# Copyright The Royal Society of Chemistry, 1998. data_kora # 1. SUBMISSION DETAILS _publ_contact_author ; Dr. Franc Meyer Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; _publ_contact_author_phone '049 6221 54-8315' _publ_contact_author_fax '049 6221 54-5707' _publ_contact_author_email MESS@MONDO.ACI.UNI-HEIDELBERG.DE _publ_requested_journal 'JCS Dalton Trans' _publ_requested_coeditor_name ? #================================================================ # 2. TITLE AND AUTHOR LIST _publ_section_title ; 'Unsymmetrically Substituted Pyrazolates: Nickel(II) Complexes of a Novel Dinucleating Ligand Providing both N- and S-rich Coordination Spheres' ; loop_ _publ_author_name _publ_author_address 'Matthias Konrad' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Franc Meyer' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Katja Heinze' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Laszlo Zsolnai' ; Anorganisch-Chemisches Institut Ruprecht-Karls Universitaet Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #================================================================ _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'compound 6' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52.20 H71 B Cl2 N6 Ni2 O0.80 S2' _chemical_formula_weight 1058.60 _chemical_melting_point ? _chemical_compound_source ? 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triklin _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.884(2) _cell_length_b 15.205(2) _cell_length_c 15.675(2) _cell_angle_alpha 70.820(10) _cell_angle_beta 65.930(10) _cell_angle_gamma 62.850(10) _cell_volume 2837.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method ? _exptl_crystal_F_000 1119 _exptl_absorpt_coefficient_mu 0.871 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11574 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11121 _reflns_number_observed 7865 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+5.8495P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11119 _refine_ls_number_parameters 654 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_obs 0.0544 _refine_ls_wR_factor_all 0.1771 _refine_ls_wR_factor_obs 0.1508 _refine_ls_goodness_of_fit_all 1.065 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_restrained_S_all 1.067 _refine_ls_restrained_S_obs 1.091 _refine_ls_shift/esd_max 0.719 _refine_ls_shift/esd_mean 0.011 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.26804(4) 0.36080(4) 0.91098(4) 0.02096(15) Uani 1 d . . Ni2 Ni 0.15294(4) 0.31838(4) 0.75084(4) 0.0245(2) Uani 1 d . . Cl1 Cl 0.10379(8) 0.37032(8) 0.90859(8) 0.0240(2) Uani 1 d . . Cl2 Cl -0.01288(9) 0.33183(8) 0.76086(9) 0.0320(3) Uani 1 d . . S1 S 0.12046(10) 0.49259(10) 0.65704(9) 0.0313(3) Uani 1 d . . S2 S 0.20445(11) 0.13581(9) 0.81260(11) 0.0391(3) Uani 1 d . . N1 N 0.3379(3) 0.3197(3) 0.7881(2) 0.0220(8) Uani 1 d . . N2 N 0.2988(3) 0.3047(3) 0.7317(3) 0.0265(8) Uani 1 d . . N3 N 0.2372(3) 0.2722(4) 0.6120(3) 0.0411(11) Uani 1 d . . N4 N 0.4269(3) 0.3447(3) 0.8899(3) 0.0258(8) Uani 1 d . . N5 N 0.2384(3) 0.5169(3) 0.8746(3) 0.0279(9) Uani 1 d . . N6 N 0.3055(3) 0.2202(3) 1.0062(3) 0.0250(8) Uani 1 d . . C1 C 0.4423(3) 0.2978(3) 0.7455(3) 0.0266(10) Uani 1 d . . C2 C 0.4724(4) 0.2676(4) 0.6599(4) 0.0330(11) Uani 1 d . . H2 H 0.5399(4) 0.2473(4) 0.6164(4) 0.034(14) Uiso 1 calc R . C3 C 0.3790(4) 0.2747(4) 0.6545(3) 0.0328(11) Uani 1 d . . C4 C 0.3536(4) 0.2529(5) 0.5827(4) 0.054(2) Uani 1 d . . H4A H 0.3950(4) 0.1833(5) 0.5752(4) 0.041(3) Uiso 1 calc R . H4B H 0.3730(4) 0.2948(5) 0.5220(4) 0.041(3) Uiso 1 calc R . C5 C 0.1882(5) 0.3557(5) 0.5417(4) 0.0455(15) Uani 1 d . . H5A H 0.1156(5) 0.3626(5) 0.5565(4) 0.041(3) Uiso 1 calc R . H5B H 0.2270(5) 0.3390(5) 0.4786(4) 0.041(3) Uiso 1 calc R . C6 C 0.1892(5) 0.4543(5) 0.5425(4) 0.0474(14) Uani 1 d . . H6A H 0.1565(5) 0.5060(5) 0.4964(4) 0.041(3) Uiso 1 calc R . H6B H 0.2622(5) 0.4485(5) 0.5231(4) 0.041(3) Uiso 1 calc R . C7 C 0.2205(5) 0.1800(4) 0.6206(4) 0.052(2) Uani 1 d . . H7A H 0.2576(5) 0.1563(4) 0.5605(4) 0.041(3) Uiso 1 calc R . H7B H 0.1454(5) 0.1964(4) 0.6344(4) 0.041(3) Uiso 1 calc R . C8 C 0.2593(6) 0.0975(4) 0.6976(5) 0.059(2) Uani 1 d . . H8A H 0.3360(6) 0.0741(4) 0.6785(5) 0.041(3) Uiso 1 calc R . H8B H 0.2411(6) 0.0415(4) 0.7038(5) 0.041(3) Uiso 1 calc R . C9 C 0.5002(4) 0.3099(4) 0.7980(4) 0.0312(11) Uani 1 d . . H9A H 0.5560(4) 0.2462(4) 0.8103(4) 0.041(3) Uiso 1 calc R . H9B H 0.5330(4) 0.3581(4) 0.7585(4) 0.041(3) Uiso 1 calc R . C10 C 0.4195(4) 0.4457(4) 0.8890(4) 0.0299(10) Uani 1 d . . H10A H 0.4891(4) 0.4498(4) 0.8590(4) 0.041(3) Uiso 1 calc R . H10B H 0.3936(4) 0.4574(4) 0.9535(4) 0.041(3) Uiso 1 calc R . C11 C 0.3444(4) 0.5241(4) 0.8348(4) 0.0287(10) Uani 1 d . . H11A H 0.3368(4) 0.5903(4) 0.8368(4) 0.041(3) Uiso 1 calc R . H11B