Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Way-Zen Lee' _publ_contact_author_address ; Department of Chemistry National Taiwan Normal University 88 Sec. 4, Ting-Chow Rd. Taipei 11677 TAIWAN ; _publ_contact_author_email WZLEE@NTNU.EDU.TW _publ_section_title ; Ligand-Controlled Nuclearity in Nickel Bis(benzimidazolyl) Complexes ; loop_ _publ_author_name 'Way-Zen Lee.' 'Ting-Shen Kuo.' 'Huan-Sheng Tsang.' data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 618812' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 Cl2 N10 Ni O8' _chemical_formula_sum 'C28 H34 Cl2 N10 Ni O8' _chemical_formula_weight 768.26 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' Ni Ni 0.3393 1.1124 '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 11.1550(3) _cell_length_b 12.2320(4) _cell_length_c 14.5190(4) _cell_angle_alpha 83.7640(10) _cell_angle_beta 74.6100(10) _cell_angle_gamma 63.7730(10) _cell_volume 1713.33(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 59317 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8633 _exptl_absorpt_correction_T_max 0.9401 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24043 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.04 _reflns_number_total 6026 _reflns_number_gt 5284 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0999P)^2^+1.3956P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.036(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6026 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1631 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.32183(4) 0.30864(3) 0.74901(3) 0.02214(19) Uani 1 1 d . . . Cl1 Cl 0.16176(9) 0.67042(8) 0.43715(6) 0.0319(2) Uani 1 1 d . . . Cl2 Cl 0.20522(9) 0.23202(7) 0.12864(6) 0.0309(2) Uani 1 1 d . . . O1 O 0.2058(3) 0.5880(3) 0.51299(19) 0.0434(7) Uani 1 1 d . . . O2 O 0.2435(3) 0.6127(3) 0.34615(18) 0.0397(6) Uani 1 1 d . . . O3 O 0.0192(3) 0.7015(3) 0.44381(19) 0.0428(7) Uani 1 1 d . . . O4 O 0.1765(5) 0.7787(3) 0.4452(3) 0.0741(11) Uani 1 1 d . . . O5 O 0.2332(4) 0.1733(3) 0.2166(2) 0.0622(10) Uani 1 1 d . . . O6 O 0.3202(3) 0.2532(3) 0.0728(3) 0.0577(8) Uani 1 1 d . . . O7 O 0.1811(3) 0.1563(3) 0.0750(2) 0.0532(8) Uani 1 1 d . . . O8 O 0.0872(3) 0.3466(2) 0.1493(2) 0.0451(7) Uani 1 1 d . . . N1 N 0.2464(3) 0.1845(2) 0.80931(19) 0.0238(6) Uani 1 1 d . . . N2 N 0.2796(3) 0.0125(2) 0.89014(19) 0.0256(6) Uani 1 1 d . . . N3' N 0.4899(3) 0.1885(2) 0.81121(19) 0.0242(6) Uani 1 1 d . . . H3' H 0.5048 0.2368 0.8509 0.029 Uiso 1 1 d R . . N4 N 0.6661(3) 0.0652(2) 0.5646(2) 0.0270(6) Uani 1 1 d . . . N5 N 0.4523(3) 0.1971(2) 0.63202(19) 0.0229(6) Uani 1 1 d . . . N6 N 0.4110(3) 0.4291(3) 0.6913(2) 0.0273(6) Uani 1 1 d . . . N7 N 0.1577(3) 0.4153(3) 0.6907(2) 0.0270(6) Uani 1 1 d . . . N8 N 0.2246(3) 0.4206(3) 0.8709(2) 0.0279(6) Uani 1 1 d . . . N9 N 0.7406(4) 0.2932(3) 0.1780(3) 0.0543(10) Uani 1 1 d . . . N10 N 0.4374(4) 0.6478(3) 0.0902(3) 0.0464(8) Uani 1 1 d . . . C1 C 0.1356(3) 0.1575(3) 0.8134(2) 0.0255(7) Uani 1 1 d . . . C2 C 0.0210(4) 0.2167(3) 0.7754(3) 0.0321(8) Uani 1 1 d . . . H2 H 0.0049 0.2897 0.7385 0.039 Uiso 1 1 d R . . C3 C -0.0717(4) 0.1657(4) 0.7919(3) 0.0375(9) Uani 1 1 d . . . H3 H -0.1528 0.2061 0.7678 0.045 Uiso 1 1 d R . . C4 C -0.0508(4) 0.0583(4) 0.8444(3) 0.0368(8) Uani 1 1 d . . . H4 H -0.1157 0.0238 0.8546 0.044 Uiso 1 1 d R . . C5 C 0.0619(4) -0.0020(3) 0.8824(2) 0.0309(8) Uani 1 1 d . . . H5 H 0.0731 -0.0753 0.9180 0.037 Uiso 1 1 d R . . C6 C 0.1554(3) 0.0495(3) 0.8652(2) 0.0258(7) Uani 1 1 d . . . C7 C 0.3428(4) -0.0953(3) 0.9454(3) 0.0324(8) Uani 1 1 d . . . H7A H 0.2868 -0.1390 0.9608 0.039 Uiso 1 1 d R . . H7B H 0.3509 -0.0709 1.0032 0.039 Uiso 1 1 d R . . H7C H 0.4327 -0.1470 0.9083 0.039 Uiso 1 1 d R . . C8 C 0.3270(3) 0.0972(3) 0.8556(2) 0.0228(7) Uani 1 1 d . . . C9 C 0.4560(3) 0.0945(3) 0.8702(2) 0.0282(7) Uani 1 1 d . . . H9A H 0.5306 0.0158 0.8515 0.034 Uiso 1 1 d R . . H9B H 0.4435 0.1089 0.9366 0.034 Uiso 1 1 d R . . C10 C 0.6161(3) 0.1387(3) 0.7331(2) 0.0284(7) Uani 1 1 d . . . H10A H 0.6629 0.1903 0.7230 0.034 Uiso 1 1 d R . . H10B H 0.6756 0.0587 0.7504 0.034 Uiso 1 1 d R . . C11 C 0.5781(3) 0.1298(3) 0.6435(2) 0.0240(7) Uani 1 1 d . . . C12 C 0.8113(3) -0.0217(3) 0.5524(3) 0.0338(8) Uani 1 1 d . . . H12A H 0.8476 -0.0532 0.4882 0.041 Uiso 1 1 d R . . H12B H 0.8179 -0.0874 0.5964 0.041 Uiso 1 1 d R . . H12C H 0.8632 0.0181 0.5643 0.041 Uiso 1 1 d R . . C13 C 0.5927(3) 0.0934(3) 0.4948(2) 0.0251(7) Uani 1 1 d . . . C14 C 0.6317(4) 0.0567(3) 0.3999(2) 0.0308(8) Uani 1 1 d . . . H14 H 0.7237 0.0018 0.3687 0.037 Uiso 1 1 d R . . C15 C 0.5304(4) 0.1053(3) 0.3500(3) 0.0327(8) Uani 1 1 d . . . H15 H 0.5549 0.0821 0.2842 0.039 Uiso 1 1 d R . . C16 C 0.3942(4) 0.1864(3) 0.3930(2) 0.0308(8) Uani 1 1 d . . . H16 H 0.3256 0.2180 0.3567 0.037 Uiso 1 1 d R . . C17 C 0.3555(3) 0.2226(3) 0.4877(2) 0.0262(7) Uani 1 1 d . . . H17 H 0.2621 0.2772 0.5165 0.031 Uiso 1 1 d R . . C18 C 0.4574(3) 0.1762(3) 0.5386(2) 0.0242(7) Uani 1 1 d . . . C19 C 0.4400(3) 0.5012(3) 0.6489(2) 0.0270(7) Uani 1 1 d . . . C20 C 0.4736(4) 0.5957(3) 0.5936(3) 0.0335(8) Uani 1 1 d . . . H20A H 0.5660 0.5807 0.5927 0.040 Uiso 1 1 d R . . H20B H 0.4104 0.6737 0.6228 0.040 Uiso 1 1 d R . . H20C H 0.4659 0.5953 0.5294 0.040 Uiso 1 1 d R . . C21 C 0.0609(3) 0.4818(3) 0.6682(2) 0.0251(7) Uani 1 1 d . . . C22 C -0.0659(3) 0.5655(3) 0.6411(2) 0.0289(7) Uani 1 1 d . . . H22A H -0.0509 0.6296 0.6031 0.035 Uiso 1 1 d R . . H22B H -0.1380 0.5997 0.6976 0.035 Uiso 1 1 d R . . H22C H -0.0922 0.5223 0.6048 0.035 Uiso 1 1 d R . . C23 C 0.1777(3) 0.4915(3) 0.9309(2) 0.0278(7) Uani 1 1 d . . . C24 C 0.1173(4) 0.5813(3) 1.0077(3) 0.0358(8) Uani 1 1 d . . . H24A H 0.0519 0.6569 0.9883 0.043 Uiso 1 1 d R . . H24B H 0.1889 0.5943 1.0227 0.043 Uiso 1 1 d R . . H24C H 0.0716 0.5516 1.0632 0.043 Uiso 1 1 d R . . C25 C 0.8064(5) 0.2583(4) 0.2323(3) 0.0492(11) Uani 1 1 d . . . C26 C 0.8904(5) 0.2121(5) 0.3024(3) 0.0591(13) Uani 1 1 d . . . H26A H 0.9578 0.1296 0.2874 0.071 Uiso 1 1 d R . . H26B H 0.8314 0.2154 0.3648 0.071 Uiso 1 1 d R . . H26C H 0.9361 0.2630 0.3015 0.071 Uiso 1 1 d R . . C27 C 0.4246(4) 0.5611(4) 0.1169(3) 0.0373(9) Uani 1 1 d . . . C28 C 0.4093(5) 0.4498(4) 0.1504(3) 0.0487(10) Uani 1 1 d . . . H28A H 0.4790 0.4007 0.1837 0.058 Uiso 1 1 d R . . H28B H 0.4186 0.4047 0.0968 0.058 Uiso 1 1 d R . . H28C H 0.3199 0.4711 0.1928 0.058 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0200(3) 0.0206(3) 0.0270(3) -0.00018(17) -0.00779(18) -0.00862(19) Cl1 0.0368(5) 0.0340(5) 0.0299(4) 0.0004(3) -0.0067(4) -0.0205(4) Cl2 0.0305(5) 0.0262(4) 0.0349(5) -0.0023(3) -0.0107(3) -0.0091(4) O1 0.0339(14) 0.0620(18) 0.0356(14) 0.0130(13) -0.0140(11) -0.0214(13) O2 0.0329(14) 0.0497(16) 0.0315(13) -0.0020(12) -0.0056(11) -0.0140(12) O3 0.0280(13) 0.0462(16) 0.0413(15) 0.0054(12) -0.0073(11) -0.0064(12) O4 0.121(3) 0.070(2) 0.060(2) -0.0071(17) -0.003(2) -0.076(2) O5 0.076(2) 0.0395(17) 0.0450(17) -0.0017(13) -0.0301(16) 0.0076(16) O6 0.0366(16) 0.060(2) 0.080(2) -0.0054(17) -0.0071(15) -0.0269(15) O7 0.072(2) 0.0539(18) 0.0479(17) -0.0121(14) -0.0062(15) -0.0415(17) O8 0.0415(16) 0.0335(14) 0.0434(15) -0.0011(12) -0.0141(13) 0.0011(12) N1 0.0222(14) 0.0246(14) 0.0267(14) -0.0013(11) -0.0068(11) -0.0111(12) N2 0.0264(14) 0.0246(14) 0.0267(14) 0.0012(11) -0.0070(11) -0.0115(12) N3 0.0226(14) 0.0231(14) 0.0294(14) -0.0010(11) -0.0100(11) -0.0099(12) N4 0.0197(14) 0.0239(14) 0.0363(16) -0.0009(12) -0.0055(12) -0.0089(12) N5 0.0210(14) 0.0210(13) 0.0282(14) -0.0003(11) -0.0074(11) -0.0095(11) N6 0.0235(14) 0.0254(15) 0.0333(15) -0.0051(12) -0.0064(12) -0.0100(12) N7 0.0259(15) 0.0259(15) 0.0298(15) 0.0012(12) -0.0059(12) -0.0124(13) N8 0.0273(15) 0.0268(15) 0.0322(15) 0.0029(13) -0.0110(12) -0.0124(12) N9 0.061(2) 0.042(2) 0.055(2) -0.0090(18) -0.007(2) -0.0201(19) N10 0.050(2) 0.047(2) 0.052(2) -0.0073(17) -0.0134(17) -0.0274(18) C1 0.0249(17) 0.0274(17) 0.0265(16) -0.0009(13) -0.0053(13) -0.0135(14) C2 0.0306(18) 0.0347(19) 0.0388(19) 0.0090(15) -0.0151(15) -0.0192(16) C3 0.0336(19) 0.046(2) 0.042(2) 0.0090(17) -0.0175(16) -0.0227(18) C4 0.035(2) 0.046(2) 0.042(2) 0.0035(17) -0.0096(16) -0.0287(18) C5 0.0339(19) 0.0323(18) 0.0294(18) 0.0012(14) -0.0058(15) -0.0180(16) C6 0.0259(17) 0.0249(17) 0.0259(16) -0.0017(13) -0.0056(13) -0.0105(14) C7 0.0334(19) 0.0266(18) 0.0385(19) 0.0082(15) -0.0138(15) -0.0131(15) C8 0.0235(16) 0.0212(16) 0.0218(15) -0.0024(12) -0.0051(13) -0.0076(13) C9 0.0245(17) 0.0276(17) 0.0333(18) 0.0025(14) -0.0098(14) -0.0109(14) C10 0.0219(16) 0.0322(18) 0.0342(18) 0.0042(14) -0.0109(14) -0.0130(14) C11 0.0218(16) 0.0229(16) 0.0317(17) 0.0020(13) -0.0068(13) -0.0136(14) C12 0.0218(17) 0.0292(18) 0.047(2) -0.0001(15) -0.0076(15) -0.0081(15) C13 0.0232(16) 0.0213(16) 0.0329(17) -0.0007(13) -0.0060(13) -0.0117(14) C14 0.0302(18) 0.0262(17) 0.0343(18) -0.0053(14) -0.0007(15) -0.0133(15) C15 0.044(2) 0.0286(18) 0.0291(17) -0.0028(14) -0.0052(15) -0.0205(17) C16 0.037(2) 0.0301(18) 0.0317(18) 0.0014(14) -0.0131(15) -0.0182(16) C17 0.0255(17) 0.0235(16) 0.0327(17) -0.0007(13) -0.0086(14) -0.0122(14) C18 0.0241(16) 0.0203(16) 0.0301(17) -0.0011(13) -0.0055(13) -0.0115(14) C19 0.0236(17) 0.0260(17) 0.0327(18) -0.0037(14) -0.0092(14) -0.0097(14) C20 0.0335(19) 0.0315(19) 0.0383(19) 0.0032(15) -0.0095(16) -0.0167(16) C21 0.0241(17) 0.0239(17) 0.0273(16) 0.0003(13) -0.0052(13) -0.0111(15) C22 0.0233(17) 0.0292(18) 0.0331(18) -0.0017(14) -0.0106(14) -0.0077(14) C23 0.0254(17) 0.0276(18) 0.0305(18) 