120.0 . . ? C231 C236 C235 119.9(3) . . ? C231 C236 H032 120.1 . . ? C235 C236 H032 120.1 . . ? C6 N1 C2 118.8(2) . . ? C6 N1 C11 119.3(2) . . ? C2 N1 C11 121.9(2) . . ? C131 P1 C121 109.09(11) . . ? C131 P1 C111 103.72(11) . . ? C121 P1 C111 104.89(10) . . ? C131 P1 Ni1 113.08(8) . . ? C121 P1 Ni1 109.25(8) . . ? C111 P1 Ni1 116.29(7) . . ? C231 P2 C221 106.20(11) . . ? C231 P2 C211 104.53(11) . . ? C221 P2 C211 103.51(10) . . ? C231 P2 Ni1 116.02(9) . . ? C221 P2 Ni1 111.34(8) . . ? C211 P2 Ni1 114.14(7) . . ? O2 S1 O3 115.72(11) . . ? O2 S1 O1 114.96(11) . . ? O3 S1 O1 114.82(11) . . ? O2 S1 C01 103.36(12) . . ? O3 S1 C01 103.02(11) . . ? O1 S1 C01 102.32(12) . . ? C4 Ni1 Cl1 170.24(7) . . ? C4 Ni1 P1 88.69(7) . . ? Cl1 Ni1 P1 91.57(2) . . ? C4 Ni1 P2 88.57(7) . . ? Cl1 Ni1 P2 92.69(2) . . ? P1 Ni1 P2 170.34(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C4 C3 C2 0.7(3) . . . . ? Ni1 C4 C3 C2 -179.66(17) . . . . ? C4 C3 C2 N1 -1.4(3) . . . . ? C4 C3 C2 Cl21 178.02(17) . . . . ? N1 C6 C5 C4 -1.9(3) . . . . ? C3 C4 C5 C6 0.9(3) . . . . ? Ni1 C4 C5 C6 -178.75(17) . . . . ? C116 C111 C112 C113 -0.3(3) . . . . ? P1 C111 C112 C113 169.49(17) . . . . ? C111 C112 C113 C114 -0.1(3) . . . . ? C112 C113 C114 C115 0.3(4) . . . . ? C113 C114 C115 C116 0.0(3) . . . . ? C114 C115 C116 C111 -0.4(3) . . . . ? C112 C111 C116 C115 0.5(3) . . . . ? P1 C111 C116 C115 -169.32(17) . . . . ? C126 C121 C122 C123 0.9(4) . . . . ? P1 C121 C122 C123 -178.2(2) . . . . ? C121 C122 C123 C124 0.0(4) . . . . ? C122 C123 C124 C125 -1.0(4) . . . . ? C123 C124 C125 C126 1.1(4) . . . . ? C122 C121 C126 C125 -0.8(4) . . . . ? P1 C121 C126 C125 178.3(2) . . . . ? C124 C125 C126 C121 -0.2(4) . . . . ? C136 C131 C132 C133 -0.5(3) . . . . ? P1 C131 C132 C133 -176.97(18) . . . . ? C131 C132 C133 C134 0.1(4) . . . . ? C132 C133 C134 C135 -0.3(4) . . . . ? C133 C134 C135 C136 0.9(4) . . . . ? C134 C135 C136 C131 -1.3(4) . . . . ? C132 C131 C136 C135 1.1(4) . . . . ? P1 C131 C136 C135 177.50(19) . . . . ? C216 C211 C212 C213 0.4(3) . . . . ? P2 C211 C212 C213 -168.72(18) . . . . ? C211 C212 C213 C214 0.6(3) . . . . ? C212 C213 C214 C215 -1.1(3) . . . . ? C213 C214 C215 C216 0.6(3) . . . . ? C214 C215 C216 C211 0.3(3) . . . . ? C212 C211 C216 C215 -0.8(3) . . . . ? P2 C211 C216 C215 168.06(17) . . . . ? C226 C221 C222 C223 0.6(4) . . . . ? P2 C221 C222 C223 177.0(2) . . . . ? C221 C222 C223 C224 0.5(4) . . . . ? C222 C223 C224 C225 -1.7(4) . . . . ? C223 C224 C225 C226 1.7(4) . . . . ? C222 C221 C226 C225 -0.6(4) . . . . ? P2 C221 C226 C225 -177.0(2) . . . . ? C224 C225 C226 C221 -0.6(4) . . . . ? C236 C231 C232 C233 -1.6(4) . . . . ? P2 C231 C232 C233 175.1(2) . . . . ? C231 C232 C233 C234 0.9(4) . . . . ? C232 C233 C234 C235 0.8(5) . . . . ? C233 C234 C235 C236 -1.9(5) . . . . ? C232 C231 C236 C235 0.5(4) . . . . ? P2 C231 C236 C235 -176.2(2) . . . . ? C234 C235 C236 C231 1.2(5) . . . . ? C5 C6 N1 C2 1.2(3) . . . . ? C5 C6 N1 C11 -179.5(2) . . . . ? C3 C2 N1 C6 0.5(3) . . . . ? Cl21 C2 N1 C6 -178.96(17) . . . . ? C3 C2 N1 C11 -178.8(2) . . . . ? Cl21 C2 N1 C11 