H 0.3743(4) 0.5158(4) 0.7689(4) 0.041(3) Uiso 1 calc R . C12 C -0.0153(4) 0.5583(4) 0.6536(4) 0.0393(12) Uani 1 d . . H12A H -0.0317(4) 0.5192(4) 0.6282(4) 0.041(3) Uiso 1 calc R . H12B H -0.0628(4) 0.5637(4) 0.7178(4) 0.041(3) Uiso 1 calc R . C13 C -0.0348(5) 0.6625(4) 0.5937(5) 0.053(2) Uani 1 d . . H13A H -0.1086(8) 0.6957(12) 0.5982(23) 0.065(5) Uiso 1 calc R . H13B H 0.0069(25) 0.6573(5) 0.5288(7) 0.065(5) Uiso 1 calc R . H13C H -0.0151(30) 0.7005(11) 0.6164(18) 0.065(5) Uiso 1 calc R . C14 C 0.0901(5) 0.1002(4) 0.8677(6) 0.059(2) Uani 1 d . . H14A H 0.0411(5) 0.1362(4) 0.8307(6) 0.041(3) Uiso 1 calc R . H14B H 0.1119(5) 0.0288(4) 0.8712(6) 0.041(3) Uiso 1 calc R . C15 C 0.0364(6) 0.1264(5) 0.9678(6) 0.068(2) Uani 1 d . . H15A H -0.0242(19) 0.1074(28) 0.9990(12) 0.065(5) Uiso 1 calc R . H15B H 0.0140(29) 0.1974(7) 0.9635(6) 0.065(5) Uiso 1 calc R . H15C H 0.0857(11) 0.0909(24) 1.0037(11) 0.065(5) Uiso 1 calc R . C16 C 0.4572(4) 0.2688(4) 0.9711(4) 0.0327(11) Uani 1 d . . H16A H 0.4229(4) 0.2989(4) 1.0277(4) 0.041(3) Uiso 1 calc R . H16B H 0.5333(4) 0.2437(4) 0.9583(4) 0.041(3) Uiso 1 calc R . C17 C 0.4236(4) 0.1841(3) 0.9864(4) 0.0298(10) Uani 1 d . . H17A H 0.4435(4) 0.1339(3) 1.0395(4) 0.041(3) Uiso 1 calc R . H17B H 0.4603(4) 0.1529(3) 0.9304(4) 0.041(3) Uiso 1 calc R . C18 C 0.2821(4) 0.1466(3) 0.9826(4) 0.0302(10) Uani 1 d . . H18A H 0.3181(4) 0.1432(3) 0.9158(4) 0.041(3) Uiso 1 calc R . H18B H 0.2065(4) 0.1725(3) 0.9921(4) 0.041(3) Uiso 1 calc R . C19 C 0.3135(5) 0.0407(4) 1.0388(4) 0.0422(13) Uani 1 d . . H19A H 0.3009(30) -0.0015(8) 1.0144(19) 0.065(5) Uiso 1 calc R . H19B H 0.2721(23) 0.0415(6) 1.1043(6) 0.065(5) Uiso 1 calc R . H19C H 0.3875(9) 0.0150(12) 1.0331(24) 0.065(5) Uiso 1 calc R . C20 C 0.2529(4) 0.2286(4) 1.1090(4) 0.0355(12) Uani 1 d . . H20A H 0.2661(4) 0.2800(4) 1.1205(4) 0.041(3) Uiso 1 calc R . H20B H 0.2859(4) 0.1655(4) 1.1464(4) 0.041(3) Uiso 1 calc R . C21 C 0.1343(5) 0.2539(5) 1.1437(4) 0.0450(14) Uani 1 d . . H21A H 0.1060(7) 0.2648(30) 1.2081(10) 0.065(5) Uiso 1 calc R . H21B H 0.1205(5) 0.1993(13) 1.1408(27) 0.065(5) Uiso 1 calc R . H21C H 0.1012(6) 0.3136(18) 1.1042(18) 0.065(5) Uiso 1 calc R . C22 C 0.1718(4) 0.5668(4) 0.9593(4) 0.0392(12) Uani 1 d . . H22A H 0.1950(4) 0.6190(4) 0.9542(4) 0.041(3) Uiso 1 calc R . H22B H 0.0989(4) 0.5990(4) 0.9584(4) 0.041(3) Uiso 1 calc R . C23 C 0.1748(4) 0.4988(4) 1.0520(4) 0.0460(14) Uani 1 d . . H23A H 0.1269(24) 0.5361(8) 1.1025(4) 0.065(5) Uiso 1 calc R . H23B H 0.2455(8) 0.4708(23) 1.0561(12) 0.065(5) Uiso 1 calc R . H23C H 0.1538(30) 0.4457(17) 1.0573(12) 0.065(5) Uiso 1 calc R . C24 C 0.1839(4) 0.5637(4) 0.8014(4) 0.0372(12) Uani 1 d . . H24A H 0.1163(4) 0.5554(4) 0.8279(4) 0.041(3) Uiso 1 calc R . H24B H 0.2259(4) 0.5273(4) 0.7488(4) 0.041(3) Uiso 1 calc R . C25 C 0.1633(5) 0.6749(4) 0.7623(5) 0.058(2) Uani 1 d . . H25A H 0.1222(28) 0.6992(8) 0.7197(23) 0.065(5) Uiso 1 calc R . H25B H 0.2298(6) 0.6836(5) 0.7289(25) 0.065(5) Uiso 1 calc R . H25C H 0.1251(28) 0.7118(6) 0.8138(6) 0.065(5) Uiso 1 calc R . B1 B 0.5163(4) 0.2213(4) 1.2373(4) 0.0241(10) Uani 1 d . . C60 C 0.4465(4) 0.3827(3) 1.3153(3) 0.0252(9) Uani 1 d . . H60 H 0.5037(4) 0.3501(3) 1.3392(3) 0.038(3) Uiso 1 calc R . C61 C 0.3795(4) 0.4803(4) 1.3302(3) 0.0306(11) Uani 1 d . . H61 H 0.3929(4) 0.5116(4) 1.3631(3) 0.038(3) Uiso 1 calc R . C62 C 0.2933(4) 0.5307(3) 1.2965(3) 0.0316(11) Uani 1 d . . H62 H 0.2487(4) 0.5960(3) 1.3061(3) 0.038(3) Uiso 1 calc R . C63 C 0.2742(4) 0.4829(3) 1.2481(3) 0.0296(10) Uani 1 d . . H63 H 0.2156(4) 0.5154(3) 1.2261(3) 0.038(3) Uiso 1 calc R . C64 C 0.3427(4) 0.3863(3) 1.2325(3) 0.0263(10) Uani 1 d . . H64 H 0.3292(4) 0.3562(3) 1.1984(3) 0.038(3) Uiso 1 calc R . C65 C 0.4312(3) 0.3315(3) 1.2654(3) 0.0232(9) Uani 1 d . . C66 C 0.6836(4) 0.1624(4) 1.0855(4) 0.0306(10) Uani 1 d . . H66 H 0.6992(4) 0.0979(4) 1.1210(4) 0.038(3) Uiso 1 calc R . C67 C 0.7508(4) 0.1767(4) 0.9944(4) 0.0350(11) Uani 1 d . . H67 H 0.8083(4) 0.1221(4) 0.9696(4) 0.038(3) Uiso 1 calc R . C68 C 0.7329(4) 0.2721(4) 0.9398(4) 0.0351(11) Uani 1 d . . H68 H 0.7781(4) 0.2826(4) 0.8788(4) 0.038(3) Uiso 1 calc R . C69 C 0.6460(4) 0.3510(4) 0.9788(3) 0.0292(10) Uani 1 d . . H69 H 0.6326(4) 0.4157(4) 0.9438(3) 0.038(3) Uiso 1 calc R . C70 C 0.5783(4) 0.3351(3) 1.0694(3) 0.0257(10) Uani 1 d . . H70 H 0.5203(4) 0.3901(3) 1.0930(3) 0.038(3) Uiso 1 calc R . C71 C 0.5931(3) 0.2403(3) 1.1271(3) 0.0235(9) Uani 1 d . . C72 C 0.5518(4) 0.1149(3) 1.4014(3) 0.0286(10) Uani 1 d . . H72 H 0.4861(4) 0.1102(3) 1.4197(3) 0.038(3) Uiso 1 calc R . C73 C 0.6084(4) 0.0724(3) 1.4657(3) 0.0300(11) Uani 1 d . . H73 H 0.5800(4) 0.0403(3) 1.5258(3) 0.038(3) Uiso 1 calc R . C74 C 0.7065(4) 0.0768(4) 1.4419(4) 0.0363(12) Uani 1 d . . H74 H 0.7445(4) 0.0486(4) 1.4852(4) 0.038(3) Uiso 1 calc R . C75 C 0.7466(4) 0.1244(4) 1.3519(4) 0.0397(13) Uani 1 d . . H75 H 0.8128(4) 0.1279(4) 1.3340(4) 0.038(3) Uiso 1 calc R . C76 C 0.6892(4) 0.1672(4) 1.2874(4) 0.0320(11) Uani 1 d . . H76 H 0.7184(4) 0.1985(4) 1.2273(4) 0.038(3) Uiso 1 calc R . C77 C 0.5891(4) 0.1648(3) 1.3100(3) 0.0252(10) Uani 1 d . . C78 C 0.3501(4) 0.1645(3) 1.3153(3) 0.0261(10) Uani 1 d . . H78 H 0.3140(4) 0.2207(3) 1.3443(3) 0.038(3) Uiso 1 calc R . C79 C 0.2994(4) 0.0993(4) 1.3362(3) 0.0310(11) Uani 1 d . . H79 H 0.2307(4) 0.1131(4) 1.3779(3) 0.038(3) Uiso 1 calc R . C80 C 0.3502(4) 0.0133(4) 1.2952(4) 0.0335(11) Uani 1 d . . H80 H 0.3169(4) -0.0311(4) 1.3093(4) 0.038(3) Uiso 1 calc R . C81 C 0.4519(4) -0.0037(4) 1.2328(4) 0.0338(11) Uani 1 d . . H81 H 0.4878(4) -0.0605(4) 1.2045(4) 0.038(3) Uiso 1 calc R . C82 C 0.5012(4) 0.0632(3) 1.2117(3) 0.0302(10) Uani 1 d . . H82 H 0.5691(4) 0.0498(3) 1.1685(3) 0.038(3) Uiso 1 calc R . C83 C 0.4535(4) 0.1497(3) 1.2523(3) 0.0222(9) Uani 1 d . . O1 O -0.0118(28) 0.1050(26) 0.6318(28) 0.063(8) Uiso 0.15 d P 1 C50 C -0.0095(30) 0.0326(31) 0.5972(26) 0.035(8) Uiso 0.15 d P 1 C51 C -0.0618(35) -0.0219(34) 0.6800(34) 0.050(10) Uiso 0.15 d P 1 C52 C -0.0685(47) 0.0086(44) 0.7465(42) 0.076(15) Uiso 0.15 d P 1 C53 C -0.0482(46) 0.0870(44) 0.7010(41) 0.061(13) Uiso 0.15 d P 1 O1X O -0.0788(30) 0.1387(30) 0.6880(27) 0.066(9) Uiso 0.15 d P 2 C50X C -0.0131(33) 0.0864(36) 0.5930(31) 0.044(9) Uiso 0.15 d P 2 C51X C -0.0634(40) 0.0126(37) 0.6302(38) 0.056(11) Uiso 0.15 d P 2 C52X C -0.1252(46) 0.0342(43) 0.7138(40) 0.072(14) Uiso 0.15 d P 2 C53X C -0.1148(40) 0.0935(36) 0.7409(34) 0.056(11) Uiso 0.15 d P 2 O2 O 0.5982(6) 0.4143(6) 0.5233(6) 0.043(2) Uani 0.50 d P . C54 C 0.7668(12) 0.2734(13) 0.5290(13) 0.082(5) Uani 0.50 d P . C55 C 0.6859(11) 0.3460(11) 0.4675(10) 0.059(3) Uani 0.50 d P . C56 C 0.5200(12) 0.4715(12) 0.4788(10) 0.045(3) Uani 0.50 d P . C57 C 0.4231(12) 0.5400(14) 0.5454(13) 0.055(4) Uani 0.50 d P . 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 Ni1 0.0191(3) 0.0211(3) 0.0232(3) -0.0056(2) -0.0073(2) -0.0060(2) Ni2 0.0206(3) 0.0245(3) 0.0285(3) -0.0108(2) -0.0096(2) -0.0025(2) Cl1 0.0202(5) 0.0257(5) 0.0259(5) -0.0063(4) -0.0061(4) -0.0080(4) Cl2 0.0254(6) 0.0252(6) 0.0483(7) -0.0076(5) -0.0174(5) -0.0058(5) S1 0.0312(6) 0.0365(7) 0.0285(6) -0.0025(5) -0.0123(5) -0.0141(5) S2 0.0432(8) 0.0229(6) 0.0596(9) -0.0141(6) -0.0329(7) 0.0003(5) N1 0.019(2) 0.026(2) 0.020(2) -0.0048(15) -0.0077(15) -0.006(2) N2 0.017(2) 0.034(2) 0.026(2) -0.015(2) -0.004(2) -0.004(2) N3 0.034(2) 0.049(3) 0.040(3) -0.027(2) -0.018(2) 0.003(2) N4 0.024(2) 0.026(2) 0.031(2) -0.009(2) -0.010(2) -0.007(2) N5 0.024(2) 0.024(2) 0.038(2) -0.006(2) -0.011(2) -0.009(2) N6 0.025(2) 0.025(2) 0.026(2) -0.004(2) -0.012(2) -0.006(2) C1 0.018(2) 0.023(2) 0.029(2) -0.004(2) -0.003(2) -0.004(2) C2 0.017(2) 0.039(3) 0.030(3) -0.011(2) 0.000(2) -0.003(2) C3 0.022(2) 0.041(3) 0.024(2) -0.013(2) -0.005(2) -0.001(2) C4 0.029(3) 0.083(5) 0.039(3) -0.037(3) -0.008(2) 0.003(3) C5 0.037(3) 0.066(4) 0.027(3) -0.020(3) -0.016(2) -0.001(3) C6 0.045(3) 0.059(4) 0.028(3) -0.011(3) -0.003(2) -0.017(3) C7 0.054(4) 0.050(4) 0.058(4) -0.040(3) -0.030(3) 0.009(3) C8 0.070(4) 0.036(3) 0.079(5) -0.035(3) -0.050(4) 0.015(3) C9 0.022(2) 0.035(3) 0.038(3) -0.009(2) -0.007(2) -0.011(2) C10 0.025(2) 0.031(3) 0.040(3) -0.010(2) -0.012(2) -0.012(2) C11 0.028(2) 0.027(2) 0.035(3) -0.003(2) -0.013(2) -0.012(2) C12 0.033(3) 0.032(3) 0.051(3) -0.004(2) -0.016(3) -0.011(2) C13 0.058(4) 0.041(3) 0.056(4) 0.001(3) -0.031(3) -0.011(3) C14 0.069(4) 0.021(3) 0.111(6) 0.008(3) -0.065(4) -0.018(3) C15 0.062(4) 0.053(4) 0.095(6) 0.015(4) -0.033(4) -0.038(4) C16 0.024(2) 0.032(3) 0.047(3) -0.007(2) -0.019(2) -0.008(2) C17 0.030(3) 0.026(2) 0.034(3) -0.003(2) -0.020(2) -0.005(2) C18 0.032(3) 0.024(2) 0.037(3) -0.005(2) -0.014(2) -0.009(2) C19 0.050(3) 0.026(3) 0.054(3) -0.001(2) -0.025(3) -0.013(2) C20 0.044(3) 0.031(3) 0.032(3) -0.007(2) -0.014(2) -0.010(2) C21 0.047(3) 0.051(3) 0.030(3) -0.011(3) -0.005(2) -0.016(3) C22 0.030(3) 0.027(3) 0.052(3) -0.016(2) -0.005(2) -0.004(2) C23 0.034(3) 0.051(3) 0.045(3) -0.028(3) -0.014(3) 0.006(3) C24 0.038(3) 0.029(3) 0.053(3) 0.009(2) -0.028(3) -0.017(2) C25 0.068(4) 0.034(3) 0.089(5) 0.020(3) -0.054(4) -0.028(3) B1 0.027(3) 0.019(2) 0.027(3) -0.006(2) -0.007(2) -0.008(2) C60 0.023(2) 0.024(2) 0.027(2) -0.005(2) -0.007(2) -0.008(2) C61 0.040(3) 0.026(2) 0.026(2) -0.005(2) -0.008(2) -0.013(2) C62 0.037(3) 0.019(2) 0.029(3) -0.001(2) -0.006(2) -0.008(2) C63 0.025(2) 0.026(2) 0.030(2) 0.000(2) -0.010(2) -0.005(2) C64 0.030(2) 0.025(2) 0.028(2) -0.002(2) -0.015(2) -0.010(2) C65 0.024(2) 0.019(2) 0.023(2) -0.001(2) -0.005(2) -0.009(2) C66 0.027(2) 0.025(2) 0.035(3) -0.003(2) -0.013(2) -0.005(2) C67 0.023(2) 0.035(3) 