0.0026(15) -0.0090(14) -0.0108(15) C24 0.040(2) 0.035(2) 0.0311(18) -0.0060(15) -0.0093(16) -0.0134(17) C25 0.052(3) 0.047(3) 0.047(2) -0.018(2) 0.006(2) -0.026(2) C26 0.056(3) 0.081(4) 0.049(3) -0.011(2) -0.006(2) -0.038(3) C27 0.033(2) 0.044(2) 0.038(2) -0.0113(17) -0.0082(16) -0.0173(18) C28 0.055(3) 0.046(2) 0.045(2) -0.0032(19) -0.006(2) -0.024(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 Ni1 N1 2.056(3) . ? Ni1 N7 2.059(3) . ? Ni1 N5 2.074(3) . ? Ni1 N8 2.093(3) . ? Ni1 N6 2.109(3) . ? Ni1 N3 2.160(3) . ? Cl1 O4 1.426(3) . ? Cl1 O2 1.439(3) . ? Cl1 O3 1.440(3) . ? Cl1 O1 1.442(3) . ? Cl2 O7 1.423(3) . ? Cl2 O8 1.428(3) . ? Cl2 O5 1.435(3) . ? Cl2 O6 1.438(3) . ? N1 C8 1.310(4) . ? N1 C1 1.400(4) . ? N2 C8 1.356(4) . ? N2 C6 1.389(4) . ? N2 C7 1.459(4) . ? N3 C10 1.478(4) . ? N3 C9 1.481(4) . ? N4 C11 1.347(4) . ? N4 C13 1.389(4) . ? N4 C12 1.467(4) . ? N5 C11 1.323(4) . ? N5 C18 1.389(4) . ? N6 C19 1.135(4) . ? N7 C21 1.135(4) . ? N8 C23 1.143(4) . ? N9 C25 1.139(6) . ? N10 C27 1.145(5) . ? C1 C2 1.389(5) . ? C1 C6 1.405(5) . ? C2 C3 1.387(5) . ? C3 C4 1.403(5) . ? C4 C5 1.375(5) . ? C5 C6 1.398(5) . ? C8 C9 1.495(4) . ? C10 C11 1.499(4) . ? C13 C14 1.390(5) . ? C13 C18 1.409(5) . ? C14 C15 1.380(5) . ? C15 C16 1.407(5) . ? C16 C17 1.387(5) . ? C17 C18 1.395(5) . ? C19 C20 1.464(5) . ? C21 C22 1.460(5) . ? C23 C24 1.455(5) . ? C25 C26 1.465(7) . ? C27 C28 1.462(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 N1 Ni1 N7 95.56(11) . . ? N1 Ni1 N5 93.23(10) . . ? N7 Ni1 N5 99.16(10) . . ? N1 Ni1 N8 92.77(11) . . ? N7 Ni1 N8 89.34(11) . . ? N5 Ni1 N8 169.07(10) . . ? N1 Ni1 N6 176.03(10) . . ? N7 Ni1 N6 88.41(11) . . ? N5 Ni1 N6 86.23(10) . . ? N8 Ni1 N6 87.15(11) . . ? N1 Ni1 N3 81.20(10) . . ? N7 Ni1 N3 176.63(10) . . ? N5 Ni1 N3 80.17(10) . . ? N8 Ni1 N3 91.74(10) . . ? N6 Ni1 N3 94.83(10) . . ? O4 Cl1 O2 109.54(19) . . ? O4 Cl1 O3 109.2(2) . . ? O2 Cl1 O3 109.08(16) . . ? O4 Cl1 O1 110.0(2) . . ? O2 Cl1 O1 109.72(17) . . ? O3 Cl1 O1 109.25(16) . . ? O7 Cl2 O8 110.31(19) . . ? O7 Cl2 O5 109.4(2) . . ? O8 Cl2 O5 109.16(18) . . ? O7 Cl2 O6 108.76(19) . . ? O8 Cl2 O6 108.58(19) . . ? O5 Cl2 O6 110.6(2) . . ? C8 N1 C1 106.0(3) . . ? C8 N1 Ni1 113.9(2) . . ? C1 N1 Ni1 140.0(2) . . ? C8 N2 C6 106.7(3) . . ? C8 N2 C7 127.4(3) . . ? C6 N2 C7 125.9(3) . . ? C10 N3 C9 114.2(3) . . ? C10 N3 Ni1 107.99(19) . . ? C9 N3 Ni1 110.77(19) . . ? C11 N4 C13 107.1(3) . . ? C11 N4 C12 127.9(3) . . ? C13 N4 C12 125.0(3) . . ? C11 N5 C18 105.8(3) . . ? C11 N5 Ni1 112.9(2) . . ? C18 N5 Ni1 140.9(2) . . ? C19 N6 Ni1 165.8(3) . . ? C21 N7 Ni1 172.0(3) . . ? C23 N8 Ni1 171.4(3) . . ? C2 C1 N1 131.3(3) . . ? C2 C1 C6 120.4(3) . . ? N1 C1 C6 108.3(3) . . ? C1 C2 C3 117.4(3) . . ? C2 C3 C4 121.5(3) . . ? C5 C4 C3 122.1(3) . . ? C4 C5 C6 116.2(3) . . ? N2 C6 C5 131.6(3) . . ? N2 C6 C1 105.9(3) . . ? C5 C6 C1 122.5(3) . . ? N1 C8 N2 113.1(3) . . ? N1 C8 C9 122.7(3) . . ? N2 C8 C9 124.1(3) . . ? N3 C9 C8 110.4(3) . . ? N3 C10 C11 109.3(3) . . ? N5 C11 N4 112.9(3) . . ? N5 C11 C10 121.1(3) . . ? N4 C11 C10 125.7(3) . . ? N4 C13 C14 132.0(3) . . ? N4 C13 C18 105.5(3) . . ? C14 C13 C18 122.4(3) . . ? C15 C14 C13 116.5(3) . . ? C14 C15 C16 121.9(3) . . ? C17 C16 C15 121.5(3) . . ? C16 C17 C18 117.2(3) . . ? N5 C18 C17 130.9(3) . . ? N5 C18 C13 108.6(3) . . ? C17 C18 C13 120.5(3) . . ? N6 C19 C20 178.4(4) . . ? N7 C21 C22 178.3(4) . . ? N8 C23 C24 179.5(4) . . ? N9 C25 C26 179.2(5) . . ? N10 C27 C28 179.5(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.809 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.213 data_complex_6 _database_code_depnum_ccdc_archive 'CCDC 618813' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H88 N10 Ni2 O15 S2' _chemical_formula_sum 'C68 H88 N10 Ni2 O15 S2' _chemical_formula_weight 1467.02 _chemical_absolute_configuration unk 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' Ni Ni 0.3393 1.1124 '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' 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' _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 11.31500(10) _cell_length_b 12.7650(2) _cell_length_c 12.9400(2) _cell_angle_alpha 85.8370(10) _cell_angle_beta 89.3790(10) _cell_angle_gamma 69.3040(10) _cell_volume 1743.56(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 24276 _cell_measurement_theta_min 1.958 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 774 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8672 _exptl_absorpt_correction_T_max 0.9197 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24681 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.06 _reflns_number_total 6168 _reflns_number_gt 5525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & M 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0450P)^2^+7.0705P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0144(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6168 _refine_ls_number_parameters 459 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1756 _refine_ls_wR_factor_gt 0.1693 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.010 _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 Ni1 Ni 0.23967(6) 0.60269(5) 0.27222(4) 0.0259(2) Uani 1 1 d . . . S1 S 0.12610(12) 0.30167(11) 0.12072(10) 0.0333(3) Uani 1 1 d . A . N1 N 0.3329(3) 0.4955(3) 0.1612(3) 0.0255(8) Uani 1 1 d . . . N2 N 0.3765(4) 0.4027(3) 0.0174(3) 0.0273(8) Uani 1 1 d . . . N3 N 0.0870(4) 0.4368(3) 0.1284(3) 0.0290(9) Uani 1 1 d . . . N4 N 0.0468(3) 0.3931(3) 0.3962(3) 0.0284(9) Uani 1 1 d . . . N5 N 0.1790(3) 0.4821(3) 0.3497(3) 0.0245(8) Uani 1 1 d . . . O1 O 0.3870(3) 0.6014(3) 0.3718(2) 0.0321(8) Uani 1 1 d . . . O2 O 0.1908(3) 0.7062(3) 0.3973(2) 0.0326(8) Uani 1 1 d . . . O3 O 0.2415(4) 0.7493(3) 0.1792(3) 0.0430(9) Uani 1 1 d . . . O4 O 0.0746(3) 0.7009(3) 0.1910(3) 0.0399(9) Uani 1 1 d . . . O5 O 0.0275(4) 0.2712(3) 0.1682(3) 0.0468(10) Uani 1 1 d . . . O6 O 0.1548(4) 0.2810(3) 0.0137(3) 0.0444(9) Uani 1 1 d . . . C1 C 0.2138(4) 0.4290(4) 0.4487(3) 0.0250(9) Uani 1 1 d . . . C2 C 0.3135(4) 0.4213(4) 0.5151(4) 0.0294(10) Uani 1 1 d . . . H2 H 0.3733 0.4556 0.4925 0.035 Uiso 1 1 d R . . C3 C 0.3215(5) 0.3632(4) 0.6099(4) 0.0349(11) Uani 1 1 d . . . H3 H 0.3882 0.3567 0.6580 0.042 Uiso 1 1 d R . . C4 C 0.2328(5) 0.3130(4) 0.6405(4) 0.0370(12) Uani 1 1 d . . . H4 H 0.2408 0.2732 0.7074 0.044 Uiso 1 1 d R . . C5 C 0.1352(5) 0.3181(4) 0.5755(4) 0.0341(11) Uani 1 1 d . . . H5 H 0.0762 0.2832 0.5988 0.041 Uiso 1 1 d R . . C6 C 0.1285(4) 0.3751(4) 0.4798(4) 0.0275(10) Uani 1 1 d . . . C7 C -0.0571(5) 0.3492(5) 0.3940(4) 0.0382(12) Uani 1 1 d . . . H7A H -0.1009 0.3720 0.3284 0.046 Uiso 1 1 d R . . H7B H -0.1148 0.3781 0.4487 0.046 Uiso 1 1 d R . . H7C H -0.0234 0.2687 0.4030 0.046 Uiso 1 1 d R . . C8 C 0.0802(4) 0.4566(4) 0.3211(4) 0.0274(10) Uani 1 1 d . . . C9 C 0.0137(4) 0.4900(4) 0.2174(4) 0.0298(10) Uani 1 1 d . . . H9A H -0.0096 0.5700 0.2068 0.036 Uiso 1 1 d R . . H9B H -0.0611 0.4711 0.2238 0.036 Uiso 1 1 d R . . C10 C 0.1471(4) 0.4989(4) 0.0570(4) 0.0293(10) Uani 1 1 d . . . H10A H 0.1377 0.4825 -0.0130 0.035 Uiso 1 1 d R . . H10B H 0.1076 0.5782 0.0633 0.035 Uiso 1 1 d R . . C11 C 0.2851(4) 0.4689(4) 0.0775(3) 0.0258(10) Uani 1 1 d . . . C12 C 0.3637(5) 0.3557(5) -0.0806(4) 0.0380(12) Uani 1 1 d . . . H12A H 0.4456 0.3119 -0.1047 0.046 Uiso 1 1 d R . . H12B H 0.3227 0.4161 -0.1314 0.046 Uiso 1 1 d R . . H12C H 0.3137 0.3088 -0.0699 0.046 Uiso 1 1 d R . . C13 C 0.4916(4) 0.3840(4) 0.0647(3) 0.0270(10) Uani 1 1 d . . . C14 C 0.6144(5) 0.3210(4) 0.0369(4) 0.0350(11) Uani 1 1 d . . . H14 H 0.6278 0.2830 -0.0260 0.042 Uiso 1 1 d R . . C15 C 0.7090(5) 0.3177(5) 0.1045(4) 0.0410(13) Uani 1 1 d . . . H15 H 0.7952 0.2764 0.0882 0.049 Uiso 1 1 d R . . C16 C 0.6824(5) 0.3730(5) 0.1962(4) 0.0404(12) Uani 1 1 d . . . H16 H 0.7505 0.3674 0.2425 0.049 Uiso 1 1 d R . . C17 C 0.5615(5) 0.4360(4) 0.2229(4) 0.0328(11) Uani 1 1 d . . . H17 H 0.5478 0.4738 0.2859 0.039 Uiso 1 1 d R . . C18 C 0.4645(4) 0.4406(4) 0.1558(3) 0.0260(10) Uani 1 1 d . . . C19 C 0.3062(5) 0.6740(4) 0.4222(4) 0.0314(11) Uani 1 1 d . . . C20 C 0.3492(6) 0.7199(5) 0.5122(4) 0.0437(13) Uani 1 1 d . . . H20A H 0.2776 0.7731 0.5432 0.052 Uiso 1 1 d R . . H20B H 0.4063 0.7564 0.4879 0.052 Uiso 1 1 d R . . H20C H 0.3916 0.6597 0.5628 0.052 Uiso 1 1 d R . . C21 C 0.1279(6) 0.7689(5) 0.1583(4) 0.0442(14) Uani 1 1 d . . . C22 C 0.0536(8) 0.8728(5) 0.0912(6) 0.075(2) Uani 1 1 d . . . H22A H -0.0313 0.8745 0.0832 0.090 Uiso 1 1 d R . . H22B H 0.0916 0.8708 0.0242 0.090 Uiso 1 1 d R . . H22C H 0.0526 0.9386 0.1232 0.090 Uiso 1 1 d R . . C23 C 0.2677(5) 0.2410(4) 0.1968(4) 0.0310(10) Uani 1 1 d . . . H23A H 0.3351 0.2575 0.1620 0.037 Uiso 1 1 d R A . H23B H 0.2554 0.2717 0.2634 0.037 Uiso 1 1 d R . . C24 C 0.3188(5) 0.1145(4) 0.2202(4) 0.0332(11) Uani 0.458(5) 1 d PD A 1 C25 C 0.2217(14) 0.0545(12) 0.2563(15) 0.065(3) Uani 0.458(5) 1 d PD A 1 H25A H 0.1575 0.1008 0.3005 0.078 Uiso 0.458(5) 1 calc PR A 1 H25B H 0.1809 0.0380 0.1972 0.078 Uiso 0.458(5) 1 calc PR A 1 O7 O 0.3940(13) 0.0817(11) 0.0502(10) 0.100(3) Uani 0.458(5) 1 d P A 1 C26 C 0.3065(16) -0.0542(14) 0.3166(14) 0.068(3) Uiso 0.458(5) 1 d PD A 1 H26A H 0.3012 -0.1198 0.2863 0.081 Uiso 0.458(5) 1 calc PR A 1 H26B H 0.2822 -0.0558 0.3886 0.081 Uiso 0.458(5) 1 calc PR A 1 C27 C 0.4408(16) -0.0504(14) 0.3068(15) 0.052(4) Uani 0.458(5) 1 d PD A 1 H27A H 0.5044 -0.1023 0.3551 0.063 Uiso 0.458(5) 1 calc PR A 1 C28 C 0.4639(17) -0.0692(13) 0.1925(15) 0.067(3) Uiso 0.458(5) 1 d PD A 1 H28A H 0.4352 -0.1280 0.1721 