1.8(3) . . . . ? C132 C131 P1 C121 -115.38(19) . . . . ? C136 C131 P1 C121 68.2(2) . . . . ? C132 C131 P1 C111 133.24(18) . . . . ? C136 C131 P1 C111 -43.2(2) . . . . ? C132 C131 P1 Ni1 6.4(2) . . . . ? C136 C131 P1 Ni1 -170.02(17) . . . . ? C126 C121 P1 C131 -17.9(2) . . . . ? C122 C121 P1 C131 161.21(19) . . . . ? C126 C121 P1 C111 92.7(2) . . . . ? C122 C121 P1 C111 -88.2(2) . . . . ? C126 C121 P1 Ni1 -141.9(2) . . . . ? C122 C121 P1 Ni1 37.1(2) . . . . ? C112 C111 P1 C131 149.86(18) . . . . ? C116 C111 P1 C131 -40.5(2) . . . . ? C112 C111 P1 C121 35.4(2) . . . . ? C116 C111 P1 C121 -154.87(18) . . . . ? C112 C111 P1 Ni1 -85.35(18) . . . . ? C116 C111 P1 Ni1 84.33(18) . . . . ? C236 C231 P2 C221 102.5(2) . . . . ? C232 C231 P2 C221 -74.2(2) . . . . ? C236 C231 P2 C211 -148.4(2) . . . . ? C232 C231 P2 C211 34.9(2) . . . . ? C236 C231 P2 Ni1 -21.8(2) . . . . ? C232 C231 P2 Ni1 161.48(18) . . . . ? C226 C221 P2 C231 -155.7(2) . . . . ? C222 C221 P2 C231 27.9(2) . . . . ? C226 C221 P2 C211 94.5(2) . . . . ? C222 C221 P2 C211 -81.9(2) . . . . ? C226 C221 P2 Ni1 -28.6(2) . . . . ? C222 C221 P2 Ni1 155.09(18) . . . . ? C212 C211 P2 C231 -149.35(18) . . . . ? C216 C211 P2 C231 41.8(2) . . . . ? C212 C211 P2 C221 -38.3(2) . . . . ? C216 C211 P2 C221 152.77(18) . . . . ? C212 C211 P2 Ni1 82.86(18) . . . . ? C216 C211 P2 Ni1 -86.04(19) . . . . ? F1 C01 S1 O2 -170.39(17) . . . . ? F2 C01 S1 O2 68.86(19) . . . . ? F3 C01 S1 O2 -50.8(2) . . . . ? F1 C01 S1 O3 68.77(19) . . . . ? F2 C01 S1 O3 -52.0(2) . . . . ? F3 C01 S1 O3 -171.61(17) . . . . ? F1 C01 S1 O1 -50.67(19) . . . . ? F2 C01 S1 O1 -171.42(17) . . . . ? F3 C01 S1 O1 68.95(19) . . . . ? C3 C4 Ni1 Cl1 173.4(3) . . . . ? C5 C4 Ni1 Cl1 -7.0(5) . . . . ? C3 C4 Ni1 P1 81.70(18) . . . . ? C5 C4 Ni1 P1 -98.64(17) . . . . ? C3 C4 Ni1 P2 -89.04(18) . . . . ? C5 C4 Ni1 P2 90.62(17) . . . . ? C131 P1 Ni1 C4 99.05(11) . . . . ? C121 P1 Ni1 C4 -139.26(11) . . . . ? C111 P1 Ni1 C4 -20.82(11) . . . . ? C131 P1 Ni1 Cl1 -71.19(8) . . . . ? C121 P1 Ni1 Cl1 50.50(8) . . . . ? C111 P1 Ni1 Cl1 168.94(8) . . . . ? C131 P1 Ni1 P2 172.61(15) . . . . ? C121 P1 Ni1 P2 -65.70(17) . . . . ? C111 P1 Ni1 P2 52.74(18) . . . . ? C231 P2 Ni1 C4 -98.95(11) . . . . ? C221 P2 Ni1 C4 139.44(11) . . . . ? C211 P2 Ni1 C4 22.69(11) . . . . ? C231 P2 Ni1 Cl1 71.36(9) . . . . ? C221 P2 Ni1 Cl1 -50.24(8) . . . . ? C211 P2 Ni1 Cl1 -166.99(8) . . . . ? C231 P2 Ni1 P1 -172.52(16) . . . . ? C221 P2 Ni1 P1 65.87(18) . . . . ? C211 P2 Ni1 P1 -50.88(18) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.720 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.071 #===END data_9aOTf _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H38 Cl2 N P2 Pd, C F3 O3 S' _chemical_formula_sum 'C47 H38 Cl2 F3 N O3 P2 Pd S' _chemical_formula_weight 993.