0.040(3) -0.011(2) -0.004(2) -0.007(2) C68 0.033(3) 0.045(3) 0.027(3) -0.005(2) -0.004(2) -0.021(2) C69 0.039(3) 0.027(2) 0.030(2) 0.003(2) -0.017(2) -0.019(2) C70 0.028(2) 0.022(2) 0.029(2) -0.003(2) -0.012(2) -0.009(2) C71 0.023(2) 0.022(2) 0.029(2) -0.004(2) -0.013(2) -0.008(2) C72 0.027(2) 0.026(2) 0.029(2) -0.010(2) -0.006(2) -0.006(2) C73 0.041(3) 0.024(2) 0.022(2) 0.001(2) -0.016(2) -0.007(2) C74 0.048(3) 0.028(3) 0.041(3) 0.001(2) -0.032(3) -0.010(2) C75 0.040(3) 0.036(3) 0.054(3) 0.010(2) -0.031(3) -0.020(2) C76 0.042(3) 0.030(3) 0.032(3) 0.009(2) -0.024(2) -0.020(2) C77 0.030(2) 0.017(2) 0.031(2) -0.007(2) -0.011(2) -0.007(2) C78 0.031(2) 0.026(2) 0.024(2) -0.003(2) -0.016(2) -0.007(2) C79 0.033(3) 0.035(3) 0.026(2) 0.001(2) -0.011(2) -0.017(2) C80 0.047(3) 0.030(3) 0.035(3) 0.006(2) -0.022(2) -0.023(2) C81 0.048(3) 0.022(2) 0.036(3) -0.003(2) -0.020(2) -0.012(2) C82 0.034(3) 0.024(2) 0.031(3) -0.002(2) -0.012(2) -0.010(2) C83 0.028(2) 0.025(2) 0.017(2) 0.001(2) -0.018(2) -0.006(2) O2 0.049(5) 0.046(5) 0.042(5) -0.013(4) -0.014(4) -0.022(4) C54 0.052(9) 0.090(12) 0.104(13) -0.050(10) 0.016(9) -0.038(9) C55 0.049(8) 0.059(8) 0.061(8) -0.023(7) -0.002(6) -0.019(7) C56 0.059(10) 0.038(8) 0.027(8) -0.003(5) -0.016(8) -0.007(9) C57 0.043(9) 0.060(9) 0.055(11) -0.031(8) -0.010(9) -0.004(9) _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 Ni1 N1 1.936(4) . ? Ni1 N5 2.125(4) . ? Ni1 N6 2.145(4) . ? Ni1 N4 2.156(4) . ? Ni1 Cl1 2.3972(12) . ? Ni2 N2 1.986(4) . ? Ni2 N3 2.185(4) . ? Ni2 Cl2 2.3242(13) . ? Ni2 S2 2.4756(14) . ? Ni2 S1 2.5029(14) . ? Ni2 Cl1 2.5600(12) . ? S1 C6 1.804(6) . ? S1 C12 1.815(5) . ? S2 C14 1.808(6) . ? S2 C8 1.820(6) . ? N1 C1 1.341(6) . ? N1 N2 1.358(5) . ? N2 C3 1.336(6) . ? N3 C7 1.487(8) . ? N3 C5 1.500(7) . ? N3 C4 1.508(7) . ? N4 C16 1.478(6) . ? N4 C10 1.483(6) . ? N4 C9 1.496(6) . ? N5 C24 1.475(6) . ? N5 C11 1.484(6) . ? N5 C22 1.490(6) . ? N6 C18 1.497(6) . ? N6 C20 1.498(6) . ? N6 C17 1.508(6) . ? C1 C2 1.393(7) . ? C1 C9 1.508(7) . ? C2 C3 1.381(7) . ? C2 H2 0.93 . ? C3 C4 1.491(7) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.510(9) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.509(8) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 C11 1.511(6) . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C11 H11A 0.97 . ? C11 H11B 0.97 . ? C12 C13 1.517(8) . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C13 H13C 0.96 . ? C14 C15 1.536(10) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C16 C17 1.501(7) . ? C16 H16A 0.97 . ? C16 H16B 0.97 . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C18 C19 1.518(7) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? C20 C21 1.516(8) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 C23 1.485(8) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 C25 1.525(7) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? B1 C83 1.641(7) . ? B1 C65 1.644(6) . ? B1 C77 1.651(7) . ? B1 C71 1.654(7) . ? C60 C61 1.392(6) . ? C60 C65 1.405(6) . ? C60 H60 0.93 . ? C61 C62 1.379(7) . ? C61 H61 0.93 . ? C62 C63 1.382(7) . ? C62 H62 0.93 . ? C63 C64 1.386(6) . ? C63 H63 0.93 . ? C64 C65 1.403(6) . ? C64 H64 0.93 . ? C66 C67 1.384(7) . ? C66 C71 1.407(6) . ? C66 H66 0.93 . ? C67 C68 1.387(7) . ? C67 H67 0.93 . ? C68 C69 1.382(7) . ? C68 H68 0.93 . ? C69 C70 1.385(7) . ? C69 H69 0.93 . ? C70 C71 1.400(6) . ? C70 H70 0.93 . ? C72 C73 1.382(6) . ? C72 C77 1.399(7) . ? C72 H72 0.93 . ? C73 C74 1.380(7) . ? C73 H73 0.93 . ? C74 C75 1.381(8) . ? C74 H74 0.93 . ? C75 C76 1.392(7) . ? C75 H75 0.93 . ? C76 C77 1.398(7) . ? C76 H76 0.93 . ? C78 C79 1.390(7) . ? C78 C83 1.409(6) . ? C78 H78 0.93 . ? C79 C80 1.395(7) . ? C79 H79 0.93 . ? C80 C81 1.384(7) . ? C80 H80 0.93 . ? C81 C82 1.395(7) . ? C81 H81 0.93 . ? C82 C83 1.403(6) . ? C82 H82 0.93 . ? O1 C53 1.00(6) . ? O1 C50 1.36(5) . ? C50 C51 1.43(6) . ? C50 C53 1.83(7) . ? C50 C52 2.11(7) . ? C51 C52 1.23(7) . ? C51 C53 1.90(7) . ? C52 C53 1.27(8) . ? O1X C53X 1.02(6) . ? O1X C50X 1.64(6) . ? O1X C52X 1.87(7) . ? C50X C51X 1.46(7) . ? C51X C52X 1.30(7) . ? C52X C53X 1.20(7) . ? O2 C57 1.15(2) 2_666 ? O2 C56 1.39(2) . ? O2 C55 1.405(15) . ? O2 C56 1.83(2) 2_666 ? C54 C55 1.62(2) . ? C55 C57 1.77(2) 2_666 ? C56 C57 0.73(2) 2_666 ? C56 C56 1.06(3) 2_666 ? C56 C57 1.54(2) . ? C56 O2 1.83(2) 2_666 ? C57 C56 0.73(2) 2_666 ? C57 O2 1.15(2) 2_666 ? C57 C55 1.77(2) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N5 102.2(2) . . ? N1 Ni1 N6 102.38(15) . . ? N5 Ni1 N6 150.62(15) . . ? N1 Ni1 N4 80.57(15) . . ? N5 Ni1 N4 84.08(14) . . ? N6 Ni1 N4 84.38(15) . . ? N1 Ni1 Cl1 89.67(11) . . ? N5 Ni1 Cl1 98.05(11) . . ? N6 Ni1 Cl1 97.87(11) . . ? N4 Ni1 Cl1 170.25(11) . . ? N2 Ni2 N3 78.8(2) . . ? N2 Ni2 Cl2 175.36(11) . . ? N3 Ni2 Cl2 96.61(12) . . ? N2 Ni2 S2 88.85(12) . . ? N3 Ni2 S2 