0.080 Uiso 0.458(5) 1 calc PR A 1 H28B H 0.5528 -0.0888 0.1766 0.080 Uiso 0.458(5) 1 calc PR A 1 C29 C 0.3835(19) 0.0473(12) 0.1374(11) 0.066(3) Uani 0.458(5) 1 d PD A 1 C30 C 0.4187(12) 0.0719(11) 0.3133(12) 0.044(2) Uani 0.458(5) 1 d P A 1 C31 C 0.5357(14) 0.1023(14) 0.2894(18) 0.069(3) Uani 0.458(5) 1 d P A 1 H31A H 0.5942 0.0762 0.3469 0.103 Uiso 0.458(5) 1 calc PR A 1 H31B H 0.5113 0.1823 0.2779 0.103 Uiso 0.458(5) 1 calc PR A 1 H31C H 0.5750 0.0674 0.2285 0.103 Uiso 0.458(5) 1 calc PR A 1 C32 C 0.3665(16) 0.1155(13) 0.4179(12) 0.066(3) Uani 0.458(5) 1 d P A 1 H32A H 0.4317 0.0861 0.4702 0.100 Uiso 0.458(5) 1 calc PR A 1 H32B H 0.2969 0.0918 0.4361 0.100 Uiso 0.458(5) 1 calc PR A 1 H32C H 0.3381 0.1961 0.4128 0.100 Uiso 0.458(5) 1 calc PR A 1 C24' C 0.3188(5) 0.1145(4) 0.2202(4) 0.0332(11) Uani 0.542(5) 1 d PD A 2 C25' C 0.3123(14) 0.0376(10) 0.1299(11) 0.065(3) Uani 0.542(5) 1 d PD A 2 H25C H 0.2290 0.0325 0.1248 0.078 Uiso 0.542(5) 1 calc PR A 2 H25D H 0.3333 0.0663 0.0636 0.078 Uiso 0.542(5) 1 calc PR A 2 O7' O 0.1713(11) 0.1314(10) 0.3572(8) 0.100(3) Uani 0.542(5) 1 d P A 2 C26' C 0.4123(14) -0.0772(12) 0.1650(11) 0.068(3) Uiso 0.542(5) 1 d PD A 2 H26C H 0.3755 -0.1354 0.1704 0.081 Uiso 0.542(5) 1 calc PR A 2 H26D H 0.4816 -0.0979 0.1169 0.081 Uiso 0.542(5) 1 calc PR A 2 C27' C 0.4574(15) -0.0592(11) 0.2718(10) 0.052(4) Uani 0.542(5) 1 d PD A 2 H27B H 0.5375 -0.1165 0.2962 0.063 Uiso 0.542(5) 1 calc PR A 2 C28' C 0.3455(14) -0.0451(12) 0.3472(12) 0.067(3) Uiso 0.542(5) 1 d PD A 2 H28C H 0.3720 -0.0505 0.4191 0.080 Uiso 0.542(5) 1 calc PR A 2 H28D H 0.3048 -0.0991 0.3378 0.080 Uiso 0.542(5) 1 calc PR A 2 C29' C 0.2594(15) 0.0766(10) 0.3098(10) 0.066(3) Uani 0.542(5) 1 d PD A 2 C30' C 0.4619(10) 0.0621(9) 0.2530(10) 0.044(2) Uani 0.542(5) 1 d P A 2 C31' C 0.5550(11) 0.0743(11) 0.1721(12) 0.069(3) Uani 0.542(5) 1 d P A 2 H31D H 0.5510 0.1508 0.1650 0.103 Uiso 0.542(5) 1 calc PR A 2 H31E H 0.5340 0.0534 0.1068 0.103 Uiso 0.542(5) 1 calc PR A 2 H31F H 0.6389 0.0262 0.1931 0.103 Uiso 0.542(5) 1 calc PR A 2 C32' C 0.4911(15) 0.1120(11) 0.3522(11) 0.066(3) Uani 0.542(5) 1 d P A 2 H32D H 0.4995 0.1832 0.3334 0.100 Uiso 0.542(5) 1 calc PR A 2 H32E H 0.5685 0.0615 0.3839 0.100 Uiso 0.542(5) 1 calc PR A 2 H32F H 0.4233 0.1221 0.4001 0.100 Uiso 0.542(5) 1 calc PR A 2 O8 O -0.0296(16) 0.0417(16) 0.4162(13) 0.127(5) Uiso 0.50 1 d PD . . C33 C 0.0000 0.0000 0.5000 0.123(5) Uani 1 2 d SD . . C34 C 0.0855(18) 0.0330(16) 0.577(2) 0.129(8) Uani 0.50 1 d PD . . H34A H 0.1372 -0.0349 0.5476 0.194 Uiso 0.50 1 calc PR . . H34B H 0.1327 0.0819 0.5815 0.194 Uiso 0.50 1 calc PR . . H34C H 0.0119 0.0697 0.5339 0.194 Uiso 0.50 1 calc PR . . C35 C -0.063(3) -0.017(2) 0.3632(18) 0.123(5) Uani 0.50 1 d PD . . C36 C -0.1331(16) 0.0706(15) 0.277(2) 0.129(8) Uani 0.50 1 d PD . . H36A H -0.1705 0.0369 0.2292 0.194 Uiso 0.50 1 calc PR . . H36B H -0.0747 0.0989 0.2413 0.194 Uiso 0.50 1 calc PR . . H36C H -0.1981 0.1313 0.3067 0.194 Uiso 0.50 1 calc PR . . 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 0.0292(4) 0.0266(3) 0.0229(3) -0.0024(2) 0.0013(2) -0.0107(3) S1 0.0319(7) 0.0336(7) 0.0367(7) -0.0054(5) -0.0065(5) -0.0137(5) N1 0.026(2) 0.027(2) 0.0229(19) -0.0004(15) -0.0004(15) -0.0091(16) N2 0.032(2) 0.029(2) 0.0197(18) -0.0040(15) 0.0017(16) -0.0081(17) N3 0.027(2) 0.031(2) 0.029(2) -0.0028(16) -0.0042(16) -0.0097(17) N4 0.0216(19) 0.033(2) 0.031(2) -0.0019(17) 0.0017(16) -0.0101(17) N5 0.0225(19) 0.0252(19) 0.0243(19) -0.0031(15) 0.0010(15) -0.0065(15) O1 0.0339(18) 0.0371(19) 0.0291(17) -0.0068(15) 0.0033(14) -0.0163(15) O2 0.037(2) 0.0347(19) 0.0275(17) -0.0048(14) 0.0038(14) -0.0145(15) O3 0.064(3) 0.035(2) 0.0312(19) -0.0008(15) 0.0071(18) -0.0208(19) O4 0.045(2) 0.0311(19) 0.037(2) -0.0004(16) -0.0069(16) -0.0052(16) O5 0.038(2) 0.048(2) 0.064(3) -0.0036(19) -0.0036(18) -0.0265(18) O6 0.053(2) 0.046(2) 0.036(2) -0.0118(17) -0.0095(17) -0.0178(19) C1 0.026(2) 0.023(2) 0.024(2) -0.0041(18) 0.0039(18) -0.0062(18) C2 0.030(3) 0.026(2) 0.033(3) -0.0020(19) -0.002(2) -0.011(2) C3 0.038(3) 0.034(3) 0.029(3) 0.000(2) -0.006(2) -0.010(2) C4 0.044(3) 0.032(3) 0.030(3) 0.002(2) 0.001(2) -0.010(2) C5 0.038(3) 0.030(3) 0.034(3) 0.000(2) 0.006(2) -0.013(2) C6 0.024(2) 0.025(2) 0.032(2) -0.0048(19) 0.0022(19) -0.0065(19) C7 0.026(3) 0.048(3) 0.046(3) -0.003(2) 0.006(2) -0.019(2) C8 0.020(2) 0.026(2) 0.034(3) -0.0043(19) 0.0023(19) -0.0055(18) C9 0.021(2) 0.035(3) 0.032(3) -0.003(2) -0.0003(19) -0.008(2) C10 0.033(3) 0.031(2) 0.023(2) -0.0002(19) -0.0054(19) -0.010(2) C11 0.027(2) 0.024(2) 0.024(2) 0.0010(18) -0.0002(18) -0.0067(19) C12 0.046(3) 0.044(3) 0.024(2) -0.011(2) 0.004(2) -0.014(2) C13 0.028(2) 0.027(2) 0.025(2) 0.0004(18) 0.0010(19) -0.0092(19) C14 0.035(3) 0.035(3) 0.036(3) -0.004(2) 0.013(2) -0.013(2) C15 0.026(3) 0.046(3) 0.048(3) -0.002(3) 0.006(2) -0.010(2) C16 0.029(3) 0.051(3) 0.040(3) 0.001(2) -0.005(2) -0.013(2) C17 0.033(3) 0.041(3) 0.026(2) -0.002(2) 0.001(2) -0.015(2) C18 0.028(2) 0.027(2) 0.023(2) 0.0015(18) 0.0030(18) -0.0106(19) C19 0.043(3) 0.031(3) 0.025(2) 0.001(2) 0.001(2) -0.019(2) C20 0.060(4) 0.044(3) 0.030(3) -0.007(2) -0.002(2) -0.022(3) C21 0.066(4) 0.031(3) 0.029(3) -0.003(2) -0.004(3) -0.008(3) C22 0.116(7) 0.037(4) 0.061(4) 0.014(3) -0.026(4) -0.016(4) C23 0.031(3) 0.030(3) 0.034(3) -0.004(2) -0.003(2) -0.014(2) C24 0.037(3) 0.024(2) 0.037(3) -0.001(2) 0.000(2) -0.010(2) C25 0.065(7) 0.045(6) 0.088(8) -0.007(5) -0.002(6) -0.024(5) O7 0.105(6) 0.088(6) 0.066(5) 0.007(4) 0.033(5) 0.013(5) C27 0.061(6) 0.026(4) 0.060(12) 0.001(6) -0.005(7) -0.004(3) C29 0.086(8) 0.043(5) 0.054(6) -0.001(4) 0.027(6) -0.006(5) C30 0.036(5) 0.034(4) 0.061(7) 0.000(5) -0.001(4) -0.011(4) C31 0.036(5) 0.054(6) 0.106(8) 0.025(6) 0.000(6) -0.009(4) C32 0.075(7) 0.053(6) 0.058(6) 0.005(5) -0.030(5) -0.007(5) C24' 0.037(3) 0.024(2) 0.037(3) -0.001(2) 0.000(2) -0.010(2) C25' 0.065(7) 0.045(6) 0.088(8) -0.007(5) -0.002(6) -0.024(5) O7' 0.105(6) 0.088(6) 0.066(5) 0.007(4) 0.033(5) 0.013(5) C27' 0.061(6) 0.026(4) 0.060(12) 0.001(6) -0.005(7) -0.004(3) C29' 0.086(8) 0.043(5) 0.054(6) -0.001(4) 0.027(6) -0.006(5) C30' 0.036(5) 0.034(4) 0.061(7) 0.000(5) -0.001(4) -0.011(4) C31' 0.036(5) 0.054(6) 0.106(8) 0.025(6) 0.000(6) -0.009(4) C32' 0.075(7) 0.053(6) 0.058(6) 0.005(5) -0.030(5) -0.007(5) C33 0.143(12) 0.123(12) 0.113(11) -0.071(10) 0.053(9) -0.048(10) C34 0.052(7) 0.057(7) 0.27(2) -0.015(11) 0.031(11) -0.011(6) C35 0.143(12) 0.123(12) 0.113(11) -0.071(10) 0.053(9) -0.048(10) C36 0.052(7) 0.057(7) 0.27(2) -0.015(11) 0.031(11) -0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.069(4) . ? Ni1 O4 2.088(4) . ? Ni1 N5 2.087(4) . ? Ni1 O2 2.109(3) . ? Ni1 O1 2.113(3) . ? Ni1 O3 2.157(4) . ? Ni1 C19 2.435(5) . ? Ni1 C21 2.442(5) . ? S1 O5 1.425(4) . ? S1 O6 1.440(4) . ? S1 N3 1.632(4) . ? S1 C23 1.784(5) . ? N1 C11 1.333(6) . ? N1 C18 1.407(6) . ? N2 C11 1.360(6) . ? N2 C13 1.379(6) . ? N2 C12 1.472(6) . ? N3 C9 1.472(6) . ? N3 C10 1.486(6) . ? N4 C8 1.356(6) . ? N4 C6 1.384(6) . ? N4 C7 1.472(6) . ? N5 C8 1.332(6) . ? N5 C1 1.397(6) . ? O1 C19 1.264(6) . ? O2 C19 1.260(6) . ? O3 C21 1.248(7) . ? O4 C21 1.268(7) . ? C1 C2 1.397(6) . ? C1 C6 1.409(6) . ? C2 C3 1.373(7) . ? C2 H2 0.9601 . ? C3 C4 1.408(7) . ? C3 H3 0.9600 . ? C4 C5 1.375(7) . ? C4 H4 0.9599 . ? C5 C6 1.379(7) . ? C5 H5 0.9599 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.504(6) . ? C9 H9A 0.9599 . ? C9 H9B 0.9601 . ? C10 C11 1.492(6) . ? C10 H10A 0.9599 . ? C10 H10B 0.9602 . ? C12 H12A 0.9600 . ? C12 H12B 0.9599 . ? C12 H12C 0.9600 . ? C13 C14 1.396(7) . ? C13 C18 1.402(6) . ? C14 C15 1.377(8) . ? C14 H14 0.9601 . ? C15 C16 1.401(8) . ? C15 H15 0.9601 . ? C16 C17 1.375(7) . ? C16 H16 0.9601 . ? C17 C18 1.390(7) . ? C17 H17 0.9600 . ? C19 C20 1.500(7) . ? C20 H20A 0.9602 . ? C20 H20B 0.9593 . ? C20 H20C 0.9606 . ? C21 C22 1.510(8) . ? C22 H22A 0.9596 . ? C22 H22B 0.9605 . ? C22 H22C 0.9596 . ? C23 C24 1.519(7) . ? C23 H23A 0.9599 . ? C23 H23B 0.9603 . ? C24 C29 1.445(13) . ? C24 C30 1.590(15) . ? C24 C25 1.595(14) . ? C25 C26 1.540(18) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? O7 C29 1.201(17) . ? C26 C27 1.541(15) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C30 1.50(2) . ? C27 C28 1.521(15) . ? C27 H27A 0.9800 . ? C28 C29 1.565(18) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C30 C31 1.528(19) . ? C30 C32 1.53(2) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C25' C26' 1.541(17) . ? C25' H25C 0.9700 . ? C25' H25D 0.9700 . ? O7' C29' 1.190(15) . ? C26' C27' 1.538(14) . ? C26' H26C 0.9700 . ? C26' H26D 0.9700 . ? C27' C28' 1.557(14) . ? C27' C30' 1.569(19) . ? C27' H27B 0.9800 . ? C28' C29' 1.557(17) . ? C28' H28C 0.9700 . ? C28' H28D 0.9700 . ? C30' C31' 1.516(17) . ? C30' C32' 1.562(18) . ? C31' H31D 0.9600 . ? C31' H31E 0.9600 . ? C31' H31F 0.9600 . ? C32' H32D 0.9600 . ? C32' H32E 0.9600 . ? C32' H32F 0.9600 . ? O8 C33 1.171(16) . ? O8 C34 1.31(3) 2_556 ? O8 C35 1.210(19) . ? C33 O8 1.171(16) 2_556 ? C33 C34 1.57(2) 2_556 ? C33 C34 1.57(2) . ? C34 C35 0.84(3) 2_556 ? C34 O8 1.31(3) 2_556 ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C34 0.84(3) 2_556 ? C35 C36 1.53(3) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? 