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.183(6) _cell_length_b 11.472(2) _cell_length_c 34.952(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.278(4) _cell_angle_gamma 90.00 _cell_volume 9966(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5762 _cell_measurement_theta_min 2.217 _cell_measurement_theta_max 26.193 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7512 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area detector' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26296 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.35 _reflns_number_total 9103 _reflns_number_gt 7069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2003)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. During the structure refinement 2 dichloromethane molecules were found, but could not be refined properly due to disorder. The SQUEEZE routine of Platon was used to modify the hkl-file (see end of file)! ; _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^)+(0.0534P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9103 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _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 C01 C 0.37395(15) 0.5550(4) 0.09703(12) 0.0390(10) Uani 1 1 d . . . C2 C 0.07165(13) 0.9097(3) 0.09229(10) 0.0202(7) Uani 1 1 d . . . H47 H 0.0386 0.9424 0.0947 0.024 Uiso 1 1 calc R . . C3 C 0.09232(12) 0.8218(3) 0.11753(9) 0.0184(7) Uani 1 1 d . . . H8 H 0.0731 0.7976 0.1367 0.022 Uiso 1 1 calc R . . C4 C 0.14085(12) 0.7695(2) 0.11469(9) 0.0145(7) Uani 1 1 d . . . C5 C 0.22086(12) 0.7695(3) 0.08137(10) 0.0200(7) Uani 1 1 d . . . H42 H 0.2357 0.7086 0.0971 0.024 Uiso 1 1 calc R . . C6 C 0.24867(13) 0.8131(3) 0.05439(10) 0.0241(8) Uani 1 1 d . . . H41 H 0.2823 0.7833 0.0519 0.029 Uiso 1 1 calc R . . C7 C 0.22572(13) 0.9039(3) 0.03021(10) 0.0214(7) Uani 1 1 d . . . C8 C 0.17620(13) 0.9489(3) 0.03284(9) 0.0184(7) Uani 1 1 d . . . H45 H 0.1614 1.0077 0.0161 0.022 Uiso 1 1 calc R . . C9 C 0.14814(12) 0.9049(3) 0.06114(9) 0.0153(7) Uani 1 1 d . . . C10 C 0.16981(12) 0.8140(3) 0.08634(9) 0.0155(7) Uani 1 1 d . . . C11 C 0.07280(13) 1.0388(3) 0.03769(10) 0.0245(8) Uani 1 1 d . . . H48A H 0.0375 1.0562 0.0432 0.037 Uiso 1 1 calc R . . H48B H 0.0700 1.0110 0.0115 0.037 Uiso 1 1 calc R . . H48C H 0.0944 1.1081 0.0407 0.037 Uiso 1 1 calc R . . C111 C 0.19998(13) 0.9100(3) 0.18511(9) 0.0192(7) Uani 1 1 d . . . C112 C 0.23182(14) 0.9603(3) 0.16058(10) 0.0242(8) Uani 1 1 d . . . H11 H 0.2591 0.9169 0.1524 0.029 Uiso 1 1 calc R . . C113 C 0.22327(16) 1.0742(3) 0.14827(11) 0.0350(9) Uani 1 1 d . . . H340 H 0.2449 1.1075 0.1320 0.042 Uiso 1 1 calc R . . C114 C 0.18257(17) 1.1386(3) 0.16008(11) 0.0355(9) Uani 1 1 d . . . H13 H 0.1766 1.2151 0.1516 0.043 Uiso 1 1 calc R . . C115 C 0.15080(16) 1.0894(3) 0.18444(11) 0.0332(9) Uani 1 1 d . . . H390 H 0.1236 1.1333 0.1925 0.040 Uiso 1 1 calc R . . C116 C 0.15898(14) 0.9762(3) 0.19696(10) 0.0248(8) Uani 1 1 d . . . H24 H 0.1372 0.9437 0.2133 0.030 Uiso 1 1 calc R . . C121 C 0.28071(12) 0.7362(3) 0.20779(9) 0.0192(7) Uani 1 1 d . . . C122 C 0.30459(14) 0.6337(3) 0.19787(10) 0.0245(8) Uani 1 1 d . . . H33 H 0.2833 0.5754 0.1848 0.029 Uiso 1 1 calc R . . C123 C 0.35969(14) 0.6171(3) 0.20723(11) 0.0296(8) Uani 1 1 d . . . H34 H 0.3751 0.5482 0.2003 0.036 Uiso 1 1 calc R . . C124 C 0.39156(14) 0.7028(3) 0.22674(10) 0.0300(9) Uani 1 1 d . . . H23 H 