84.20(14) . . ? Cl2 Ni2 S2 91.13(5) . . ? N2 Ni2 S1 88.75(12) . . ? N3 Ni2 S1 84.49(13) . . ? Cl2 Ni2 S1 90.37(5) . . ? S2 Ni2 S1 168.68(5) . . ? N2 Ni2 Cl1 85.61(11) . . ? N3 Ni2 Cl1 164.37(12) . . ? Cl2 Ni2 Cl1 99.01(5) . . ? S2 Ni2 Cl1 96.12(5) . . ? S1 Ni2 Cl1 94.72(4) . . ? Ni1 Cl1 Ni2 103.82(4) . . ? C6 S1 C12 101.8(3) . . ? C6 S1 Ni2 95.4(2) . . ? C12 S1 Ni2 112.4(2) . . ? C14 S2 C8 102.0(3) . . ? C14 S2 Ni2 111.5(2) . . ? C8 S2 Ni2 96.1(2) . . ? C1 N1 N2 108.2(4) . . ? C1 N1 Ni1 121.4(3) . . ? N2 N1 Ni1 130.5(3) . . ? C3 N2 N1 107.9(4) . . ? C3 N2 Ni2 121.7(3) . . ? N1 N2 Ni2 130.4(3) . . ? C7 N3 C5 110.7(4) . . ? C7 N3 C4 111.4(5) . . ? C5 N3 C4 109.5(5) . . ? C7 N3 Ni2 106.4(4) . . ? C5 N3 Ni2 107.4(3) . . ? C4 N3 Ni2 111.3(3) . . ? C16 N4 C10 113.6(4) . . ? C16 N4 C9 110.9(4) . . ? C10 N4 C9 110.8(4) . . ? C16 N4 Ni1 104.9(3) . . ? C10 N4 Ni1 105.8(3) . . ? C9 N4 Ni1 110.5(3) . . ? C24 N5 C11 109.6(4) . . ? C24 N5 C22 109.5(4) . . ? C11 N5 C22 111.6(4) . . ? C24 N5 Ni1 109.5(3) . . ? C11 N5 Ni1 105.5(3) . . ? C22 N5 Ni1 111.1(3) . . ? C18 N6 C20 111.1(4) . . ? C18 N6 C17 109.0(4) . . ? C20 N6 C17 107.9(4) . . ? C18 N6 Ni1 110.4(3) . . ? C20 N6 Ni1 114.1(3) . . ? C17 N6 Ni1 104.0(3) . . ? N1 C1 C2 109.5(4) . . ? N1 C1 C9 116.0(4) . . ? C2 C1 C9 134.5(4) . . ? C3 C2 C1 104.0(4) . . ? C3 C2 H2 128.0(3) . . ? C1 C2 H2 128.0(3) . . ? N2 C3 C2 110.4(4) . . ? N2 C3 C4 116.9(4) . . ? C2 C3 C4 132.7(4) . . ? C3 C4 N3 111.3(4) . . ? C3 C4 H4A 109.4(3) . . ? N3 C4 H4A 109.4(3) . . ? C3 C4 H4B 109.4(4) . . ? N3 C4 H4B 109.4(3) . . ? H4A C4 H4B 108.0 . . ? N3 C5 C6 111.8(4) . . ? N3 C5 H5A 109.3(3) . . ? C6 C5 H5A 109.3(3) . . ? N3 C5 H5B 109.3(3) . . ? C6 C5 H5B 109.3(3) . . ? H5A C5 H5B 107.9 . . ? C5 C6 S1 113.3(4) . . ? C5 C6 H6A 108.9(3) . . ? S1 C6 H6A 108.9(2) . . ? C5 C6 H6B 108.9(3) . . ? S1 C6 H6B 108.9(2) . . ? H6A C6 H6B 107.7 . . ? N3 C7 C8 112.2(5) . . ? N3 C7 H7A 109.2(3) . . ? C8 C7 H7A 109.2(3) . . ? N3 C7 H7B 109.2(3) . . ? C8 C7 H7B 109.2(4) . . ? H7A C7 H7B 107.9 . . ? C7 C8 S2 113.7(4) . . ? C7 C8 H8A 108.8(4) . . ? S2 C8 H8A 108.8(2) . . ? C7 C8 H8B 108.8(3) . . ? S2 C8 H8B 108.8(2) . . ? H8A C8 H8B 107.7 . . ? N4 C9 C1 111.6(4) . . ? N4 C9 H9A 109.3(2) . . ? C1 C9 H9A 109.3(3) . . ? N4 C9 H9B 109.3(2) . . ? C1 C9 H9B 109.3(3) . . ? H9A C9 H9B 108.0 . . ? N4 C10 C11 109.2(4) . . ? N4 C10 H10A 109.8(2) . . ? C11 C10 H10A 109.9(3) . . ? N4 C10 H10B 109.9(3) . . ? C11 C10 H10B 109.9(3) . . ? H10A C10 H10B 108.3 . . ? N5 C11 C10 111.9(4) . . ? N5 C11 H11A 109.2(2) . . ? C10 C11 H11A 109.2(2) . . ? N5 C11 H11B 109.2(2) . . ? C10 C11 H11B 109.2(3) . . ? H11A C11 H11B 107.9 . . ? C13 C12 S1 112.9(4) . . ? C13 C12 H12A 109.0(3) . . ? S1 C12 H12A 109.0(2) . . ? C13 C12 H12B 109.0(3) . . ? S1 C12 H12B 109.0(2) . . ? H12A C12 H12B 107.8 . . ? C12 C13 H13A 109.5(3) . . ? C12 C13 H13B 109.5(3) . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5(3) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 S2 107.9(4) . . ? C15 C14 H14A 110.1(3) . . ? S2 C14 H14A 110.1(2) . . ? C15 C14 H14B 110.1(3) . . ? S2 C14 H14B 110.1(2) . . ? H14A C14 H14B 108.4 . . ? C14 C15 H15A 109.5(3) . . ? C14 C15 H15B 109.5(3) . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5(3) . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 108.9(4) . . ? N4 C16 H16A 109.9(2) . . ? C17 C16 H16A 109.9(3) . . ? N4 C16 H16B 109.9(2) . . ? C17 C16 H16B 109.9(3) . . ? H16A C16 H16B 108.3 . . ? C16 C17 N6 111.6(4) . . ? C16 C17 H17A 109.3(3) . . ? N6 C17 H17A 109.3(2) . . ? C16 C17 H17B 109.3(3) . . ? N6 C17 H17B 109.3(2) . . ? H17A C17 H17B 108.0 . . ? N6 C18 C19 116.3(4) . . ? N6 C18 H18A 108.2(2) . . ? C19 C18 H18A 108.2(3) . . ? N6 C18 H18B 108.2(2) . . ? C19 C18 H18B 108.2(3) . . ? H18A C18 H18B 107.4 . . ? C18 C19 H19A 109.5(3) . . ? C18 C19 H19B 109.5(3) . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5(3) . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N6 C20 C21 115.0(4) . . ? N6 C20 H20A 108.5(3) . . ? C21 C20 H20A 108.5(3) . . ? N6 C20 H20B 108.5(2) . . ? C21 C20 H20B 108.5(3) . . ? H20A C20 H20B 107.5 . . ? C20 C21 H21A 109.5(3) . . ? C20 C21 H21B 109.5(3) . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5(3) . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 N5 114.9(4) . . ? C23 C22 H22A 108.5(3) . . ? N5 C22 H22A 108.5(3) . . ? C23 C22 H22B 108.5(3) . . ? N5 C22 H22B 108.5(3) . . ? H22A C22 H22B 107.5 . . ? C22 C23 H23A 109.5(3) . . ? C22 C23 H23B 109.5(3) . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5(3) . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 C25 116.2(4) . . ? N5 C24 H24A 108.2(3) . . ? C25 C24 H24A 108.2(3) . . ? N5 C24 H24B 108.2(3) . . ? C25 C24 H24B 108.2(4) . . ? H24A C24 H24B 107.4 . . ? C24 C25 H25A 109.5(3) . . ? C24 C25 H25B 109.5(3) . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5(4) . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C83 B1 C65 110.4(4) . . ? C83 B1 C77 106.9(3) . . ? C65 B1 C77 108.8(4) . . ? C83 B1 C71 113.3(4) . . ? C65 B1 C71 107.7(4) . . ? C77 B1 C71 109.7(4) . . ? C61 C60 C65 122.7(4) . . ? C61 C60 H60 118.7(3) . . ? C65 C60 H60 118.7(3) . . ? C62 C61 C60 120.3(4) . . ? C62 C61 H61 119.8(3) . . ? C60 C61 H61 119.8(3) . . ? C61 C62 C63 119.1(4) . . ? C61 C62 H62 120.4(3) . . ? C63 C62 H62 120.4(3) . . ? C62 C63 C64 119.9(4) . . ? C62 C63 H63 120.1(3) . . ? C64 C63 H63 120.1(3) . . ? C63 C64 C65 123.3(4) . . ? C63 C64 H64 118.3(3) . . ? C65 C64 H64 118.3(3) . . ? C64 C65 C60 114.7(4) . . ? C64 C65 B1 121.7(4) . . ? C60 C65 B1 123.3(4) . . ? C67 C66 C71 123.5(5) . . ? C67 C66 H66 118.3(3) . . ? C71 C66 H66 118.3(3) . . ? C66 C67 C68 120.4(5) . . ? C66 C67 H67 119.8(3) . . ? C68 C67 H67 119.8(3) . . ? C69 C68 C67 118.0(5) . . ? C69 C68 H68 121.0(3) . . ? C67 C68 H68 121.0(3) . . ? C68 C69 C70 121.0(4) . . ? C68 C69 H69 119.5(3) . . ? C70 C69 H69 119.5(3) . . ? C69 C70 C71 123.2(4) . . ? C69 C70 H70 118.4(3) . . ? C71 C70 H70 118.4(3) . . ? C70 C71 C66 114.1(4) . . ? C70 C71 B1 123.6(4) . . ? C66 C71 B1 122.2(4) . . ? C73 C72 C77 122.8(5) . . ? C73 C72 H72 118.6(3) . . ? C77 C72 H72 118.6(3) . . ? C74 C73 C72 120.9(5) . . ? C74 C73 H73 119.6(3) . . ? C72 C73 H73 119.6(3) . . ? C73 C74 C75 118.0(4) . . ? C73 C74 H74 121.0(3) . . ? C75 C74 H74 121.0(3) . . ? C74 C75 C76 120.8(5) . . ? C74 C75 H75 119.6(3) . . ? C76 C75 H75 119.6(3) . . ? C75 C76 C77 122.4(5) . . ? C75 C76 H76 118.8(3) . . ? C77 C76 H76 118.8(3) . . ? C76 C77 C72 115.1(4) . . ? C76 C77 B1 123.2(4) . . ? C72 C77 B1 121.7(4) . . ? C79 C78 C83 123.3(4) . . ? C79 C78 H78 118.3(3) . . ? C83 C78 H78 118.3(3) . . ? C78 C79 C80 120.7(5) . . ? C78 C79 H79 119.6(3) . . ? C80 C79 H79 119.6(3) . . ? C81 C80 C79 117.6(4) . . ? C81 C80 H80 121.2(3) . . ? C79 C80 H80 121.2(3) . . ? C80 C81 C82 120.9(5) . . ? C80 C81 H81 119.6(3) . . ? C82 C81 H81 119.6(3) . . ? C81 C82 C83 123.3(5) . . ? C81 C82 H82 118.3(3) . . ? C83 C82 H82 118.3(3) . . ? C82 C83 C78 114.1(4) . . ? C82 C83 B1 123.3(4) . . ? C78 C83 B1 122.3(4) . . ? C53 O1 C50 100.5(46) . . ? O1 C50 C51 102.8(33) . . ? O1 C50 C53 32.6(23) . . ? C51 C50 C53 70.1(29) . . ? O1 C50 C52 69.2(26) . . ? C51 C50 C52 34.2(24) . . ? C53 C50 C52 36.8(24) . . ? C52 C51 C50 104.9(44) . . ? C52 C51 C53 41.3(34) . . ? C50 C51 C53 64.9(28) . . ? C51 C52 C53 99.1(53) . . ? C51 C52 C50 40.9(30) . . ? C53 C52 C50 59.7(36) . . ? O1 C53 C52 129.7(64) . . ? O1 C53 C50 46.9(34) . . ? C52 C53 C50 83.5(41) . . ? O1 C53 C51 91.8(45) . . ? C52 C53 C51 39.6(33) . . ? C50 C53 C51 44.9(23) . . ? C53X O1X C50X 109.2(43) . . ? C53X O1X C52X 35.8(34) . . ? C50X O1X C52X 75.3(27) . . ? C51X C50X O1X 93.5(32) . . ? C52X C51X C50X 102.2(44) . . ? C53X C52X C51X 117.0(55) . . ? C53X C52X O1X 29.8(29) . . ? C51X C52X O1X 88.9(39) . . ? O1X C53X C52X 114.4(55) . . ? C57 O2 C56 31.7(8) 2_666 . ? C57 O2 C55 87.2(11) 2_666 . ? C56 O2 C55 111.3(11) . . ? C57 O2 C56 57.0(9) 2_666 2_666 ? C56 O2 C56 35.5(12) . 2_666 ? C55 O2 C56 144.1(9) . 2_666 ? O2 C55 C54 108.4(11) . . ? O2 C55 C57 40.5(7) . 2_666 ? C54 C55 C57 146.8(12) . 2_666 ? C57 C56 C56 116.7(39) 2_666 2_666 ? C57 C56 O2 55.9(21) 2_666 . ? C56 C56 O2 95.1(19) 2_666 . ? C57 C56 C57 141.8(27) 2_666 . ? C56 C56 C57 25.2(14) 2_666 . ? O2 C56 C57 109.2(9) . . ? C57 C56 O2 133.6(27) 2_666 2_666 ? C56 C56 O2 49.4(13) 2_666 2_666 ? O2 C56 O2 144.5(12) . 2_666 ? C57 C56 O2 38.9(8) . 2_666 ? C56 C57 O2 92.4(25) 2_666 2_666 ? C56 C57 C56 38.2(27) 2_666 . ? O2 C57 C56 84.1(10) 2_666 . ? C56 C57 C55 129.3(28) 2_666 2_666 ? O2 C57 C55 52.3(9) 2_666 2_666 ? C56 C57 C55 136.3(12) . 2_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 Cl1 Ni2 0.49(11) . . . . ? N5 Ni1 Cl1 Ni2 102.81(12) . . . . ? N6 Ni1 Cl1 Ni2 -101.97(11) . . . . ? N4 Ni1 Cl1 Ni2 0.8(7) . . . . ? N2 Ni2 Cl1 Ni1 -0.49(12) . . . . ? N3 Ni2 Cl1 Ni1 -2.5(5) . . . . ? Cl2 Ni2 Cl1 Ni1 179.99(5) . . . . ? S2 Ni2 Cl1 Ni1 87.87(5) . . . . ? S1 Ni2 Cl1 Ni1 -88.88(5) . . . . ? N2 Ni2 S1 C6 79.2(2) . . . . ? N3 Ni2 S1 C6 0.4(2) . . . . ? Cl2 Ni2 S1 C6 -96.2(2) . . . . ? S2 Ni2 S1 C6 1.4(3) . . . . ? Cl1 Ni2 S1 C6 164.7(2) . . . . ? N2 Ni2 S1 C12 -175.6(2) . . . . ? N3 Ni2 S1 C12 105.6(2) . . . . ? Cl2 Ni2 S1 C12 9.0(2) . . . . ? S2 Ni2 S1 C12 106.6(3) . . . . ? Cl1 Ni2 S1 C12 -90.1(2) . . . . ? N2 Ni2 S2 C14 168.6(3) . . . . ? N3 Ni2 S2 C14 -112.6(3) . . . . ? Cl2 Ni2 S2 C14 -16.0(3) . . . . ? S1 Ni2 S2 C14 -113.6(4) . . . . ? Cl1 Ni2 S2 C14 83.2(3) . . . . ? N2 Ni2 S2 C8 -85.9(3) . . . . ? N3 Ni2 S2 C8 -7.1(3) . . . . ? Cl2 Ni2 S2 C8 89.5(2) . . . . ? S1 Ni2 S2 C8 -8.1(4) . . . . ? Cl1 Ni2 S2 C8 -171.4(2) . . . . ? N5 Ni1 N1 C1 83.5(4) . . . . ? N6 Ni1 N1 C1 -80.4(4) . . . . ? N4 Ni1 N1 C1 1.7(3) . . . . ? Cl1 Ni1 N1 C1 -178.3(3) . . . . ? N5 Ni1 N1 N2 -98.6(4) . . . . ? N6 Ni1 N1 N2 97.6(4) . . . . ? N4 Ni1 N1 N2 179.7(4) . . . . ? Cl1 Ni1 N1 N2 -0.4(4) . . . . ? C1 N1 N2 C3 -0.6(5) . . . . ? Ni1 N1 N2 C3 -178.7(3) . . . . ? C1 N1 N2 Ni2 178.1(3) . . . . ? Ni1 N1 N2 Ni2 0.0(6) . . . . ? N3 Ni2 N2 C3 -1.6(4) . . . . ? Cl2 Ni2 N2 C3 -7.0(18) . . . . ? S2 Ni2 N2 C3 82.7(4) . . . . ? S1 Ni2 N2 C3 -86.2(4) . . . . ? Cl1 Ni2 N2 C3 179.0(4) . . . . ? N3 Ni2 N2 N1 179.9(4) . . . . ? Cl2 Ni2 N2 N1 174.4(12) . . . . ? S2 Ni2 N2 N1 -95.8(4) . . . . ? S1 Ni2 N2 N1 95.2(4) . . . . ? Cl1 Ni2 N2 N1 0.4(4) . . . . ? N2 Ni2 N3 C7 123.6(3) . . . . ? Cl2 Ni2 N3 C7 -56.8(3) . . . . ? S2 Ni2 N3 C7 33.7(3) . . . . ? S1 Ni2 N3 C7 -146.5(3) . . . . ? Cl1 Ni2 N3 C7 125.6(5) . . . . ? N2 Ni2 N3 C5 -117.8(4) . . . . ? Cl2 Ni2 N3 C5 61.8(4) . . . . ? S2 Ni2 N3 C5 152.3(4) . . . . ? S1 Ni2 N3 C5 -27.9(3) . . . . ? Cl1 Ni2 N3 C5 -115.8(5) . . . . ? N2 Ni2 N3 C4 2.1(4) . . . . ? Cl2 Ni2 N3 C4 -178.3(4) . . . . ? S2 Ni2 N3 C4 -87.9(4) . . . . ? S1 Ni2 N3 C4 91.9(4) . . . . ? Cl1 Ni2 N3 C4 4.1(8) . . . . ? N1 Ni1 N4 C16 -121.0(3) . . . . ? N5 Ni1 N4 C16 135.5(3) . . . . ? N6 Ni1 N4 C16 -17.5(3) . . . . ? Cl1 Ni1 N4 C16 -121.3(6) . . . . ? N1 Ni1 N4 C10 118.6(3) . . . . ? N5 Ni1 N4 C10 15.1(3) . . . . ? N6 Ni1 N4 C10 -137.9(3) . . . . ? Cl1 Ni1 N4 C10 118.3(6) . . . . ? N1 Ni1 N4 C9 -1.4(3) . . . . ? N5 Ni1 N4 C9 -104.9(3) . . . . ? N6 Ni1 N4 C9 102.2(3) . . . . ? Cl1 Ni1 N4 C9 -1.7(8) . . . . ? N1 Ni1 N5 C24 51.7(3) . . . . ? N6 Ni1 N5 C24 -161.9(3) . . . . ? N4 Ni1 N5 C24 130.7(3) . . . . ? Cl1 Ni1 N5 C24 -39.7(3) . . . . ? N1 Ni1 N5 C11 -66.2(3) . . . . ? N6 Ni1 N5 C11 80.2(4) . . . . ? N4 Ni1 N5 C11 12.8(3) . . . . ? Cl1 Ni1 N5 C11 -157.6(3) . . . . ? N1 Ni1 N5 C22 172.8(3) . . . . ? N6 Ni1 N5 C22 -40.9(5) . . . . ? N4 Ni1 N5 C22 -108.2(3) . . . . ? Cl1 Ni1 N5 C22 81.3(3) . . . . ? N1 Ni1 N6 C18 -49.2(3) . . . . ? N5 Ni1 N6 C18 164.5(3) . . . . ? N4 Ni1 N6 C18 -128.2(3) . . . . ? Cl1 Ni1 N6 C18 42.2(3) . . . . ? N1 Ni1 N6 C20 -175.1(3) . . . . ? N5 Ni1 N6 C20 38.5(5) . . . . ? N4 Ni1 N6 C20 105.8(3) . . . . ? Cl1 Ni1 N6 C20 -83.7(3) . . . . ? N1 Ni1 N6 C17 67.6(3) . . . . ? N5 Ni1 N6 C17 -78.8(4) . . . . ? N4 Ni1 N6 C17 -11.5(3) . . . . ? Cl1 Ni1 N6 C17 159.0(2) . . . . ? N2 N1 C1 C2 -0.2(5) . . . . ? Ni1 N1 C1 C2 178.1(3) . . . . ? N2 N1 C1 C9 -179.9(4) . . . . ? Ni1 N1 C1 C9 -1.6(5) . . . . ? N1 C1 C2 C3 0.9(5) . . . . ? C9 C1 C2 C3 -179.5(5) . . . . ? N1 N2 C3 C2 1.2(6) . . . . ? Ni2 N2 C3 C2 -177.7(3) . . . . ? N1 N2 C3 C4 179.5(5) . . . . ? Ni2 N2 C3 C4 0.6(7) . . . . ? C1 C2 C3 N2 -1.3(6) . . . . ? C1 C2 C3 C4 -179.2(6) . . . . ? N2 C3 C4 N3 1.3(8) . . . . ? C2 C3 C4 N3 179.1(6) . . . . ? C7 N3 C4 C3 -121.0(5) . . . . ? C5 N3 C4 C3 116.3(5) . . . . ? Ni2 N3 C4 C3 -2.4(7) . . . . ? C7 N3 C5 C6 171.3(5) . . . . ? C4 N3 C5 C6 -65.6(5) . . . . ? Ni2 N3 C5 C6 55.5(5) . . . . ? N3 C5 C6 S1 -58.3(6) . . . . ? C12 S1 C6 C5 -86.2(5) . . . . ? Ni2 S1 C6 C5 28.1(4) . . . . ? C5 N3 C7 C8 -174.5(5) . . . . ? C4 N3 C7 C8 63.5(6) . . . . ? Ni2 N3 C7 C8 -58.0(5) . . . . ? N3 C7 C8 S2 53.7(7) . . . . ? C14 S2 C8 C7 93.2(6) . . . . ? Ni2 S2 C8 C7 -20.3(5) . . . . ? C16 N4 C9 C1 117.0(4) . . . . ? C10 N4 C9 C1 -115.9(4) . . . . ? Ni1 N4 C9 C1 1.1(5) . . . . ? N1 C1 C9 N4 0.2(6) . . . . ? C2 C1 C9 N4 -179.4(5) . . . . ? C16 N4 C10 C11 -154.8(4) . . . . ? C9 N4 C10 C11 79.6(5) . . . . ? Ni1 N4 C10 C11 -40.2(4) . . . . ? C24 N5 C11 C10 -157.6(4) . . . . ? C22 N5 C11 C10 81.0(5) . . . . ? Ni1 N5 C11 C10 -39.7(4) . . . . ? N4 C10 C11 N5 56.1(5) . . . . ? C6 S1 C12 C13 -76.8(5) . . . . ? Ni2 S1 C12 C13 -177.8(4) . . . . ? C8 S2 C14 C15 178.8(4) . . . . ? Ni2 S2 C14 C15 -79.7(4) . . . . ? C10 N4 C16 C17 159.0(4) . . . . ? C9 N4 C16 C17 -75.4(5) . . . . ? Ni1 N4 C16 C17 43.9(4) . . . . ? N4 C16 C17 N6 -59.3(5) . . . . ? C18 N6 C17 C16 157.6(4) . . . . ? C20 N6 C17 C16 -81.6(5) . . . . ? Ni1 N6 C17 C16 39.9(4) . . . . ? C20 N6 C18 C19 -57.5(6) . . . . ? C17 N6 C18 C19 61.3(5) . . . . ? Ni1 N6 C18 C19 174.9(4) . . . . ? C18 N6 C20 C21 -54.6(5) . . . . ? C17 N6 C20 C21 -174.0(4) . . . . ? Ni1 N6 C20 C21 70.9(5) . . . . ? C24 N5 C22 C23 143.5(5) . . . . ? C11 N5 C22 C23 -95.0(5) . . . . ? Ni1 N5 C22 C23 22.5(6) . . . . ? C11 N5 C24 C25 -60.7(6) . . . . ? C22 N5 C24 C25 62.0(6) . . . . ? Ni1 N5 C24 C25 -176.0(4) . . . . ? C65 C60 C61 C62 0.6(7) . . . . ? C60 C61 C62 C63 0.3(7) . . . . ? C61 C62 C63 C64 -1.4(7) . . . . ? C62 C63 C64 C65 1.6(7) . . . . ? C63 C64 C65 C60 -0.7(7) . . . . ? C63 C64 C65 B1 -174.4(4) . . . . ? C61 C60 C65 C64 -0.4(7) . . . . ? C61 C60 C65 B1 173.2(4) . . . . ? C83 B1 C65 C64 -47.2(6) . . . . ? C77 B1 C65 C64 -164.2(4) . . . . ? C71 B1 C65 C64 76.9(5) . . . . ? C83 B1 C65 C60 139.6(4) . . . . ? C77 