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 O4 100.89(14) . . ? N1 Ni1 N5 92.88(14) . . ? O4 Ni1 N5 100.50(15) . . ? N1 Ni1 O2 165.72(14) . . ? O4 Ni1 O2 91.40(14) . . ? N5 Ni1 O2 91.98(13) . . ? N1 Ni1 O1 103.48(14) . . ? O4 Ni1 O1 146.17(14) . . ? N5 Ni1 O1 101.32(14) . . ? O2 Ni1 O1 62.37(13) . . ? N1 Ni1 O3 92.74(14) . . ? O4 Ni1 O3 61.92(16) . . ? N5 Ni1 O3 162.29(16) . . ? O2 Ni1 O3 86.61(13) . . ? O1 Ni1 O3 93.66(15) . . ? N1 Ni1 C19 134.64(16) . . ? O4 Ni1 C19 119.57(16) . . ? N5 Ni1 C19 98.58(15) . . ? O2 Ni1 C19 31.15(15) . . ? O1 Ni1 C19 31.24(15) . . ? O3 Ni1 C19 89.32(15) . . ? N1 Ni1 C21 98.99(16) . . ? O4 Ni1 C21 31.27(19) . . ? N5 Ni1 C21 131.66(19) . . ? O2 Ni1 C21 87.71(15) . . ? O1 Ni1 C21 120.64(18) . . ? O3 Ni1 C21 30.68(18) . . ? C19 Ni1 C21 105.21(17) . . ? O5 S1 O6 119.3(2) . . ? O5 S1 N3 106.6(2) . . ? O6 S1 N3 106.4(2) . . ? O5 S1 C23 109.8(2) . . ? O6 S1 C23 109.0(2) . . ? N3 S1 C23 104.6(2) . . ? C11 N1 C18 105.3(4) . . ? C11 N1 Ni1 128.7(3) . . ? C18 N1 Ni1 125.9(3) . . ? C11 N2 C13 107.6(4) . . ? C11 N2 C12 129.2(4) . . ? C13 N2 C12 123.1(4) . . ? C9 N3 C10 120.8(4) . . ? C9 N3 S1 119.5(3) . . ? C10 N3 S1 118.6(3) . . ? C8 N4 C6 107.9(4) . . ? C8 N4 C7 128.2(4) . . ? C6 N4 C7 123.9(4) . . ? C8 N5 C1 105.6(4) . . ? C8 N5 Ni1 124.9(3) . . ? C1 N5 Ni1 128.4(3) . . ? C19 O1 Ni1 88.6(3) . . ? C19 O2 Ni1 88.9(3) . . ? C21 O3 Ni1 87.4(3) . . ? C21 O4 Ni1 90.0(3) . . ? N5 C1 C2 131.6(4) . . ? N5 C1 C6 109.1(4) . . ? C2 C1 C6 119.4(4) . . ? C3 C2 C1 117.7(4) . . ? C3 C2 H2 123.2 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 121.9(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 118.0 . . ? C5 C4 C3 121.3(5) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 116.7(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 124.0 . . ? C5 C6 N4 131.7(4) . . ? C5 C6 C1 123.1(4) . . ? N4 C6 C1 105.3(4) . . ? N4 C7 H7A 109.2 . . ? N4 C7 H7B 109.7 . . ? H7A C7 H7B 109.5 . . ? N4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N5 C8 N4 112.1(4) . . ? N5 C8 C9 125.3(4) . . ? N4 C8 C9 122.6(4) . . ? N3 C9 C8 115.9(4) . . ? N3 C9 H9A 109.4 . . ? C8 C9 H9A 106.3 . . ? N3 C9 H9B 109.6 . . ? C8 C9 H9B 106.0 . . ? H9A C9 H9B 109.5 . . ? N3 C10 C11 113.5(4) . . ? N3 C10 H10A 109.5 . . ? C11 C10 H10A 107.1 . . ? N3 C10 H10B 109.8 . . ? C11 C10 H10B 107.3 . . ? H10A C10 H10B 109.5 . . ? N1 C11 N2 112.2(4) . . ? N1 C11 C10 124.0(4) . . ? N2 C11 C10 123.5(4) . . ? N2 C12 H12A 109.9 . . ? N2 C12 H12B 109.0 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 131.2(4) . . ? N2 C13 C18 106.0(4) . . ? C14 C13 C18 122.7(4) . . ? C15 C14 C13 115.9(5) . . ? C15 C14 H14 124.6 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 121.6(5) . . ? C14 C15 H15 119.1 . . ? C16 C15 H15 119.3 . . ? C17 C16 C15 122.3(5) . . ? C17 C16 H16 118.2 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 117.0(5) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 123.4 . . ? C17 C18 C13 120.3(4) . . ? C17 C18 N1 130.9(4) . . ? C13 C18 N1 108.8(4) . . ? O2 C19 O1 120.0(4) . . ? O2 C19 C20 120.7(5) . . ? O1 C19 C20 119.2(5) . . ? O2 C19 Ni1 60.0(2) . . ? O1 C19 Ni1 60.1(2) . . ? C20 C19 Ni1 178.1(4) . . ? C19 C20 H20A 109.7 . . ? C19 C20 H20B 109.0 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.7 . . ? H20A C20 H20C 109.4 . . ? H20B C20 H20C 109.5 . . ? O3 C21 O4 120.5(5) . . ? O3 C21 C22 120.1(6) . . ? O4 C21 C22 119.4(6) . . ? O3 C21 Ni1 61.9(3) . . ? O4 C21 Ni1 58.7(3) . . ? C22 C21 Ni1 177.3(5) . . ? C21 C22 H22A 108.8 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 109.4 . . ? C21 C22 H22C 109.8 . . ? H22A C22 H22C 109.6 . . ? H22B C22 H22C 109.6 . . ? C24 C23 S1 118.2(3) . . ? C24 C23 H23A 104.7 . . ? S1 C23 H23A 109.3 . . ? C24 C23 H23B 105.2 . . ? S1 C23 H23B 109.6 . . ? H23A C23 H23B 109.5 . . ? C29 C24 C23 116.9(7) . . ? C29 C24 C30 103.0(10) . . ? C23 C24 C30 114.4(6) . . ? C29 C24 C25 101.7(11) . . ? C23 C24 C25 118.1(7) . . ? C30 C24 C25 100.2(8) . . ? C26 C25 C24 103.1(11) . . ? C26 C25 H25A 111.1 . . ? C24 C25 H25A 111.1 . . ? C26 C25 H25B 111.1 . . ? C24 C25 H25B 111.1 . . ? H25A C25 H25B 109.1 . . ? C25 C26 C27 104.4(12) . . ? C25 C26 H26A 110.9 . . ? C27 C26 H26A 110.9 . . ? C25 C26 H26B 110.9 . . ? C27 C26 H26B 110.9 . . ? H26A C26 H26B 108.9 . . ? C30 C27 C28 104.3(13) . . ? C30 C27 C26 102.7(12) . . ? C28 C27 C26 100.3(17) . . ? C30 C27 H27A 115.8 . . ? C28 C27 H27A 115.8 . . ? C26 C27 H27A 115.8 . . ? C27 C28 C29 103.1(12) . . ? C27 C28 H28A 111.1 . . ? C29 C28 H28A 111.1 . . ? C27 C28 H28B 111.1 . . ? C29 C28 H28B 111.1 . . ? H28A C28 H28B 109.1 . . ? O7 C29 C24 126.1(13) . . ? O7 C29 C28 127.2(14) . . ? C24 C29 C28 105.0(11) . . ? C27 C30 C31 113.5(13) . . ? C27 C30 C32 113.3(13) . . ? C31 C30 C32 108.9(14) . . ? C27 C30 C24 95.4(11) . . ? C31 C30 C24 111.0(12) . . ? C32 C30 C24 114.2(10) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C26' C25' H25C 111.2 . . ? C26' C25' H25D 111.2 . . ? H25C C25' H25D 109.1 . . ? C27' C26' C25' 104.1(10) . . ? C27' C26' H26C 110.9 . . ? C25' C26' H26C 110.9 . . ? C27' C26' H26D 110.9 . . ? C25' C26' H26D 110.9 . . ? H26C C26' H26D 109.0 . . ? C26' C27' C28' 106.9(14) . . ? C26' C27' C30' 101.5(10) . . ? C28' C27' C30' 104.3(10) . . ? C26' C27' H27B 114.3 . . ? C28' C27' H27B 114.3 . . ? C30' C27' H27B 114.3 . . ? C27' C28' C29' 99.1(10) . . ? C27' C28' H28C 111.9 . . ? C29' C28' H28C 111.9 . . ? C27' C28' H28D 111.9 . . ? C29' C28' H28D 111.9 . . ? H28C C28' H28D 109.6 . . ? O7' C29' C28' 123.3(11) . . ? C31' C30' C32' 106.3(11) . . ? C31' C30' C27' 115.0(10) . . ? C32' C30' C27' 114.5(10) . . ? C30' C31' H31D 109.5 . . ? C30' C31' H31E 109.5 . . ? H31D C31' H31E 109.5 . . ? C30' C31' H31F 109.5 . . ? H31D C31' H31F 109.5 . . ? H31E C31' H31F 109.5 . . ? C30' C32' H32D 109.5 . . ? C30' C32' H32E 109.5 . . ? H32D C32' H32E 109.5 . . ? C30' C32' H32F 109.5 . . ? H32D C32' H32F 109.5 . . ? H32E C32' H32F 109.5 . . ? C33 O8 C34 78.3(17) . 2_556 ? C33 O8 C35 112(2) . . ? C34 O8 C35 38.7(17) 2_556 . ? O8 C33 O8 180.000(4) . 2_556 ? O8 C33 C34 54.9(12) . 2_556 ? O8 C33 C34 125.1(12) 2_556 2_556 ? O8 C33 C34 125.1(12) . . ? O8 C33 C34 54.9(12) 2_556 . ? C34 C33 C34 180.0(16) 2_556 . ? C35 C34 O8 63.9(19) 2_556 2_556 ? C35 C34 C33 105(3) 2_556 . ? O8 C34 C33 46.8(11) 2_556 . ? C35 C34 H34A 109.5 2_556 . ? O8 C34 H34A 69.5 2_556 . ? C33 C34 H34A 72.3 . . ? C35 C34 H34B 109.5 2_556 . ? O8 C34 H34B 171.4 2_556 . ? C33 C34 H34B 141.7 . . ? H34A C34 H34B 109.5 . . ? C35 C34 H34C 109.5 2_556 . ? O8 C34 H34C 78.6 2_556 . ? C33 C34 H34C 41.8 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C34 C35 O8 77(3) 2_556 . ? C34 C35 C36 132(4) 2_556 . ? O8 C35 C36 99(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.691 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.127 data_complex_7 _database_code_depnum_ccdc_archive 'CCDC 618814' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H53 Cl N10 Ni2 O13' _chemical_formula_sum 'C42 H53 Cl N10 Ni2 O13' _chemical_formula_weight 1058.81 _chemical_absolute_configuration unk 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 16.0340(4) _cell_length_b 22.0010(6) _cell_length_c 16.1850(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.247(2) _cell_angle_gamma 90.00 _cell_volume 5533.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 86418 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour 'pale blue' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8412 _exptl_absorpt_correction_T_max 0.8919 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39313 _diffrn_reflns_av_R_equivalents 0.0863 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9749 _reflns_number_gt 5568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & M 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1580P)^2^+8.6161P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9749 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1578 _refine_ls_R_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.3015 _refine_ls_wR_factor_gt 0.2538 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.91598(5) 0.18544(4) 0.52308(6) 0.0404(3) Uani 1 1 d . . . Ni2 Ni 1.07896(5) 0.18582(4) 0.45386(6) 0.0410(3) Uani 1 1 d . . . Cl1 Cl 0.36799(13) 0.00406(8) 0.35639(14) 0.0543(5) Uani 1 1 d . . . O1 O 0.9487(3) 0.1630(2) 0.4100(3) 0.0498(13) Uani 1 1 d . . . O2 O 0.8801(6) 0.1121(3) 0.2955(5) 0.116(3) Uani 1 1 d . . . O3 O 0.9400(3) 0.2753(2) 0.5172(3) 0.0447(12) Uani 1 1 d . . . O4 O 1.0569(3) 0.2754(2) 0.4638(3) 0.0445(12) Uani 1 1 d . . . O5 O 1.0443(3) 0.1588(3) 0.5652(3) 0.0525(13) Uani 1 1 d . . . O6 O 1.1067(6) 0.1023(3) 0.6758(5) 0.112(3) Uani 1 1 d . . . O7 O 0.3426(7) 0.0600(3) 0.3831(6) 0.138(4) Uani 1 1 d . . . O8 O 0.3331(6) -0.0448(4) 0.3930(6) 0.124(3) Uani 1 1 d . . . O9 O 0.3359(9) 0.0015(4) 0.2673(6) 0.168(6) Uani 1 1 d . . . O10 O 0.4543(5) -0.0011(4) 0.3745(9) 0.154(5) Uani 1 1 d . . . O11 O 0.5529(4) 0.5137(3) 0.0946(4) 0.085(2) Uani 1 1 d . . . H11A H 0.5590 0.4689 0.0841 0.102 Uiso 1 1 d R . . H11B H 0.5756 0.5310 0.1500 0.102 Uiso 1 1 d R . . O12 O 0.073(4) 0.0010(7) 0.8366(14) 0.38(4) Uani 0.50 1 d P . . H12D H 0.1283 0.0011 0.8759 0.451 Uiso 0.50 1 d PR . . H12E H 0.0216 0.0011 0.8575 0.451 Uiso 0.50 1 d PR . . O13 O 0.312(3) 0.0018(9) 0.0557(18) 0.234(17) Uani 0.50 1 d P . . H13A H 0.3388 0.0018 0.0089 0.281 Uiso 0.50 1 d PR . . H13B H 0.3466 0.0018 0.1132 0.281 Uiso 0.50 1 d PR . . O14 O 0.672(2) 0.1076(17) 0.2106(18) 0.29(2) Uani 0.50 1 d P . . H14B H 0.7062 0.1124 0.1695 0.349 Uiso 0.50 1 d PR . . H14C H 0.6989 0.1124 0.2703 0.349 Uiso 0.50 1 d PR . . O15 O 0.305(2) 0.0884(19) 0.754(2) 0.34(3) Uani 0.50 1 d P . . H15B H 0.3660 0.0919 0.7757 0.404 Uiso 0.50 1 d PR . . H15C H 0.2678 0.0919 0.7925 0.404 Uiso 0.50 1 d PR . . N1 N 0.7867(4) 0.1957(3) 0.4689(4) 0.0428(14) Uani 1 1 d . . . N2 N 0.6576(4) 