0.4285 0.6917 0.2332 0.036 Uiso 1 1 calc R . . C125 C 0.36856(14) 0.8046(3) 0.23665(10) 0.0311(9) Uani 1 1 d . . . H430 H 0.3901 0.8621 0.2499 0.037 Uiso 1 1 calc R . . C126 C 0.31320(14) 0.8229(3) 0.22701(10) 0.0268(8) Uani 1 1 d . . . H31 H 0.2981 0.8929 0.2334 0.032 Uiso 1 1 calc R . . C131 C 0.18189(13) 0.7374(3) 0.24177(10) 0.0198(7) Uani 1 1 d . . . C132 C 0.14266(17) 0.6563(4) 0.24597(12) 0.0423(10) Uani 1 1 d . . . H27 H 0.1285 0.6096 0.2251 0.051 Uiso 1 1 calc R . . C133 C 0.12408(19) 0.6438(4) 0.28134(14) 0.0514(12) Uani 1 1 d . . . H102 H 0.0982 0.5877 0.2838 0.062 Uiso 1 1 calc R . . C134 C 0.14331(15) 0.7127(3) 0.31225(11) 0.0339(9) Uani 1 1 d . . . H104 H 0.1302 0.7048 0.3355 0.041 Uiso 1 1 calc R . . C135 C 0.18194(16) 0.7931(4) 0.30857(10) 0.0363(9) Uani 1 1 d . . . H15 H 0.1954 0.8404 0.3295 0.044 Uiso 1 1 calc R . . C136 C 0.20138(15) 0.8048(4) 0.27377(10) 0.0360(10) Uani 1 1 d . . . H18 H 0.2281 0.8594 0.2719 0.043 Uiso 1 1 calc R . . C211 C 0.07771(13) 0.5835(3) 0.05820(9) 0.0203(7) Uani 1 1 d . . . C212 C 0.10207(15) 0.6256(3) 0.02794(10) 0.0272(8) Uani 1 1 d . . . H10 H 0.1383 0.6103 0.0276 0.033 Uiso 1 1 calc R . . C213 C 0.07284(17) 0.6902(3) -0.00172(11) 0.0368(10) Uani 1 1 d . . . H20 H 0.0894 0.7171 -0.0220 0.044 Uiso 1 1 calc R . . C214 C 0.01983(18) 0.7145(3) -0.00126(12) 0.0438(11) Uani 1 1 d . . . H79 H 0.0004 0.7580 -0.0212 0.053 Uiso 1 1 calc R . . C215 C -0.00491(16) 0.6748(4) 0.02872(13) 0.0452(11) Uani 1 1 d . . . H440 H -0.0409 0.6920 0.0290 0.054 Uiso 1 1 calc R . . C216 C 0.02390(14) 0.6089(3) 0.05863(11) 0.0309(9) Uani 1 1 d . . . H400 H 0.0071 0.5821 0.0788 0.037 Uiso 1 1 calc R . . C221 C 0.16168(12) 0.4134(3) 0.07720(9) 0.0173(7) Uani 1 1 d . . . C222 C 0.14231(13) 0.3541(3) 0.04292(9) 0.0203(7) Uani 1 1 d . . . H39 H 0.1073 0.3676 0.0306 0.024 Uiso 1 1 calc R . . C223 C 0.17406(14) 0.2760(3) 0.02697(10) 0.0246(8) Uani 1 1 d . . . H38 H 0.1606 0.2374 0.0041 0.030 Uiso 1 1 calc R . . C224 C 0.22618(14) 0.2555(3) 0.04524(10) 0.0253(8) Uani 1 1 d . . . H37 H 0.2475 0.2015 0.0349 0.030 Uiso 1 1 calc R . . C225 C 0.24667(13) 0.3150(3) 0.07875(10) 0.0235(7) Uani 1 1 d . . . H36 H 0.2819 0.3021 0.0907 0.028 Uiso 1 1 calc R . . C226 C 0.21456(13) 0.3939(3) 0.09451(10) 0.0206(7) Uani 1 1 d . . . H29 H 0.2286 0.4343 0.1169 0.025 Uiso 1 1 calc R . . C231 C 0.07150(12) 0.4232(3) 0.12099(9) 0.0209(7) Uani 1 1 d . . . C232 C 0.04691(15) 0.4737(3) 0.14990(11) 0.0349(9) Uani 1 1 d . . . H26 H 0.0555 0.5498 0.1577 0.042 Uiso 1 1 calc R . . C233 C 0.00993(16) 0.4125(4) 0.16719(12) 0.0420(10) Uani 1 1 d . . . H105 H -0.0063 0.4475 0.1863 0.050 Uiso 1 1 calc R . . C234 C -0.00280(15) 0.2993(3) 0.15594(11) 0.0360(9) Uani 1 1 d . . . H80 H -0.0278 0.2581 0.1674 0.043 Uiso 1 1 calc R . . C235 C 0.02144(15) 0.2474(3) 0.12772(12) 0.0367(9) Uani 1 1 d . . . H380 H 0.0133 0.1706 0.1205 0.044 Uiso 1 1 calc R . . C236 C 0.05825(14) 0.3099(3) 0.10999(10) 0.0282(8) Uani 1 1 d . . . H310 H 0.0740 0.2750 0.0906 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.18686(3) 0.46230(7) 0.18487(2) 0.02262(19) Uani 1 1 d . . . Cl71 Cl 0.26188(4) 0.96181(8) -0.00363(3) 0.0371(2) Uani 1 1 d . . . F1 F 0.40403(10) 0.6173(2) 0.12420(8) 0.0548(7) Uani 1 1 d . . . F2 F 0.35004(13) 0.6281(3) 0.07103(10) 0.0933(12) Uani 1 1 d . . . F3 F 0.33741(12) 0.5022(3) 0.11387(10) 0.0955(13) Uani 1 1 d . . . N1 N 0.09796(10) 0.9484(2) 0.06470(7) 0.0167(6) Uani 1 1 d . . . O1 O 0.37564(11) 0.3940(2) 0.04631(7) 0.0353(6) Uani 1 1 d . . . O2 O 0.45080(11) 0.5247(3) 0.05925(9) 0.0502(8) Uani 1 1 d . . . O3 O 0.43960(17) 0.3816(3) 0.10621(9) 0.0743(11) Uani 1 1 d . . . P1 P 0.20770(3) 0.75517(7) 0.19639(2) 0.01689(18) Uani 1 1 d . . . P2 P 0.11908(3) 0.51190(7) 0.09952(2) 0.01547(18) Uani 1 1 d . . . Pd1 Pd 0.165045(9) 0.632136(19) 0.147589(7) 0.01403(8) Uani 1 1 d . . . S1 S 0.41369(4) 0.45115(8) 0.07487(3) 0.0298(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C01 0.025(2) 0.045(3) 0.047(3) -0.019(2) 0.0048(19) -0.0038(19) C2 0.0206(16) 0.0152(16) 0.0241(19) -0.0007(14) 0.0017(15) 0.0018(13) C3 0.0195(16) 0.0177(16) 0.0181(17) 0.0013(13) 0.0033(14) -0.0004(14) C4 0.0202(16) 0.0083(15) 0.0129(16) -0.0027(12) -0.0041(13) -0.0043(12) C5 0.0205(16) 0.0115(16) 0.0271(19) 0.0025(14) 0.0013(14) 0.0035(13) C6 0.0159(16) 0.0203(18) 0.037(2) -0.0051(16) 0.0087(15) 0.0011(14) C7 0.0256(18) 0.0156(16) 0.0255(19) -0.0010(14) 0.0115(15) -0.0036(14) C8 0.0232(17) 0.0108(16) 0.0214(17) 0.0038(13) 0.0047(14) 0.0001(13) C9 0.0167(15) 0.0106(15) 0.0184(17) -0.0032(12) 0.0020(13) 0.0000(12) C10 0.0180(15) 0.0123(15) 0.0153(16) -0.0012(13) 0.0001(13) -0.0005(13) C11 0.0230(17) 0.0229(18) 0.029(2) 0.0129(15) 0.0072(15) 0.0085(15) C111 0.0244(17) 0.0108(15) 0.0194(18) -0.0032(13) -0.0055(14) -0.0020(13) C112 0.0264(18) 0.0155(17) 0.030(2) -0.0046(15) 0.0028(16) -0.0033(14) C113 0.042(2) 0.023(2) 0.039(2) 0.0061(17) 0.0055(19) -0.0102(17) C114 0.053(2) 0.0112(17) 0.038(2) 0.0022(16) -0.0061(19) 0.0006(17) C115 0.046(2) 0.0190(18) 0.035(2) -0.0033(16) 0.0069(19) 0.0067(17) C116 0.0319(19) 0.0190(17) 0.0239(19) -0.0029(14) 0.0055(16) 0.0034(15) C121 0.0183(16) 0.0223(17) 0.0165(17) 0.0021(13) 0.0011(14) -0.0010(14) C122 0.0260(18) 0.0257(19) 0.0209(18) -0.0040(15) 0.0005(15) -0.0002(15) C123 0.0294(19) 0.033(2) 0.028(2) -0.0001(16) 0.0091(16) 0.0068(16) C124 0.0162(16) 0.046(2) 0.027(2) 0.0063(17) 0.0013(15) 0.0041(17) C125 0.0271(19) 0.037(2) 0.027(2) -0.0029(17) -0.0023(16) -0.0063(17) C126 0.0270(18) 0.0288(19) 0.0237(19) -0.0088(15) 0.0010(15) 0.0016(16) C131 0.0210(16) 0.0140(16) 0.0230(18) 0.0024(13) -0.0006(14) 0.0029(13) C132 0.049(2) 0.045(3) 0.036(2) -0.0198(19) 0.015(2) -0.017(2) C133 0.060(3) 0.043(3) 0.060(3) -0.016(2) 0.036(2) -0.020(2) C134 0.042(2) 0.033(2) 0.030(2) 0.0024(17) 0.0148(18) 0.0048(18) C135 0.042(2) 0.045(2) 0.0186(19) -0.0023(17) -0.0023(17) -0.0066(19) C136 0.039(2) 0.048(2) 0.0181(19) -0.0016(17) -0.0030(17) -0.0185(19) C211 0.0222(17) 0.0153(16) 0.0202(18) -0.0071(13) -0.0064(14) -0.0001(14) C212 0.0310(19) 0.0248(19) 0.0226(19) 0.0017(15) -0.0051(16) -0.0023(16) C213 0.054(3) 0.028(2) 0.024(2) 0.0045(17) -0.0086(19) 0.0000(19) C214 0.061(3) 0.032(2) 0.030(2) 