B1 C65 C60 22.6(6) . . . . ? C71 B1 C65 C60 -96.3(5) . . . . ? C71 C66 C67 C68 2.1(8) . . . . ? C66 C67 C68 C69 -0.8(8) . . . . ? C67 C68 C69 C70 -0.5(7) . . . . ? C68 C69 C70 C71 0.5(7) . . . . ? C69 C70 C71 C66 0.7(6) . . . . ? C69 C70 C71 B1 176.8(4) . . . . ? C67 C66 C71 C70 -2.0(7) . . . . ? C67 C66 C71 B1 -178.2(4) . . . . ? C83 B1 C71 C70 117.8(5) . . . . ? C65 B1 C71 C70 -4.6(6) . . . . ? C77 B1 C71 C70 -122.9(4) . . . . ? C83 B1 C71 C66 -66.4(5) . . . . ? C65 B1 C71 C66 171.2(4) . . . . ? C77 B1 C71 C66 52.9(5) . . . . ? C77 C72 C73 C74 -0.4(7) . . . . ? C72 C73 C74 C75 -0.4(7) . . . . ? C73 C74 C75 C76 0.5(8) . . . . ? C74 C75 C76 C77 0.2(8) . . . . ? C75 C76 C77 C72 -1.0(7) . . . . ? C75 C76 C77 B1 176.0(5) . . . . ? C73 C72 C77 C76 1.0(7) . . . . ? C73 C72 C77 B1 -175.9(4) . . . . ? C83 B1 C77 C76 144.6(4) . . . . ? C65 B1 C77 C76 -96.2(5) . . . . ? C71 B1 C77 C76 21.4(6) . . . . ? C83 B1 C77 C72 -38.7(5) . . . . ? C65 B1 C77 C72 80.5(5) . . . . ? C71 B1 C77 C72 -161.9(4) . . . . ? C83 C78 C79 C80 0.6(7) . . . . ? C78 C79 C80 C81 -0.6(7) . . . . ? C79 C80 C81 C82 -0.2(7) . . . . ? C80 C81 C82 C83 1.1(7) . . . . ? C81 C82 C83 C78 -1.1(6) . . . . ? C81 C82 C83 B1 172.6(4) . . . . ? C79 C78 C83 C82 0.3(6) . . . . ? C79 C78 C83 B1 -173.5(4) . . . . ? C65 B1 C83 C82 162.7(4) . . . . ? C77 B1 C83 C82 -79.1(5) . . . . ? C71 B1 C83 C82 41.8(6) . . . . ? C65 B1 C83 C78 -24.1(5) . . . . ? C77 B1 C83 C78 94.0(5) . . . . ? C71 B1 C83 C78 -145.0(4) . . . . ? C53 O1 C50 C51 1.2(54) . . . . ? C53 O1 C50 C53 0.000(5) . . . . ? C53 O1 C50 C52 -5.8(44) . . . . ? O1 C50 C51 C52 -11.6(52) . . . . ? C53 C50 C51 C52 -10.9(43) . . . . ? C52 C50 C51 C52 0.000(2) . . . . ? O1 C50 C51 C53 -0.7(31) . . . . ? C53 C50 C51 C53 0.000(3) . . . . ? C52 C50 C51 C53 10.9(43) . . . . ? C50 C51 C52 C53 15.1(59) . . . . ? C53 C51 C52 C53 0.000(6) . . . . ? C50 C51 C52 C50 0.000(2) . . . . ? C53 C51 C52 C50 -15.1(59) . . . . ? O1 C50 C52 C51 167.9(55) . . . . ? C51 C50 C52 C51 0.000(2) . . . . ? C53 C50 C52 C51 162.7(68) . . . . ? O1 C50 C52 C53 5.2(40) . . . . ? C51 C50 C52 C53 -162.7(68) . . . . ? C53 C50 C52 C53 0.000(6) . . . . ? C50 O1 C53 C52 11.7(88) . . . . ? C50 O1 C53 C50 0.000(3) . . . . ? C50 O1 C53 C51 -0.9(39) . . . . ? C51 C52 C53 O1 -19.9(97) . . . . ? C50 C52 C53 O1 -8.6(64) . . . . ? C51 C52 C53 C50 -11.4(44) . . . . ? C50 C52 C53 C50 0.000(4) . . . . ? C51 C52 C53 C51 0.000(4) . . . . ? C50 C52 C53 C51 11.4(44) . . . . ? O1 C50 C53 O1 0.000(5) . . . . ? C51 C50 C53 O1 -178.8(56) . . . . ? C52 C50 C53 O1 171.0(69) . . . . ? O1 C50 C53 C52 -171.0(69) . . . . ? C51 C50 C53 C52 10.2(40) . . . . ? C52 C50 C53 C52 0.000(5) . . . . ? O1 C50 C53 C51 178.8(56) . . . . ? C51 C50 C53 C51 0.000(2) . . . . ? C52 C50 C53 C51 -10.2(40) . . . . ? C52 C51 C53 O1 164.8(76) . . . . ? C50 C51 C53 O1 0.9(41) . . . . ? C52 C51 C53 C52 0.000(8) . . . . ? C50 C51 C53 C52 -163.9(63) . . . . ? C52 C51 C53 C50 163.9(63) . . . . ? C50 C51 C53 C50 0.000(3) . . . . ? C53X O1X C50X C51X 12.7(52) . . . . ? C52X O1X C50X C51X 0.8(32) . . . . ? O1X C50X C51X C52X -1.2(46) . . . . ? C50X C51X C52X C53X -9.2(71) . . . . ? C50X C51X C52X O1X 1.0(40) . . . . ? C53X O1X C52X C53X 0.000(9) . . . . ? C50X O1X C52X C53X 160.6(69) . . . . ? C53X O1X C52X C51X -161.5(79) . . . . ? C50X O1X C52X C51X -0.9(36) . . . . ? C50X O1X C53X C52X -19.9(70) . . . . ? C52X O1X C53X C52X 0.000(4) . . . . ? C51X C52X C53X O1X 20.9(88) . . . . ? O1X C52X C53X O1X 0.000(5) . . . . ? C57 O2 C55 C54 165.6(14) 2_666 . . . ? C56 O2 C55 C54 -173.2(11) . . . . ? C56 O2 C55 C54 169.1(13) 2_666 . . . ? C57 O2 C55 C57 0.000(3) 2_666 . . 2_666 ? C56 O2 C55 C57 21.1(14) . . . 2_666 ? C56 O2 C55 C57 3.5(15) 2_666 . . 2_666 ? C57 O2 C56 C57 0.000(2) 2_666 . . 2_666 ? C55 O2 C56 C57 -43.2(30) . . . 2_666 ? C56 O2 C56 C57 118.9(39) 2_666 . . 2_666 ? C57 O2 C56 C56 -118.9(39) 2_666 . . 2_666 ? C55 O2 C56 C56 -162.2(17) . . . 2_666 ? C56 O2 C56 C56 0.0 2_666 . . 2_666 ? C57 O2 C56 C57 -140.3(29) 2_666 . . . ? C55 O2 C56 C57 176.4(11) . . . . ? C56 O2 C56 C57 -21.4(13) 2_666 . . . ? C57 O2 C56 O2 -118.9(39) 2_666 . . 2_666 ? C55 O2 C56 O2 -162.2(17) . . . 2_666 ? C56 O2 C56 O2 -0.001(8) 2_666 . . 2_666 ? C57 C56 C57 C56 0.01(2) 2_666 . . 2_666 ? C56 C56 C57 C56 0.0 2_666 . . 2_666 ? O2 C56 C57 C56 58.8(32) . . . 2_666 ? O2 C56 C57 C56 -101.5(37) 2_666 . . 2_666 ? C57 C56 C57 O2 101.5(37) 2_666 . . 2_666 ? C56 C56 C57 O2 101.5(37) 2_666 . . 2_666 ? O2 C56 C57 O2 160.3(14) . . . 2_666 ? O2 C56 C57 O2 0.000(4) 2_666 . . 2_666 ? C57 C56 C57 C55 98.8(40) 2_666 . . 2_666 ? C56 C56 C57 C55 98.8(39) 2_666 . . 2_666 ? O2 C56 C57 C55 157.5(17) . . . 2_666 ? O2 C56 C57 C55 -2.8(12) 2_666 . . 2_666 ? _refine_diff_density_max 0.888 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.103