0.1546(3) 0.4309(4) 0.0506(16) Uani 1 1 d . . . N3 N 0.8741(4) 0.0925(3) 0.5343(4) 0.0488(15) Uani 1 1 d . . . H3A H 0.9134 0.0650 0.5176 0.059 Uiso 1 1 d R . . N4 N 0.8545(3) 0.1434(3) 0.7479(3) 0.0432(14) Uani 1 1 d . . . N5 N 0.8944(3) 0.1898(3) 0.6420(3) 0.0399(13) Uani 1 1 d . . . N6 N 1.2075(4) 0.1941(3) 0.5093(4) 0.0449(15) Uani 1 1 d . . . N7 N 1.3352(4) 0.1493(3) 0.5520(4) 0.0549(17) Uani 1 1 d . . . N8 N 1.1191(4) 0.0931(3) 0.4378(4) 0.0497(16) Uani 1 1 d . . . H8 H 1.0766 0.0654 0.4484 0.060 Uiso 1 1 d R . . N9 N 1.1433(4) 0.1503(3) 0.2286(4) 0.0475(15) Uani 1 1 d . . . N10 N 1.1025(4) 0.1934(3) 0.3351(4) 0.0454(15) Uani 1 1 d . . . C1 C 0.7270(4) 0.2428(3) 0.4488(4) 0.0435(17) Uani 1 1 d . . . C2 C 0.7370(5) 0.3051(3) 0.4513(5) 0.0467(18) Uani 1 1 d . . . H2 H 0.7935 0.3226 0.4676 0.056 Uiso 1 1 d R . . C3 C 0.6645(5) 0.3397(4) 0.4302(5) 0.056(2) Uani 1 1 d . . . H3 H 0.6689 0.3832 0.4307 0.067 Uiso 1 1 d R . . C4 C 0.5819(6) 0.3140(4) 0.4065(5) 0.068(2) Uani 1 1 d . . . H4 H 0.5333 0.3410 0.3933 0.081 Uiso 1 1 d R . . C5 C 0.5700(5) 0.2518(4) 0.4039(5) 0.059(2) Uani 1 1 d . . . H5 H 0.5149 0.2321 0.3879 0.071 Uiso 1 1 d R . . C6 C 0.6450(4) 0.2161(4) 0.4247(4) 0.0448(18) Uani 1 1 d . . . C7 C 0.5891(5) 0.1068(4) 0.4135(6) 0.073(3) Uani 1 1 d . . . H7A H 0.6146 0.0671 0.4216 0.088 Uiso 1 1 d R . . H7B H 0.5558 0.1108 0.3557 0.088 Uiso 1 1 d R . . H7C H 0.5525 0.1124 0.4517 0.088 Uiso 1 1 d R . . C8 C 0.7433(5) 0.1445(3) 0.4595(4) 0.0453(18) Uani 1 1 d . . . C9 C 0.7873(5) 0.0842(3) 0.4770(5) 0.0519(19) Uani 1 1 d . . . H9A H 0.7919 0.0656 0.4247 0.062 Uiso 1 1 d R . . H9B H 0.7538 0.0587 0.5046 0.062 Uiso 1 1 d R . . C10 C 0.8784(5) 0.0801(3) 0.6254(5) 0.053(2) Uani 1 1 d . . . H10A H 0.8298 0.0557 0.6291 0.064 Uiso 1 1 d R . . H10B H 0.9306 0.0590 0.6515 0.064 Uiso 1 1 d R . . C11 C 0.8747(5) 0.1372(3) 0.6714(5) 0.0460(18) Uani 1 1 d . . . C12 C 0.8329(5) 0.0964(4) 0.8018(5) 0.059(2) Uani 1 1 d . . . H12A H 0.8350 0.0582 0.7737 0.071 Uiso 1 1 d R . . H12B H 0.7761 0.1029 0.8093 0.071 Uiso 1 1 d R . . H12C H 0.8735 0.0960 0.8564 0.071 Uiso 1 1 d R . . C13 C 0.8592(4) 0.2041(4) 0.7672(4) 0.0429(18) Uani 1 1 d . . . C14 C 0.8397(4) 0.2381(4) 0.8343(4) 0.051(2) Uani 1 1 d . . . H14A H 0.8223 0.2179 0.8798 0.061 Uiso 1 1 d R . . C15 C 0.8472(5) 0.2995(4) 0.8316(5) 0.051(2) Uani 1 1 d . . . H15A H 0.8337 0.3228 0.8767 0.061 Uiso 1 1 d R . . C16 C 0.8738(5) 0.3296(4) 0.7649(4) 0.0479(18) Uani 1 1 d . . . H16 H 0.8791 0.3731 0.7659 0.057 Uiso 1 1 d R . . C17 C 0.8918(4) 0.2967(4) 0.6984(5) 0.0456(18) Uani 1 1 d . . . H17 H 0.9100 0.3158 0.6526 0.055 Uiso 1 1 d R . . C18 C 0.8843(4) 0.2340(3) 0.6999(4) 0.0414(17) Uani 1 1 d . . . C19 C 1.2686(5) 0.2385(4) 0.5317(4) 0.0434(17) Uani 1 1 d . . . C20 C 1.2612(5) 0.3011(4) 0.5303(5) 0.054(2) Uani 1 1 d . . . H20 H 1.2057 0.3201 0.5132 0.065 Uiso 1 1 d R . . C21 C 1.3349(6) 0.3352(4) 0.5536(5) 0.061(2) Uani 1 1 d . . . H21 H 1.3319 0.3788 0.5537 0.073 Uiso 1 1 d R . . C22 C 1.4167(6) 0.3077(5) 0.5786(6) 0.075(3) Uani 1 1 d . . . H22 H 1.4685 0.3315 0.5931 0.090 Uiso 1 1 d R . . C23 C 1.4250(6) 0.2453(5) 0.5823(5) 0.067(2) Uani 1 1 d . . . H23 H 1.4799 0.2258 0.6015 0.081 Uiso 1 1 d R . . C24 C 1.3495(5) 0.2115(4) 0.5585(4) 0.0487(19) Uani 1 1 d . . . C25 C 1.4019(6) 0.1022(5) 0.5746(6) 0.078(3) Uani 1 1 d . . . H25A H 1.4570 0.1212 0.5947 0.094 Uiso 1 1 d R . . H25B H 1.4023 0.0774 0.5259 0.094 Uiso 1 1 d R . . H25C H 1.3898 0.0772 0.6189 0.094 Uiso 1 1 d R . . C26 C 1.2487(5) 0.1413(4) 0.5209(4) 0.0487(19) Uani 1 1 d . . . C27 C 1.2029(5) 0.0820(3) 0.5006(5) 0.054(2) Uani 1 1 d . . . H27A H 1.1919 0.0653 0.5517 0.065 Uiso 1 1 d R . . H27B H 1.2375 0.0541 0.4777 0.065 Uiso 1 1 d R . . C28 C 1.1189(5) 0.0822(4) 0.3467(5) 0.056(2) Uani 1 1 d . . . H28A H 1.1682 0.0585 0.3434 0.067 Uiso 1 1 d R . . H28B H 1.0674 0.0610 0.3183 0.067 Uiso 1 1 d R . . C29 C 1.1230(4) 0.1420(3) 0.3032(4) 0.0410(17) Uani 1 1 d . . . C30 C 1.1677(5) 0.1025(4) 0.1750(5) 0.058(2) Uani 1 1 d . . . H30A H 1.1790 0.1209 0.1250 0.069 Uiso 1 1 d R . . H30B H 1.1220 0.0734 0.1583 0.069 Uiso 1 1 d R . . H30C H 1.2187 0.0823 0.2067 0.069 Uiso 1 1 d R . . C31 C 1.1392(4) 0.2119(3) 0.2122(4) 0.0408(16) Uani 1 1 d . . . C32 C 1.1568(4) 0.2460(4) 0.1459(4) 0.0477(18) Uani 1 1 d . . . H32 H 1.1720 0.2265 0.0986 0.057 Uiso 1 1 d R . . C33 C 1.1488(4) 0.3071(4) 0.1506(5) 0.051(2) Uani 1 1 d . . . H33 H 1.1631 0.3310 0.1064 0.061 Uiso 1 1 d R . . C34 C 1.1226(4) 0.3359(4) 0.2187(4) 0.0471(18) Uani 1 1 d . . . H34 H 1.1171 0.3793 0.2203 0.057 Uiso 1 1 d R . . C35 C 1.1039(5) 0.3016(3) 0.2829(5) 0.0481(19) Uani 1 1 d . . . H35 H 1.0850 0.3197 0.3291 0.058 Uiso 1 1 d R . . C36 C 1.1125(4) 0.2384(3) 0.2791(4) 0.0390(16) Uani 1 1 d . . . C37 C 0.9987(5) 0.3012(3) 0.4898(5) 0.0471(18) Uani 1 1 d . . . C38 C 0.9990(6) 0.3688(4) 0.4901(7) 0.097(4) Uani 1 1 d . . . H38A H 1.0464 0.3827 0.4686 0.116 Uiso 1 1 d R . . H38B H 1.0059 0.3830 0.5474 0.116 Uiso 1 1 d R . . H38C H 0.9461 0.3841 0.4548 0.116 Uiso 1 1 d R . . C39 C 1.0893(6) 0.1520(4) 0.6408(5) 0.060(2) Uani 1 1 d . . . C40 C 1.1213(7) 0.2088(5) 0.6855(6) 0.085(3) Uani 1 1 d . . . H40A H 1.1547 0.1984 0.7415 0.101 Uiso 1 1 d R . . H40B H 1.0738 0.2340 0.6901 0.101 Uiso 1 1 d R . . H40C H 1.1567 0.2304 0.6554 0.101 Uiso 1 1 d R . . C41 C 0.9002(5) 0.1616(5) 0.3329(6) 0.063(2) Uani 1 1 d . . . C42 C 0.8705(6) 0.2196(4) 0.2914(6) 0.077(3) Uani 1 1 d . . . H42A H 0.8345 0.2122 0.2355 0.092 Uiso 1 1 d R . . H42B H 0.9200 0.2426 0.2867 0.092 Uiso 1 1 d R . . H42C H 0.8388 0.2422 0.3243 0.092 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0300(5) 0.0448(6) 0.0507(6) 0.0018(4) 0.0180(4) 0.0000(4) Ni2 0.0293(5) 0.0478(6) 0.0500(6) 0.0044(4) 0.0176(4) 0.0020(4) Cl1 0.0461(12) 0.0485(11) 0.0754(14) 0.0009(10) 0.0284(10) 0.0003(10) O1 0.037(3) 0.067(3) 0.048(3) 0.000(2) 0.014(2) 0.001(3) O2 0.155(8) 0.082(5) 0.089(5) -0.020(4) -0.013(5) -0.015(5) O3 0.038(3) 0.044(3) 0.058(3) -0.002(2) 0.023(2) 0.000(2) O4 0.037(3) 0.045(3) 0.060(3) 0.002(2) 0.027(2) -0.002(2) O5 0.034(3) 0.081(4) 0.047(3) 0.019(3) 0.018(2) 0.012(3) O6 0.137(7) 0.091(5) 0.098(5) 0.048(4) 0.011(5) 0.028(5) O7 0.222(11) 0.069(5) 0.174(8) 0.009(5) 0.142(8) 0.035(6) O8 0.155(8) 0.094(6) 0.155(7) 0.018(5) 0.100(6) -0.020(5) O9 0.245(14) 0.114(8) 0.101(7) 0.005(5) -0.042(8) -0.042(6) O10 0.032(4) 0.157(9) 0.267(13) 0.011(7) 0.023(6) -0.004(5) O11 0.057(4) 0.127(6) 0.072(4) -0.005(4) 0.019(3) -0.014(4) O12 0.89(10) 0.060(12) 0.094(14) -0.046(10) -0.04(3) -0.07(2) O13 0.41(5) 0.19(3) 0.15(2) 0.010(15) 0.15(3) 0.04(2) O14 0.30(4) 0.41(5) 0.19(2) -0.08(3) 0.10(2) -0.25(4) O15 0.28(4) 0.48(6) 0.31(4) 0.27(4) 0.18(3) 0.23(4) N1 0.031(3) 0.053(4) 0.049(3) 0.001(3) 0.019(3) -0.003(3) N2 0.035(4) 0.066(5) 0.054(4) -0.007(3) 0.016(3) -0.013(3) N3 0.040(4) 0.046(4) 0.069(4) 0.002(3) 0.029(3) 0.002(3) N4 0.030(3) 0.054(4) 0.048(3) 0.007(3) 0.013(3) 0.002(3) N5 0.030(3) 0.045(3) 0.048(3) -0.002(3) 0.018(3) -0.004(3) N6 0.036(4) 0.055(4) 0.048(3) 0.007(3) 0.018(3) 0.004(3) N7 0.036(4) 0.074(5) 0.057(4) 0.011(3) 0.016(3) 0.018(4) N8 0.044(4) 0.044(4) 0.067(4) 0.011(3) 0.024(3) 0.005(3) N9 0.035(4) 0.063(4) 0.047(3) -0.008(3) 0.017(3) 0.005(3) N10 0.030(3) 0.059(4) 0.051(3) 0.002(3) 0.017(3) 0.002(3) C1 0.033(4) 0.058(5) 0.040(4) -0.001(3) 0.010(3) 0.003(4) C2 0.036(4) 0.051(5) 0.054(4) -0.004(4) 0.012(3) -0.002(4) C3 0.045(5) 0.062(5) 0.062(5) 0.014(4) 0.016(4) 0.012(4) C4 0.055(6) 0.077(7) 0.069(6) 0.007(5) 0.012(4) 0.022(5) C5 0.029(4) 0.087(7) 0.059(5) 0.000(4) 0.006(3) 0.000(4) C6 0.030(4) 0.063(5) 0.043(4) -0.004(4) 0.012(3) -0.007(4) C7 0.048(6) 0.077(6) 0.091(7) -0.007(5) 0.010(4) -0.021(5) C8 0.036(4) 0.051(5) 0.054(4) -0.007(4) 0.021(3) -0.010(4) C9 0.051(5) 0.046(4) 0.065(5) -0.007(4) 0.025(4) -0.009(4) C10 0.047(5) 0.042(4) 0.074(5) 0.005(4) 0.022(4) 0.002(4) C11 0.037(4) 0.046(4) 0.057(5) 0.010(4) 0.013(3) 0.003(4) C12 0.060(6) 0.063(5) 0.056(5) 0.019(4) 0.018(4) -0.008(4) C13 0.027(4) 0.064(5) 0.038(4) 0.008(3) 0.010(3) 0.006(3) C14 0.031(4) 0.079(6) 0.043(4) 0.001(4) 0.012(3) -0.003(4) C15 0.037(4) 0.074(6) 0.042(4) -0.010(4) 0.011(3) -0.002(4) C16 0.038(4) 0.056(5) 0.052(4) 0.002(4) 0.016(3) 0.003(4) C17 0.027(4) 0.061(5) 0.053(4) 0.003(4) 0.018(3) 0.004(3) C18 0.029(4) 0.055(5) 0.043(4) 0.007(3) 0.013(3) 0.003(3) C19 0.031(4) 0.062(5) 0.041(4) -0.001(3) 0.017(3) -0.001(4) C20 0.044(5) 0.068(6) 0.053(5) -0.007(4) 0.018(4) -0.008(4) C21 0.056(6) 0.063(5) 0.065(5) -0.009(4) 0.015(4) -0.004(5) C22 0.040(5) 0.103(8) 0.081(6) -0.012(6) 0.012(4) -0.024(6) C23 0.039(5) 0.106(8) 0.055(5) -0.005(5) 0.010(4) 0.006(5) C24 0.028(4) 0.075(6) 0.046(4) 0.005(4) 0.014(3) 0.005(4) C25 0.048(6) 0.096(7) 0.084(6) 0.004(5) 0.005(4) 0.028(5) C26 0.036(5) 0.066(5) 0.050(4) 0.016(4) 0.023(3) 0.010(4) C27 0.051(5) 0.050(5) 0.068(5) 0.014(4) 0.024(4) 0.020(4) C28 0.050(5) 0.055(5) 0.065(5) -0.006(4) 0.021(4) 0.008(4) C29 0.028(4) 0.041(4) 0.058(4) 0.004(3) 0.020(3) 0.005(3) C30 0.057(5) 0.061(5) 0.056(5) -0.012(4) 0.016(4) 0.003(4) C31 0.027(4) 0.047(4) 0.050(4) -0.001(3) 0.011(3) 0.001(3) C32 0.039(4) 0.065(5) 0.043(4) 0.000(4) 0.016(3) -0.008(4) C33 0.031(4) 0.076(6) 0.046(4) 0.010(4) 0.011(3) -0.011(4) C34 0.037(4) 0.059(5) 0.045(4) 0.009(4) 0.010(3) -0.006(4) C35 0.036(4) 0.056(5) 0.054(4) -0.001(4) 0.014(3) -0.001(4) C36 0.024(4) 0.051(5) 0.044(4) 0.005(3) 0.014(3) -0.003(3) C37 0.041(4) 0.045(4) 0.058(5) 0.002(3) 0.018(4) -0.008(4) C38 0.092(8) 0.053(6) 0.170(11) 0.003(6) 0.079(8) 0.005(5) C39 0.067(6) 0.064(6) 0.056(5) 