0.0011(18) -0.021(2) 0.015(2) C215 0.032(2) 0.051(3) 0.045(3) -0.013(2) -0.019(2) 0.018(2) C216 0.0235(18) 0.033(2) 0.032(2) -0.0081(17) -0.0056(16) 0.0022(16) C221 0.0217(16) 0.0153(16) 0.0153(17) 0.0010(13) 0.0044(14) -0.0004(13) C222 0.0220(16) 0.0186(17) 0.0200(18) -0.0034(14) 0.0021(14) -0.0092(14) C223 0.040(2) 0.0151(17) 0.0203(18) -0.0044(14) 0.0089(16) -0.0078(15) C224 0.037(2) 0.0148(17) 0.028(2) 0.0013(14) 0.0174(17) 0.0015(15) C225 0.0245(17) 0.0208(18) 0.0261(19) 0.0062(15) 0.0065(15) 0.0014(15) C226 0.0270(17) 0.0165(17) 0.0177(18) -0.0013(13) 0.0023(14) -0.0052(14) C231 0.0200(16) 0.0217(17) 0.0198(18) -0.0012(14) -0.0008(14) -0.0043(14) C232 0.037(2) 0.036(2) 0.036(2) -0.0202(18) 0.0173(18) -0.0135(18) C233 0.043(2) 0.048(2) 0.040(2) -0.018(2) 0.020(2) -0.016(2) C234 0.036(2) 0.040(2) 0.034(2) 0.0004(18) 0.0142(18) -0.0136(18) C235 0.041(2) 0.024(2) 0.049(3) -0.0061(18) 0.018(2) -0.0120(17) C236 0.0300(19) 0.0246(19) 0.032(2) -0.0074(16) 0.0118(16) -0.0058(16) Cl1 0.0324(4) 0.0150(4) 0.0187(4) 0.0047(3) -0.0010(3) 0.0036(3) Cl71 0.0437(6) 0.0258(5) 0.0495(6) 0.0060(4) 0.0313(5) 0.0000(4) F1 0.0487(14) 0.0591(16) 0.0591(17) -0.0384(13) 0.0166(13) -0.0203(12) F2 0.090(2) 0.075(2) 0.102(3) -0.0298(19) -0.022(2) 0.0600(19) F3 0.072(2) 0.130(3) 0.102(2) -0.079(2) 0.0660(19) -0.070(2) N1 0.0193(13) 0.0110(13) 0.0191(14) 0.0027(11) 0.0008(11) 0.0010(11) O1 0.0465(16) 0.0342(15) 0.0238(14) -0.0088(11) 0.0013(12) -0.0086(12) O2 0.0309(15) 0.071(2) 0.0528(19) -0.0237(16) 0.0182(14) -0.0138(14) O3 0.117(3) 0.060(2) 0.0361(19) 0.0017(16) -0.019(2) 0.028(2) P1 0.0204(4) 0.0125(4) 0.0163(4) -0.0012(3) -0.0013(3) -0.0002(3) P2 0.0178(4) 0.0130(4) 0.0145(4) -0.0014(3) -0.0008(3) -0.0001(3) Pd1 0.01839(13) 0.00978(12) 0.01245(13) 0.00044(9) -0.00195(9) 0.00025(10) S1 0.0366(5) 0.0291(5) 0.0211(5) -0.0024(4) -0.0032(4) 0.0074(4) _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 C01 F2 1.310(5) . ? C01 F3 1.317(5) . ? C01 F1 1.324(4) . ? C01 S1 1.809(4) . ? C2 N1 1.331(4) . ? C2 C3 1.384(4) . ? C2 H47 0.9300 . ? C3 C4 1.379(4) . ? C3 H8 0.9300 . ? C4 C10 1.417(4) . ? C4 Pd1 1.988(3) . ? C5 C6 1.357(5) . ? C5 C10 1.420(4) . ? C5 H42 0.9300 . ? C6 C7 1.406(5) . ? C6 H41 0.9300 . ? C7 C8 1.366(4) . ? C7 Cl71 1.737(3) . ? C8 C9 1.399(4) . ? C8 H45 0.9300 . ? C9 N1 1.383(4) . ? C9 C10 1.416(4) . ? C11 N1 1.475(4) . ? C11 H48A 0.9600 . ? C11 H48B 0.9600 . ? C11 H48C 0.9600 . ? C111 C112 1.390(5) . ? C111 C116 1.397(5) . ? C111 P1 1.823(3) . ? C112 C113 1.383(5) . ? C112 H11 0.9300 . ? C113 C114 1.380(6) . ? C113 H340 0.9300 . ? C114 C115 1.380(6) . ? C114 H13 0.9300 . ? C115 C116 1.376(5) . ? C115 H390 0.9300 . ? C116 H24 0.9300 . ? C121 C122 1.389(5) . ? C121 C126 1.391(5) . ? C121 P1 1.830(3) . ? C122 C123 1.387(5) . ? C122 H33 0.9300 . ? C123 C124 1.378(5) . ? C123 H34 0.9300 . ? C124 C125 1.373(5) . ? C124 H23 0.9300 . ? C125 C126 1.396(5) . ? C125 H430 0.9300 . ? C126 H31 0.9300 . ? C131 C132 1.382(5) . ? C131 C136 1.383(5) . ? C131 P1 1.820(4) . ? C132 C133 1.398(6) . ? C132 H27 0.9300 . ? C133 C134 1.363(6) . ? C133 H102 0.9300 . ? C134 C135 1.362(5) . ? C134 H104 0.9300 . ? C135 C136 1.389(5) . ? C135 H15 0.9300 . ? C136 H18 0.9300 . ? C211 C216 1.389(5) . ? C211 C212 1.392(5) . ? C211 P2 1.833(3) . ? C212 C213 1.386(5) . ? C212 H10 0.9300 . ? C213 C214 1.366(6) . ? C213 H20 0.9300 . ? C214 C215 1.380(6) . ? C214 H79 0.9300 . ? C215 C216 1.395(5) . ? C215 H440 0.9300 . ? C216 H400 0.9300 . ? C221 C226 1.389(4) . ? C221 C222 1.395(4) . ? C221 P2 1.818(3) . ? C222 C223 1.377(5) . ? C222 H39 0.9300 . ? C223 C224 1.384(5) . ? C223 H38 0.9300 . ? C224 C225 1.381(5) . ? C224 H37 0.9300 . ? C225 C226 1.386(5) . ? C225 H36 0.9300 . ? C226 H29 0.9300 . ? C231 C236 1.382(5) . ? C231 C232 1.393(5) . ? C231 P2 1.823(3) . ? C232 C233 1.381(5) . ? C232 H26 0.9300 . ? C233 C234 1.380(5) . ? C233 H105 0.9300 . ? C234 C235 1.377(5) . ? C234 H80 0.9300 . ? C235 C236 1.394(5) . ? C235 H380 0.9300 . ? C236 H310 0.9300 . ? Cl1 Pd1 2.3590(8) . ? O1 S1 1.427(3) . ? O2 S1 1.431(3) . ? O3 S1 1.425(3) . ? P1 Pd1 2.3376(9) . ? P2 Pd1 2.3321(9) . ? 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 F2 C01 F3 109.2(4) . . ? F2 C01 F1 107.3(3) . . ? F3 C01 F1 106.7(3) . . ? F2 C01 S1 110.4(3) . . ? F3 C01 S1 111.3(3) . . ? F1 C01 S1 111.8(3) . . ? N1 C2 C3 121.7(3) . . ? N1 C2 H47 119.2 . . ? C3 C2 H47 119.2 . . ? C4 C3 C2 121.1(3) . . ? C4 C3 H8 119.4 . . ? C2 C3 H8 119.4 . . ? C3 C4 C10 117.1(3) . . ? C3 C4 Pd1 119.7(2) . . ? C10 C4 Pd1 123.1(2) . . ? C6 C5 C10 122.1(3) . . ? C6 C5 H42 119.0 . . ? C10 C5 H42 119.0 . . ? C5 C6 C7 118.9(3) . . ? C5 C6 H41 120.6 . . ? C7 C6 H41 120.6 . . ? C8 C7 C6 122.0(3) . . ? C8 C7 Cl71 119.1(3) . . ? C6 C7 Cl71 118.9(2) . . ? C7 C8 C9 118.8(3) . . ? C7 C8 H45 120.6 . . ? C9 C8 H45 120.6 . . ? N1 C9 C8 120.4(3) . . ? N1 C9 C10 118.4(3) . . ? C8 C9 C10 121.1(3) . . ? C9 C10 C4 120.6(3) . . ? C9 C10 C5 117.0(3) . . ? C4 C10 C5 122.3(3) . . ? N1 C11 H48A 109.5 . . ? N1 C11 H48B 109.5 . . ? H48A C11 H48B 109.5 . . ? N1 C11 H48C 109.5 . . ? H48A C11 H48C 109.5 . . ? H48B C11 H48C 109.5 . . ? C112 C111 C116 119.0(3) . . ? C112 C111 P1 119.0(2) . . ? C116 C111 P1 121.6(3) . . ? C113 C112 C111 120.5(3) . . ? C113 C112 H11 119.7 . . ? C111 C112 H11 119.7 . . ? C114 C113 C112 120.0(4) . . ? C114 C113 H340 120.0 . . ? C112 C113 H340 120.0 . . ? C115 C114 C113 119.9(3) . . ? C115 C114 H13 120.1 . . ? C113 C114 H13 120.1 . . ? C116 C115 C114 120.7(4) . . ? C116 C115 H390 119.6 . . ? C114 C115 H390 119.6 . . ? C115 C116 C111 119.9(3) . . ? C115 C116 H24 120.0 . . ? C111 C116 H24 120.0 . . ? C122 C121 C126 118.8(3) . . ? C122 C121 P1 120.4(2) . . ? C126 C121 P1 120.8(2) . . ? C123 C122 C121 121.0(3) . . ? C123 C122 H33 119.5 . . ? C121 C122 H33 119.5 . . ? C124 C123 C122 120.0(3) . . ? C124 C123 H34 120.0 . . ? C122 C123 H34 120.0 . . ? C125 C124 C123 119.7(3) . . ? C125 C124 H23 120.1 . . ? C123 C124 H23 120.1 . . ? C124 C125 C126 120.8(3) . . ? C124 C125 H430 119.6 . . ? C126 C125 H430 119.6 . . ? C121 C126 C125 119.7(3) . . ? C121 C126 H31 120.1 . . ? C125 C126 H31 120.1 . . ? C132 C131 C136 117.2(3) . . ? C132 C131 P1 122.0(3) . . ? C136 C131 P1 120.8(3) . . ? C131 C132 C133 120.7(4) . . ? C131 C132 H27 119.7 . . ? C133 C132 H27 119.7 . . ? C134 C133 C132 121.0(4) . . ? C134 C133 H102 119.5 . . ? C132 C133 H102 119.5 . . ? C135 C134 C133 119.1(4) . . ? C135 C134 H104 120.5 . . ? C133 C134 H104 120.5 . . ? C134 C135 C136 120.4(4) . . ? C134 C135 H15 119.8 . . ? C136 C135 H15 119.8 . . ? C131 C136 C135 121.6(3) . . ? C131 C136 H18 119.2 . . ? C135 C136 H18 119.2 . . ? C216 C211 C212 119.1(3) . . ? C216 C211 P2 121.1(3) . . ? C212 C211 P2 119.3(2) . . ? C213 C212 C211 120.6(3) . . ? C213 C212 H10 119.7 . . ? C211 C212 H10 119.7 . . ? C214 C213 C212 120.2(4) . . ? C214 C213 H20 119.9 . . ? C212 C213 H20 119.9 . . ? C213 C214 C215 120.2(4) . . ? C213 C214 H79 119.9 . . ? C215 C214 H79 119.9 . . ? C214 C215 C216 120.3(4) . . ? C214 C215 H440 119.9 . . ? C216 C215 H440 119.9 . . ? C211 C216 C215 119.8(4) . . ? C211 C216 H400 120.1 . . ? C215 C216 H400 120.1 . . ? C226 C221 C222 118.3(3) . . ? C226 C221 P2 120.2(2) . . ? C222 C221 P2 121.5(2) . . ? C223 C222 C221 121.3(3) . . ? C223 C222 H39 119.4 . . ? C221 C222 H39 119.4 . . ? C222 C223 C224 119.5(3) . . ? C222 C223 H38 120.2 . . ? C224 C223 H38 120.2 . . ? C225 C224 C223 120.3(3) . . ? C225 C224 H37 119.9 . . ? C223 C224 H37 119.9 . . ? C224 C225 C226 119.8(3) . . ? C224 C225 H36 120.1 . . ? C226 C225 H36 120.1 . . ? C225 C226 C221 120.8(3) . . ? C225 C226 H29 119.6 . . ? C221 C226 H29 119.6 . . ? C236 C231 C232 118.5(3) . . ? C236 C231 P2 123.8(3) . . ? C232 C231 P2 117.7(3) . . ? C233 C232 C231 121.1(3) . . ? C233 C232 H26 119.5 . . ? C231 C232 H26 119.5 . . ? C234 C233 C232 119.7(4) . . ? C234 C233 H105 120.1 . . ? C232 C233 H105 120.1 . . ? C235 C234 C233 120.2(3) . . ? C235 C234 H80 119.9 . . ? C233 C234 H80 119.9 . . ? C234 C235 C236 119.9(3) . . ? C234 C235 H380 120.0 . . ? C236 C235 H380 120.0 . . ? C231 C236 C235 120.6(3) . . ? C231 C236 H310 119.7 . . ? C235 C236 H310 119.7 . . ? C2 N1 C9 120.9(3) . . ? C2 N1 C11 119.1(3) . . ? C9 N1 C11 120.1(3) . . ? C131 P1 C111 104.91(15) . . ? C131 P1 C121 106.50(14) . . ? C111 P1 C121 103.38(15) . . ? C131 P1 Pd1 112.42(11) . . ? C111 P1 Pd1 114.21(10) . . ? C121 P1 Pd1 114.47(11) . . ? C221 P2 C231 107.60(15) . . ? C221 P2 C211 103.89(15) . . ? C231 P2 C211 104.27(15) . . ? C221 P2 Pd1 114.71(10) . . ? C231 P2 Pd1 108.43(11) . . ? C211 P2 Pd1 117.12(10) . . ? C4 Pd1 P2 88.97(8) . . ? C4 Pd1 P1 90.30(8) . . ? P2 Pd1 P1 177.64(3) . . ? C4 Pd1 Cl1 175.35(9) . . ? P2 Pd1 Cl1 87.35(3) . . ? P1 Pd1 Cl1 93.27(3) . . ? O3 S1 O1 116.92(19) . . ? O3 S1 O2 112.1(2) . . ? O1 S1 O2 114.23(17) . . ? O3 S1 C01 104.8(2) . . ? O1 S1 C01 104.30(17) . . ? O2 S1 C01 102.43(19) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.913 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.087 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 0.500 0.165 0.250 452 149 ' ' 2 0.000 -0.335 0.250 452 149 ' ' 3 0.500 -0.166 0.750 451 149 ' ' 4 0.000 0.334 0.750 451 149 ' ' 5 0.500 0.155 0.750 9 0 ' ' 6 0.000 0.345 0.250 9 0 ' ' 7 0.000 0.655 0.750 9 0 ' ' 8 0.500 0.845 0.250 9 0 ' ' _platon_squeeze_details ; ;