0.012(5) 0.027(4) 0.002(5) C40 0.077(7) 0.112(8) 0.072(6) 0.003(6) 0.032(5) -0.003(6) C41 0.044(5) 0.080(6) 0.069(6) -0.010(5) 0.021(4) -0.009(5) C42 0.084(7) 0.084(7) 0.069(6) 0.007(5) 0.031(5) 0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3 2.022(5) . ? Ni1 N5 2.040(5) . ? Ni1 N1 2.055(6) . ? Ni1 O1 2.083(5) . ? Ni1 O5 2.085(5) . ? Ni1 N3 2.174(6) . ? Ni2 O4 2.015(5) . ? Ni2 N6 2.043(6) . ? Ni2 N10 2.055(6) . ? Ni2 O1 2.095(5) . ? Ni2 O5 2.098(5) . ? Ni2 N8 2.173(6) . ? Cl1 O10 1.348(8) . ? Cl1 O7 1.398(7) . ? Cl1 O8 1.408(7) . ? Cl1 O9 1.408(10) . ? O1 C41 1.298(10) . ? O2 C41 1.249(11) . ? O3 C37 1.268(8) . ? O4 C37 1.251(8) . ? O5 C39 1.267(9) . ? O6 C39 1.231(10) . ? O11 H11A 1.0080 . ? O11 H11B 0.9600 . ? O12 H12D 0.9594 . ? O12 H12E 0.9601 . ? O13 H13A 0.9595 . ? O13 H13B 0.9596 . ? O14 H14B 0.9605 . ? O14 H14C 0.9604 . ? O15 H15B 0.9600 . ? O15 H15C 0.9700 . ? N1 C8 1.311(9) . ? N1 C1 1.394(9) . ? N2 C8 1.357(9) . ? N2 C6 1.366(10) . ? N2 C7 1.497(10) . ? N3 C9 1.481(9) . ? N3 C10 1.484(9) . ? N3 H3A 0.9592 . ? N4 C11 1.363(9) . ? N4 C13 1.369(9) . ? N4 C12 1.449(9) . ? N5 C11 1.319(8) . ? N5 C18 1.387(9) . ? N6 C26 1.327(9) . ? N6 C19 1.368(9) . ? N7 C26 1.364(9) . ? N7 C24 1.387(10) . ? N7 C25 1.470(10) . ? N8 C27 1.491(9) . ? N8 C28 1.493(9) . ? N8 H8 0.9606 . ? N9 C29 1.338(8) . ? N9 C31 1.379(9) . ? N9 C30 1.478(9) . ? N10 C29 1.318(8) . ? N10 C36 1.377(9) . ? C1 C2 1.380(10) . ? C1 C6 1.405(9) . ? C2 C3 1.362(10) . ? C2 H2 0.9596 . ? C3 C4 1.403(12) . ? C3 H3 0.9595 . ? C4 C5 1.381(12) . ? C4 H4 0.9611 . ? C5 C6 1.407(11) . ? C5 H5 0.9606 . ? C7 H7A 0.9596 . ? C7 H7B 0.9603 . ? C7 H7C 0.9595 . ? C8 C9 1.497(10) . ? C9 H9A 0.9592 . ? C9 H9B 0.9596 . ? C10 C11 1.468(10) . ? C10 H10A 0.9602 . ? C10 H10B 0.9594 . ? C12 H12A 0.9601 . ? C12 H12B 0.9585 . ? C12 H12C 0.9601 . ? C13 C18 1.413(9) . ? C13 C14 1.414(10) . ? C14 C15 1.357(11) . ? C14 H14A 0.9585 . ? C15 C16 1.418(10) . ? C15 H15A 0.9593 . ? C16 C17 1.385(10) . ? C16 H16 0.9606 . ? C17 C18 1.386(10) . ? C17 H17 0.9580 . ? C19 C20 1.383(11) . ? C19 C24 1.395(10) . ? C20 C21 1.371(11) . ? C20 H20 0.9602 . ? C21 C22 1.410(12) . ? C21 H21 0.9605 . ? C22 C23 1.380(13) . ? C22 H22 0.9608 . ? C23 C24 1.391(11) . ? C23 H23 0.9596 . ? C25 H25A 0.9589 . ? C25 H25B 0.9599 . ? C25 H25C 0.9606 . ? C26 C27 1.494(11) . ? C27 H27A 0.9602 . ? C27 H27B 0.9608 . ? C28 C29 1.501(10) . ? C28 H28A 0.9594 . ? C28 H28B 0.9612 . ? C30 H30A 0.9611 . ? C30 H30B 0.9604 . ? C30 H30C 0.9607 . ? C31 C36 1.387(9) . ? C31 C32 1.394(10) . ? C32 C33 1.353(10) . ? C32 H32 0.9599 . ? C33 C34 1.422(11) . ? C33 H33 0.9599 . ? C34 C35 1.376(10) . ? C34 H34 0.9596 . ? C35 C36 1.402(10) . ? C35 H35 0.9597 . ? C37 C38 1.487(12) . ? C38 H38A 0.9604 . ? C38 H38B 0.9590 . ? C38 H38C 0.9595 . ? C39 C40 1.471(13) . ? C40 H40A 0.9601 . ? C40 H40B 0.9596 . ? C40 H40C 0.9599 . ? C41 C42 1.466(13) . ? C42 H42A 0.9598 . ? C42 H42B 0.9599 . ? C42 H42C 0.9604 . ? 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 O3 Ni1 N5 94.4(2) . . ? O3 Ni1 N1 93.3(2) . . ? N5 Ni1 N1 90.6(2) . . ? O3 Ni1 O1 95.6(2) . . ? N5 Ni1 O1 167.9(2) . . ? N1 Ni1 O1 95.5(2) . . ? O3 Ni1 O5 96.1(2) . . ? N5 Ni1 O5 95.0(2) . . ? N1 Ni1 O5 168.7(2) . . ? O1 Ni1 O5 77.27(19) . . ? O3 Ni1 N3 172.1(2) . . ? N5 Ni1 N3 80.7(2) . . ? N1 Ni1 N3 80.7(2) . . ? O1 Ni1 N3 90.0(2) . . ? O5 Ni1 N3 90.5(2) . . ? O4 Ni2 N6 93.2(2) . . ? O4 Ni2 N10 94.1(2) . . ? N6 Ni2 N10 90.4(2) . . ? O4 Ni2 O1 94.7(2) . . ? N6 Ni2 O1 169.7(2) . . ? N10 Ni2 O1 95.7(2) . . ? O4 Ni2 O5 96.8(2) . . ? N6 Ni2 O5 95.7(2) . . ? N10 Ni2 O5 167.1(2) . . ? O1 Ni2 O5 76.72(19) . . ? O4 Ni2 N8 171.9(2) . . ? N6 Ni2 N8 80.8(2) . . ? N10 Ni2 N8 80.6(2) . . ? O1 Ni2 N8 92.0(2) . . ? O5 Ni2 N8 89.2(2) . . ? O10 Cl1 O7 111.7(6) . . ? O10 Cl1 O8 109.7(6) . . ? O7 Cl1 O8 111.5(5) . . ? O10 Cl1 O9 108.5(9) . . ? O7 Cl1 O9 106.9(6) . . ? O8 Cl1 O9 108.5(6) . . ? C41 O1 Ni1 129.1(5) . . ? C41 O1 Ni2 130.0(5) . . ? Ni1 O1 Ni2 95.2(2) . . ? C37 O3 Ni1 128.4(5) . . ? C37 O4 Ni2 129.1(4) . . ? C39 O5 Ni1 129.1(5) . . ? C39 O5 Ni2 130.9(5) . . ? Ni1 O5 Ni2 95.08(19) . . ? H11A O11 H11B 121.0 . . ? H12D O12 H12E 120.0 . . ? H13A O13 H13B 120.0 . . ? H14B O14 H14C 120.1 . . ? H15B O15 H15C 120.0 . . ? C8 N1 C1 107.3(6) . . ? C8 N1 Ni1 114.0(5) . . ? C1 N1 Ni1 138.0(5) . . ? C8 N2 C6 107.8(6) . . ? C8 N2 C7 125.7(7) . . ? C6 N2 C7 126.4(7) . . ? C9 N3 C10 114.0(6) . . ? C9 N3 Ni1 109.0(4) . . ? C10 N3 Ni1 108.4(4) . . ? C9 N3 H3A 109.1 . . ? C10 N3 H3A 106.9 . . ? Ni1 N3 H3A 109.4 . . ? C11 N4 C13 107.1(6) . . ? C11 N4 C12 128.4(7) . . ? C13 N4 C12 124.5(6) . . ? C11 N5 C18 107.0(6) . . ? C11 N5 Ni1 114.2(5) . . ? C18 N5 Ni1 138.2(5) . . ? C26 N6 C19 106.7(6) . . ? C26 N6 Ni2 113.4(5) . . ? C19 N6 Ni2 139.4(5) . . ? C26 N7 C24 106.8(6) . . ? C26 N7 C25 127.8(8) . . ? C24 N7 C25 125.4(7) . . ? C27 N8 C28 115.4(6) . . ? C27 N8 Ni2 108.4(5) . . ? C28 N8 Ni2 109.9(4) . . ? C27 N8 H8 109.5 . . ? C28 N8 H8 104.2 . . ? Ni2 N8 H8 109.3 . . ? C29 N9 C31 107.4(6) . . ? C29 N9 C30 126.2(7) . . ? C31 N9 C30 126.4(6) . . ? C29 N10 C36 106.1(6) . . ? C29 N10 Ni2 114.7(5) . . ? C36 N10 Ni2 138.7(5) . . ? C2 C1 N1 131.6(7) . . ? C2 C1 C6 121.2(7) . . ? N1 C1 C6 107.2(6) . . ? C3 C2 C1 117.5(7) . . ? C3 C2 H2 122.4 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 122.2(8) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 117.8 . . ? C5 C4 C3 121.5(8) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 118.0 . . ? C4 C5 C6 116.3(8) . . ? C4 C5 H5 124.5 . . ? C6 C5 H5 119.2 . . ? N2 C6 C1 106.4(6) . . ? N2 C6 C5 132.3(7) . . ? C1 C6 C5 121.3(7) . . ? N2 C7 H7A 110.3 . . ? N2 C7 H7B 109.0 . . ? H7A C7 H7B 109.4 . . ? N2 C7 H7C 109.0 . . ? H7A C7 H7C 109.7 . . ? H7B C7 H7C 109.5 . . ? N1 C8 N2 111.3(7) . . ? N1 C8 C9 121.8(7) . . ? N2 C8 C9 126.9(7) . . ? N3 C9 C8 109.6(6) . . ? N3 C9 H9A 109.9 . . ? C8 C9 H9A 110.3 . . ? N3 C9 H9B 109.1 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 109.6 . . ? C11 C10 N3 110.4(6) . . ? C11 C10 H10A 108.1 . . ? N3 C10 H10A 108.9 . . ? C11 C10 H10B 109.3 . . ? N3 C10 H10B 110.4 . . ? H10A C10 H10B 109.6 . . ? N5 C11 N4 111.7(6) . . ? N5 C11 C10 121.6(6) . . ? N4 C11 C10 126.6(7) . . ? N4 C12 H12A 107.3 . . ? N4 C12 H12B 110.2 . . ? H12A C12 H12B 109.6 . . ? N4 C12 H12C 110.6 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.6 . . ? N4 C13 C18 106.7(6) . . ? N4 C13 C14 132.9(7) . . ? C18 C13 C14 120.3(7) . . ? C15 C14 C13 117.6(7) . . ? C15 C14 H14A 122.0 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 122.3(7) . . ? C14 C15 H15A 118.0 . . ? C16 C15 H15A 119.7 . . ? C17 C16 C15 120.4(7) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 118.1(7) . . ? C16 C17 H17 122.2 . . ? C18 C17 H17 119.6 . . ? C17 C18 N5 131.4(6) . . ? C17 C18 C13 121.2(7) . . ? N5 C18 C13 107.3(6) . . ? N6 C19 C20 130.8(7) . . ? N6 C19 C24 109.2(7) . . ? C20 C19 C24 119.9(7) . . ? C21 C20 C19 118.4(8) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 121.5(8) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 118.1 . . ? C23 C22 C21 120.8(8) . . ? C23 C22 H22 117.6 . . ? C21 C22 H22 121.6 . . ? C22 C23 C24 116.8(8) . . ? C22 C23 H23 122.0 . . ? C24 C23 H23 121.1 . . ? N7 C24 C23 131.6(8) . . ? N7 C24 C19 105.8(7) . . ? C23 C24 C19 122.5(8) . . ? N7 C25 H25A 109.3 . . ? N7 C25 H25B 110.3 . . ? H25A C25 H25B 109.5 . . ? N7 C25 H25C 108.8 . . ? H25A C25 H25C 109.6 . . ? H25B C25 H25C 109.3 . . ? N6 C26 N7 111.4(7) . . ? N6 C26 C27 122.1(7) . . ? N7 C26 C27 126.4(7) . . ? N8 C27 C26 108.6(6) . . ? N8 C27 H27A 108.9 . . ? C26 C27 H27A 109.2 . . ? N8 C27 H27B 110.5 . . ? C26 C27 H27B 110.1 . . ? H27A C27 H27B 109.5 . . ? N8 C28 C29 109.4(6) . . ? N8 C28 H28A 109.9 . . ? C29 C28 H28A 108.6 . . ? N8 C28 H28B 110.1 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 109.4 . . ? N10 C29 N9 112.0(6) . . ? N10 C29 C28 121.6(6) . . ? N9 C29 C28 126.3(6) . . ? N9 C30 H30A 109.1 . . ? N9 C30 H30B 110.2 . . ? H30A C30 H30B 109.4 . . ? N9 C30 H30C 109.3 . . ? H30A C30 H30C 109.4 . . ? H30B C30 H30C 109.4 . . ? N9 C31 C36 105.7(6) . . ? N9 C31 C32 132.0(7) . . ? C36 C31 C32 122.3(7) . . ? C33 C32 C31 116.8(7) . . ? C33 C32 H32 122.3 . . ? C31 C32 H32 120.8 . . ? C32 C33 C34 122.4(7) . . ? C32 C33 H33 117.3 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 120.1(7) . . ? C35 C34 H34 119.1 . . ? C33 C34 H34 120.8 . . ? C34 C35 C36 118.0(7) . . ? C34 C35 H35 122.0 . . ? C36 C35 H35 120.0 . . ? N10 C36 C31 108.7(6) . . ? N10 C36 C35 131.0(6) . . ? C31 C36 C35 120.3(6) . . ? O4 C37 O3 126.4(7) . . ? O4 C37 C38 116.9(6) . . ? O3 C37 C38 116.7(7) . . ? C37 C38 H38A 108.6 . . ? C37 C38 H38B 109.2 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 110.3 . . ? H38A C38 H38C 109.6 . . ? H38B C38 H38C 109.7 . . ? O6 C39 O5 124.1(9) . . ? O6 C39 C40 121.0(9) . . ? O5 C39 C40 114.9(8) . . ? C39 C40 H40A 108.0 . . ? C39 C40 H40B 110.0 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 110.4 . . ? H40A C40 H40C 109.6 . . ? H40B C40 H40C 109.5 . . ? O2 C41 O1 120.6(9) . . ? O2 C41 C42 121.4(9) . . ? O1 C41 C42 118.0(8) . . ? C41 C42 H42A 109.7 . . ? C41 C42 H42B 108.2 . . ? H42A C42 H42B 109.4 . . ? C41 C42 H42C 110.7 . . ? H42A C42 H42C 109.4 . . ? H42B C42 H42C 109.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.072 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.188 data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 618815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H51 Cl N10 Ni2 O7' _chemical_formula_sum 'C43 H51 Cl N10 Ni2 O7' _chemical_formula_weight 972.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M 'C 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 20.0019(3) _cell_length_b 21.3390(5) _cell_length_c 15.9920(4) _cell_angle_alpha 90.00 _cell_angle_beta 128.4430(10) _cell_angle_gamma 90.00 _cell_volume 5346.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 27760 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6896 _exptl_absorpt_correction_T_max 0.7512 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21655 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.38 _reflns_number_total 5039 _reflns_number_gt 4221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & M 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0779P)^2^+6.8897P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5039 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.04612(19) 0.24406(14) 0.2276(2) 0.0362(6) Uani 1 1 d . . . C2 C -0.0445(2) 0.30893(14) 0.2219(3) 0.0435(7) Uani 1 1 d . . . H2 H -0.0290 0.3285 0.1843 0.052 Uiso 1 1 calc R . . C3 C -0.0671(3) 0.34314(17) 0.2745(3) 0.0561(9) Uani 1 1 d . . . H3 H -0.0670 0.3867 0.2720 0.067 Uiso 1 1 calc R . . C4 C -0.0902(3) 0.31330(18) 0.3315(3) 0.0618(10) Uani 1 1 d . . . H4 H -0.1046 0.3378 0.3663 0.074 Uiso 1 1 calc R . . C5 C -0.0922(2) 0.24947(18) 0.3376(3) 0.0549(9) Uani 1 1 d . . . H5 H -0.1082 0.2301 0.3748 0.066 Uiso 1 1 calc R . . C6 C -0.0691(2) 0.21486(16) 0.2854(2) 0.0407(7) Uani 1 1 d . . . C7 C -0.0735(3) 0.10175(18) 0.3314(3) 0.0603(10) Uani 1 1 d . . . H7A H -0.0933 0.1202 0.3672 0.090 Uiso 1 1 calc R . . H7B H -0.0208 0.0801 0.3825 0.090 Uiso 1 1 calc R . . H7C H -0.1154 0.0727 0.2785 0.090 Uiso 1 1 calc R . . C8 C -0.0321(2) 0.14397(14) 0.2218(2) 0.0383(7) Uani 1 1 d . . . C9 C -0.0111(2) 0.08343(15) 0.1968(3) 0.0465(8) Uani 1 1 d . . . H9A H 0.0146 0.0552 0.2571 0.056 Uiso 1 1 calc R . . H9B H -0.0629 0.0641 0.1357 0.056 Uiso 1 1 calc R . . C10 C 0.1387(2) 0.08267(14) 0.2635(3) 0.0464(8) Uani 1 1 d . . . H10A H 0.1654 0.0596 0.2389 0.056 Uiso 1 1 calc R . . H10B H 0.1427 0.0574 0.3169 0.056 Uiso 1 1 calc R . . C11 C 0.1847(2) 0.14299(13) 0.3123(2) 0.0359(6) Uani 1 1 d . . . C12 C 0.3146(2) 0.09950(17) 0.4857(3) 0.0535(9) Uani 1 1 d . . . H12A H 0.3659 0.1172 0.5483 0.080 Uiso 1 1 calc R . . H12B H 0.3289 0.0701 0.4536 0.080 Uiso 1 1 calc R . . H12C H 0.2837 0.0784 0.5052 0.080 Uiso 1 1 calc R . . C13 C 0.28038(19) 0.21292(15) 0.4242(2) 0.0356(6) Uani 1 1 d . . . C14 C 0.3488(2) 0.24680(17) 0.5091(2) 0.0444(8) Uani 1 1 d . . . H14 H 0.3944 0.2272 0.5711 0.053 Uiso 1 1 calc R . . C15 C 0.3460(2) 0.31033(17) 0.4971(3) 0.0479(8) Uani 1 1 d . . . H15 H 0.3908 0.3343 0.5529 0.057 Uiso 1 1 calc R . . C16 C 0.2787(2) 0.34077(15) 0.4046(2) 0.0430(7) Uani 1 1 d . . . H16 H 0.2799 0.3841 0.4000 0.052 Uiso 1 1 calc R . . C17 C 0.2101(2) 0.30743(13) 0.3196(3) 0.0392(7) Uani 1 1 d . . . H17 H 0.1649 0.3275 0.2580 0.047 Uiso 1 1 calc R . . C18 C 0.21163(19) 0.24249(13) 0.3303(2) 0.0338(6) Uani 1 1 d . . . C19 C -0.1540(3) 0.1665(3) -0.0657(4) 0.0854(15) Uani 1 1 d . . . C20 C -0.1914(4) 0.2230(3) -0.0757(4) 0.1027(18) Uani 1 1 d . . . H20A H -0.1518 0.2563 -0.0563 0.154 Uiso 1 1 calc R . . H20B H -0.2066 0.2236 -0.0294 0.154 Uiso 1 1 calc R . . H20C H -0.2417 0.2285 -0.1482 0.154 Uiso 1 1 calc R . . C21 C 0.0000 0.30881(17) 0.0000 0.0331(9) Uani 1 2 d S . . C22 C 0.0000 0.3799(2) 0.0000 0.0566(13) Uani 1 2 d S . . H22A H 0.0194 0.3949 0.0684 0.085 Uiso 0.50 1 calc PR . . H22B H -0.0568 0.3949 -0.0544 0.085 Uiso 0.50 1 calc PR . . H22C H 0.0374 0.3949 -0.0140 0.085 Uiso 0.50 1 calc PR . . C23 C 0.2871(6) 0.0000 0.7517(6) 0.102(2) Uani 1 2 d S . . H23A H 0.2855 0.0424 0.7704 0.153 Uiso 0.50 1 calc PR . . H23B H 0.3318 -0.0225 0.8145 0.153 Uiso 0.50 1 calc PR . . H23C H 0.2333 -0.0199 0.7209 0.153 Uiso 0.50 1 calc PR . . Cl1 Cl 0.12818(8) 0.0000 0.46290(9) 0.0501(3) Uani 1 2 d S . . N1 N -0.02348(16) 0.19758(11) 0.18856(19) 0.0360(6) Uani 1 1 d . . . N2 N -0.05981(16) 0.15120(12) 0.2795(2) 0.0406(6) Uani 1 1 d . . . N3 N 0.04851(17) 0.09399(11) 0.17327(19) 0.0409(6) Uani 1 1 d . . . H3' H 0.0336 0.0679 0.1191 0.049 Uiso 1 1 calc R . . N4 N 0.26123(16) 0.14971(12) 0.40902(19) 0.0386(6) Uani 1 1 d . . . N5 N 0.15247(16) 0.19686(10) 0.26151(19) 0.0350(6) Uani 1 1 d . . . Ni1 Ni 0.03361(2) 0.190054(16) 0.11825(3) 0.03282(15) Uani 1 1 d . . . O1 O -0.07957(15) 0.16528(11) -0.03354(16) 0.0437(5) Uani 1 1 d . . . O2 O -0.1937(3) 0.1136(3) -0.0867(5) 0.172(2) Uani 1 1 d . . . O3 O 0.02410(13) 0.28236(9) 0.08495(15) 0.0359(5) Uani 1 1 d . . . O4 O 0.3022(3) 0.0000 0.6791(4) 0.1018(16) Uani 1 2 d S . . H4' H 0.3528 0.0077 0.7098 0.153 Uiso 0.50 1 calc PR . . 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 0.0402(16) 0.0413(16) 0.0272(15) 0.0002(12) 0.0209(14) 0.0005(13) C2 0.056(2) 0.0423(18) 0.0407(18) 0.0029(13) 0.0344(17) 0.0020(14) C3 0.078(3) 0.045(2) 0.061(2) -0.0015(17) 0.051(2) 0.0061(18) C4 0.080(3) 0.065(3) 0.067(3) 0.0012(19) 0.059(2) 0.011(2) C5 0.061(2) 0.072(3) 0.050(2) 0.0042(18) 0.044(2) 0.0023(19) C6 0.0401(17) 0.0507(19) 0.0321(16) 0.0049(14) 0.0227(14) -0.0006(14) C7 0.067(2) 0.062(2) 0.066(2) 0.0190(19) 0.049(2) -0.0007(19) C8 0.0422(16) 0.0394(16) 0.0271(14) 0.0012(12) 0.0185(14) -0.0054(13) C9 0.060(2) 0.0347(16) 0.0435(18) 0.0018(14) 0.0315(17) -0.0072(15) C10 0.062(2) 0.0326(16) 0.0441(19) 0.0041(14) 0.0324(18) 0.0037(15) C11 0.0485(17) 0.0344(15) 0.0282(15) 0.0053(12) 0.0256(14) 0.0058(13) C12 0.057(2) 0.057(2) 0.0435(19) 0.0182(16) 0.0292(18) 0.0207(17) C13 0.0385(16) 0.0464(17) 0.0251(14) 0.0019(12) 0.0214(14) 0.0032(13) C14 0.0410(17) 0.063(2) 0.0291(16) -0.0032(14) 0.0218(15) -0.0007(15) C15 0.0468(19) 0.066(2) 0.0353(18) -0.0179(15) 0.0275(16) -0.0152(16) C16 0.0518(19) 0.0424(18) 0.0420(18) -0.0103(14) 0.0327(17) -0.0091(15) C17 0.0469(18) 0.0378(17) 0.0344(17) -0.0034(13) 0.0260(15) -0.0019(13) C18 0.0399(16) 0.0375(15) 0.0261(14) -0.0042(12) 0.0215(14) -0.0029(13) C19 0.073(3) 0.125(5) 0.049(2) -0.006(3) 0.033(2) -0.029(3) C20 0.107(4) 0.116(5) 0.066(3) 0.000(3) 0.044(3) -0.010(4) C21 0.041(2) 0.031(2) 0.031(2) 0.000 0.0243(19) 0.000 C22 0.089(4) 0.035(2) 0.051(3) 0.000 0.046(3) 0.000 C23 0.131(7) 0.111(6) 0.072(5) 0.000 0.066(5) 0.000 Cl1 0.0593(7) 0.0467(6) 0.0345(6) 0.000 0.0243(6) 0.000 N1 0.0470(15) 0.0328(13) 0.0269(13) 0.0009(10) 0.0223(12) -0.0019(11) N2 0.0432(14) 0.0441(15) 0.0359(14) 0.0053(11) 0.0254(12) -0.0056(12) N3 0.0607(17) 0.0292(13) 0.0304(13) -0.0024(10) 0.0272(14) -0.0026(12) N4 0.0453(15) 0.0419(14) 0.0299(13) 0.0093(11) 0.0240(13) 0.0084(11) N5 0.0461(14) 0.0313(13) 0.0266(13) 0.0000(10) 0.0221(12) 0.0006(11) Ni1 0.0459(3) 0.0285(2) 0.0230(2) -0.00058(14) 0.0209(2) -0.00116(15) O1 0.0539(14) 0.0485(13) 0.0253(10) -0.0016(9) 0.0229(11) -0.0075(11) O2 0.124(4) 0.145(4) 0.218(6) -0.011(4) 0.092(4) -0.064(3) O3 0.0492(12) 0.0312(10) 0.0272(10) -0.0009(8) 0.0237(10) 0.0000(9) O4 0.076(3) 0.116(4) 0.092(4) 0.000 0.042(3) 0.000 _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 N1 1.389(4) . ? C1 C2 1.389(4) . ? C1 C6 1.407(4) . ? C2 C3 1.384(4) . ? C2 H2 0.9300 . ? C3 C4 1.406(5) . ? C3 H3 0.9300 . ? C4 C5 1.368(5) . ? C4 H4 0.9300 . ? C5 C6 1.392(4) . ? C5 H5 0.9300 . ? C6 N2 1.382(4) . ? C7 N2 1.471(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N1 1.317(4) . ? C8 N2 1.348(4) . ? C8 C9 1.489(4) . ? C9 N3 1.473(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N3 1.469(4) . ? C10 C11 1.490(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N5 1.321(4) . ? C11 N4 1.346(4) . ? C12 N4 1.471(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N4 1.382(4) . ? C13 C14 1.389(4) . ? C13 C18 1.406(4) . ? C14 C15 1.365(5) . ? C14 H14 0.9300 . ? C15 C16 1.396(5) . ? C15 H15 0.9300 . ? C16 C17 1.385(4) . ? C16 H16 0.9300 . ? C17 C18 1.394(4) . ? C17 H17 0.9300 . ? C18 N5 1.393(4) . ? C19 O1 1.237(5) . ? C19 O2 1.297(7) . ? C19 C20 1.374(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 O3 1.258(3) 2 ? C21 O3 1.258(3) . ? C21 C22 1.517(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O4 1.369(8) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? N1 Ni1 2.047(2) . ? N3 Ni1 2.177(2) . ? N3 H3' 0.9100 . ? N5 Ni1 2.037(2) . ? Ni1 O3 2.018(2) . ? Ni1 O1 2.113(2) . ? Ni1 O1 2.123(2) 2 ? O1 Ni1 2.123(2) 2 ? O4 H4' 0.8200 . ? 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 C1 C2 130.9(3) . . ? N1 C1 C6 108.0(3) . . ? C2 C1 C6 120.9(3) . . ? C3 C2 C1 117.2(3) . . ? C3 C2 H2 121.4 . . ? C1 C2 H2 121.4 . . ? C2 C3 C4 121.2(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 122.2(3) . . ? C5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? C4 C5 C6 116.8(3) . . ? C4 C5 H5 121.6 . . ? C6 C5 H5 121.6 . . ? N2 C6 C5 132.2(3) . . ? N2 C6 C1 106.1(3) . . ? C5 C6 C1 121.7(3) . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 N2 112.9(3) . . ? N1 C8 C9 121.0(3) . . ? N2 C8 C9 126.1(3) . . ? N3 C9 C8 110.2(2) . . ? N3 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? N3 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N3 C10 C11 110.7(2) . . ? N3 C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? N5 C11 N4 112.7(3) . . ? N5 C11 C10 121.6(3) . . ? N4 C11 C10 125.8(3) . . ? N4 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C14 132.6(3) . . ? N4 C13 C18 105.7(2) . . ? C14 C13 C18 121.7(3) . . ? C15 C14 C13 116.8(3) . . ? C15 C14 H14 121.6 . . ? C13 C14 H14 121.6 . . ? C14 C15 C16 122.6(3) . . ? C14 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C17 C16 C15 121.1(3) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 117.2(3) . . ? C16 C17 H17 121.4 . . ? C18 C17 H17 121.4 . . ? N5 C18 C17 130.9(3) . . ? N5 C18 C13 108.4(3) . . ? C17 C18 C13 120.6(3) . . ? O1 C19 O2 118.3(6) . . ? O1 C19 C20 119.6(5) . . ? O2 C19 C20 122.1(6) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O3 C21 O3 126.7(4) 2 . ? O3 C21 C22 116.67(18) 2 . ? O3 C21 C22 116.67(18) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O4 C23 H23A 109.5 . . ? O4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C8 N1 C1 106.1(2) . . ? C8 N1 Ni1 114.3(2) . . ? C1 N1 Ni1 138.74(19) . . ? C8 N2 C6 106.8(2) . . ? C8 N2 C7 127.2(3) . . ? C6 N2 C7 125.9(3) . . ? C10 N3 C9 114.7(2) . . ? C10 N3 Ni1 109.13(18) . . ? C9 N3 Ni1 108.54(18) . . ? C10 N3 H3' 108.1 . . ? C9 N3 H3' 108.1 . . ? Ni1 N3 H3' 108.1 . . ? C11 N4 C13 107.4(2) . . ? C11 N4 C12 126.7(3) . . ? C13 N4 C12 125.9(3) . . ? C11 N5 C18 105.8(2) . . ? C11 N5 Ni1 114.3(2) . . ? C18 N5 Ni1 139.69(19) . . ? O3 Ni1 N5 94.57(8) . . ? O3 Ni1 N1 94.31(8) . . ? N5 Ni1 N1 92.07(10) . . ? O3 Ni1 O1 94.77(8) . . ? N5 Ni1 O1 167.87(9) . . ? N1 Ni1 O1 94.91(9) . . ? O3 Ni1 O1 94.69(8) . 2 ? N5 Ni1 O1 94.00(9) . 2 ? N1 Ni1 O1 168.70(9) . 2 ? O1 Ni1 O1 77.54(10) . 2 ? O3 Ni1 N3 172.92(8) . . ? N5 Ni1 N3 80.90(9) . . ? N1 Ni1 N3 80.50(9) . . ? O1 Ni1 N3 90.48(9) . . ? O1 Ni1 N3 91.07(9) 2 . ? C19 O1 Ni1 128.7(3) . . ? C19 O1 Ni1 128.1(3) . 2 ? Ni1 O1 Ni1 95.23(9) . 2 ? C21 O3 Ni1 129.3(2) . . ? C23 O4 H4' 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.412 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.087 data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 634028' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H48 Cl2 N10 Ni O11 S' _chemical_formula_sum 'C38 H48 Cl2 N10 Ni O11 S' _chemical_formula_weight 982.53 _chemical_absolute_configuration rm loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.973(2) _cell_length_b 19.921(4) _cell_length_c 18.832(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.64(3) _cell_angle_gamma 90.00 _cell_volume 4477.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 79344 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8524 _exptl_absorpt_correction_T_max 0.9198 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29858 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12719 _reflns_number_gt 10129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & M 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1782P)^2^+14.3542P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(3) _refine_ls_number_reflns 12719 _refine_ls_number_parameters 1126 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_gt 0.0870 _refine_ls_wR_factor_ref 0.2795 _refine_ls_wR_factor_gt 0.2457 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Ni1 Ni 0.55154(11) 0.31457(8) 0.13267(7) 0.0350(4) Uani 1 1 d . . . C1 C 0.6527(10) 0.2244(6) 0.2615(5) 0.034(3) Uani 1 1 d . . . C2 C 0.5589(10) 0.1983(7) 0.2936(6) 0.039(3) Uani 1 1 d . . . H2 H 0.4857 0.2062 0.2750 0.047 Uiso 1 1 calc R . . C3 C 0.5826(12) 0.1612(7) 0.3534(7) 0.044(3) Uani 1 1 d . . . H3 H 0.5231 0.1465 0.3782 0.052 Uiso 1 1 calc R . . C4 C 0.6928(10) 0.1435(6) 0.3804(6) 0.035(3) Uani 1 1 d . . . H4 H 0.7043 0.1135 0.4181 0.042 Uiso 1 1 calc R . . C5 C 0.7829(11) 0.1716(8) 0.3495(7) 0.048(4) Uani 1 1 d . . . H5 H 0.8555 0.1643 0.3695 0.058 Uiso 1 1 calc R . . C6 C 0.7646(9) 0.2107(7) 0.2888(6) 0.037(3) Uani 1 1 d . . . C7 C 0.9550(10) 0.2445(8) 0.2585(7) 0.048(3) Uani 1 1 d . . . H7A H 0.9758 0.2869 0.2800 0.072 Uiso 1 1 calc R . . H7B H 0.9874 0.2406 0.2137 0.072 Uiso 1 1 calc R . . H7C H 0.9820 0.2087 0.2895 0.072 Uiso 1 1 calc R . . C8 C 0.7648(9) 0.2736(6) 0.1954(6) 0.031(3) Uani 1 1 d . . . C9 C 0.8202(10) 0.3143(8) 0.1383(7) 0.047(3) Uani 1 1 d . . . H9A H 0.8471 0.2848 0.1025 0.057 Uiso 1 1 calc R . . H9B H 0.8828 0.3401 0.1597 0.057 Uiso 1 1 calc R . . C10 C 0.5596(9) 0.1982(7) 0.0090(6) 0.038(3) Uani 1 1 d . . . C11 C 0.4915(9) 0.1477(7) 0.0255(6) 0.035(3) Uani 1 1 d . . . H11 H 0.4552 0.1488 0.0673 0.042 Uiso 1 1 calc R . . C12 C 0.4765(9) 0.0940(7) -0.0212(6) 0.036(3) Uani 1 1 d . . . H12 H 0.4290 0.0587 -0.0119 0.043 Uiso 1 1 calc R . . C13 C 0.5353(10) 0.0945(7) -0.0832(7) 0.043(3) Uani 1 1 d . . . H13 H 0.5238 0.0591 -0.1151 0.052 Uiso 1 1 calc R . . C14 C 0.6041(10) 0.1414(7) -0.0980(6) 0.039(3) Uani 1 1 d . . . H14 H 0.6451 0.1375 -0.1377 0.047 Uiso 1 1 calc R . . C15 C 0.6171(10) 0.1999(9) -0.0527(6) 0.049(4) Uani 1 1 d . . . C16 C 0.7462(14) 0.2767(9) -0.1141(8) 0.062(4) Uani 1 1 d . . . H16A H 0.7062 0.3133 -0.1375 0.092 Uiso 1 1 calc R . . H16B H 0.7544 0.2411 -0.1476 0.092 Uiso 1 1 calc R . . H16C H 0.8189 0.2918 -0.0955 0.092 Uiso 1 1 calc R . . C17 C 0.6639(10) 0.2888(8) 0.0037(7) 0.043(3) Uani 1 1 d . . . C18 C 0.7168(13) 0.3538(9) 0.0251(6) 0.061(4) Uani 1 1 d . . . H18A H 0.6719 0.3903 0.0041 0.073 Uiso 1 1 calc R . . H18B H 0.7905 0.3563 0.0073 0.073 Uiso 1 1 calc R . . C19 C 0.8690(10) 0.4646(7) 0.0871(6) 0.040(3) Uani 1 1 d . . . H19A H 0.9200 0.4267 0.0905 0.048 Uiso 1 1 calc R . . H19B H 0.8462 0.4712 0.0370 0.048 Uiso 1 1 calc R . . C20 C 0.9345(10) 0.5270(7) 0.1141(6) 0.044(3) Uani 1 1 d . . . C21 C 0.9958(12) 0.5267(8) 0.1891(7) 0.050(4) Uani 1 1 d . . . C22 C 1.0367(12) 0.5915(8) 0.2079(7) 0.052(4) Uani 1 1 d . . . H22A H 1.1176 0.5912 0.2168 0.062 Uiso 1 1 calc R . . H22B H 1.0041 0.6078 0.2502 0.062 Uiso 1 1 calc R . . C23 C 0.9982(12) 0.6382(13) 0.1391(9) 0.087(7) Uani 1 1 d . . . H23 H 0.9932 0.6867 0.1468 0.105 Uiso 1 1 calc R . . C24 C 1.0732(10) 0.6136(8) 0.0808(7) 0.054(4) Uani 1 1 d . . . H24A H 1.1517 0.6159 0.0979 0.065 Uiso 1 1 calc R . . H24B H 1.0614 0.6411 0.0384 0.065 Uiso 1 1 calc R . . C25 C 1.0360(10) 0.5344(8) 0.0629(8) 0.057(4) Uani 1 1 d . . . H25A H 1.0105 0.5283 0.0131 0.068 Uiso 1 1 calc R . . H25B H 1.0965 0.5032 0.0759 0.068 Uiso 1 1 calc R . . C26 C 0.8845(10) 0.5990(7) 0.1151(6) 0.043(3) Uani 1 1 d . . . C27 C 0.7971(12) 0.6054(8) 0.1699(7) 0.054(4) Uani 1 1 d . . . H27A H 0.8130 0.6445 0.1987 0.081 Uiso 1 1 calc R . . H27B H 0.7999 0.5663 0.1997 0.081 Uiso 1 1 calc R . . H27C H 0.7238 0.6094 0.1456 0.081 Uiso 1 1 calc R . . C28 C 0.8347(11) 0.6240(8) 0.0413(7) 0.053(4) Uani 1 1 d . . . H28A H 0.7753 0.5945 0.0237 0.080 Uiso 1 1 calc R . . H28B H 0.8922 0.6244 0.0087 0.080 Uiso 1 1 calc R . . H28C H 0.8056 0.6686 0.0459 0.080 Uiso 1 1 calc R . . C29 C 0.3956(13) 0.4150(8) 0.0348(8) 0.055(4) Uani 1 1 d . . . C30 C 0.3043(16) 0.4527(9) -0.0141(10) 0.082(5) Uani 1 1 d . . . H30A H 0.3275 0.4552 -0.0617 0.123 Uiso 1 1 calc R . . H30B H 0.2948 0.4972 0.0039 0.123 Uiso 1 1 calc R . . H30C H 0.2346 0.4288 -0.0146 0.123 Uiso 1 1 calc R . . C31 C 0.3285(10) 0.2301(7) 0.1483(6) 0.039(3) Uani 1 1 d . . . C32 C 0.2322(12) 0.1856(9) 0.1556(7) 0.064(5) Uani 1 1 d . . . H32A H 0.2383 0.1468 0.1260 0.096 Uiso 1 1 calc R . . H32B H 0.1641 0.2091 0.1413 0.096 Uiso 1 1 calc R . . H32C H 0.2312 0.1717 0.2044 0.096 Uiso 1 1 calc R . . C33 C 0.5291(10) 0.3947(6) 0.2761(6) 0.035(3) Uani 1 1 d . . . C34 C 0.5292(14) 0.4116(12) 0.3485(7) 0.088(7) Uani 1 1 d . . . H34A H 0.4691 0.4424 0.3549 0.132 Uiso 1 1 calc R . . H34B H 0.5993 0.4323 0.3641 0.132 Uiso 1 1 calc R . . H34C H 0.5193 0.3718 0.3759 0.132 Uiso 1 1 calc R . . N1 N 0.6611(7) 0.2655(5) 0.1997(5) 0.033(2) Uani 1 1 d . . . N2 N 0.8328(7) 0.2405(5) 0.2468(5) 0.035(2) Uani 1 1 d . . . N3 N 0.7278(8) 0.3615(6) 0.1047(5) 0.039(2) Uani 1 1 d . . . N4 N 0.6817(9) 0.2514(6) -0.0538(5) 0.043(3) Uani 1 1 d . . . N5 N 0.5908(8) 0.2601(6) 0.0451(5) 0.040(3) Uani 1 1 d . . . N6 N 0.4572(9) 0.3819(6) 0.0709(5) 0.045(3) Uani 1 1 d . . . N7 N 0.4069(9) 0.2597(7) 0.1457(5) 0.047(3) Uani 1 1 d . . . N8 N 0.5243(8) 0.3762(6) 0.2173(6) 0.043(3) Uani 1 1 d . . . S1 S 0.7463(3) 0.44178(16) 0.13115(16) 0.0376(7) Uani 1 1 d . . . O1 O 0.7690(7) 0.4404(4) 0.2060(4) 0.040(2) Uani 1 1 d . . . O2 O 0.6503(8) 0.4793(5) 0.1001(5) 0.056(3) Uani 1 1 d . . . O3 O 1.0167(8) 0.4693(5) 0.2189(5) 0.058(3) Uani 1 1 d . . . Ni2 Ni 0.04746(11) 0.45891(7) 0.63222(7) 0.0268(3) Uani 1 1 d . . . C35 C 0.0687(8) 0.5686(5) 0.5092(5) 0.023(2) Uani 1 1 d . . . C36 C -0.0030(9) 0.6186(6) 0.5220(6) 0.033(3) Uani 1 1 d . . . H36 H -0.0459 0.6170 0.5610 0.040 Uiso 1 1 calc R . . C37 C -0.0106(9) 0.6727(6) 0.4749(6) 0.034(3) Uani 1 1 d . . . H37 H -0.0565 0.7085 0.4852 0.041 Uiso 1 1 calc R . . C38 C 0.0450(9) 0.6765(7) 0.4145(6) 0.036(3) Uani 1 1 d . . . H38 H 0.0358 0.7139 0.3851 0.043 Uiso 1 1 calc R . . C39 C 0.1182(9) 0.6226(6) 0.3961(6) 0.031(3) Uani 1 1 d . . . H39 H 0.1571 0.6224 0.3554 0.038 Uiso 1 1 calc R . . C40 C 0.1239(8) 0.5713(5) 0.4457(5) 0.022(2) Uani 1 1 d . . . C41 C 0.2547(10) 0.4902(7) 0.3887(6) 0.040(3) Uani 1 1 d . . . H41A H 0.3159 0.5211 0.3866 0.061 Uiso 1 1 calc R . . H41B H 0.2094 0.4909 0.3443 0.061 Uiso 1 1 calc R . . H41C H 0.2835 0.4457 0.3975 0.061 Uiso 1 1 calc R . . C42 C 0.1642(9) 0.4764(6) 0.5051(5) 0.029(3) Uani 1 1 d . . . C43 C 0.2134(9) 0.4099(6) 0.5266(5) 0.027(2) Uani 1 1 d . . . H43A H 0.2882 0.4057 0.5107 0.032 Uiso 1 1 calc R . . H43B H 0.1674 0.3739 0.5053 0.032 Uiso 1 1 calc R . . C44 C 0.1540(10) 0.5445(7) 0.7645(6) 0.037(3) Uani 1 1 d . . . C45 C 0.0648(11) 0.5669(7) 0.7983(6) 0.039(3) Uani 1 1 d . . . H45 H -0.0085 0.5570 0.7814 0.047 Uiso 1 1 calc R . . C46 C 0.0898(13) 0.6064(7) 0.8609(6) 0.048(4) Uani 1 1 d . . . H46 H 0.0329 0.6277 0.8830 0.057 Uiso 1 1 calc R . . C47 C 0.2026(13) 0.6123(7) 0.8884(6) 0.050(4) Uani 1 1 d . . . H47 H 0.2169 0.6340 0.9319 0.060 Uiso 1 1 calc R . . C48 C 0.2875(12) 0.5896(8) 0.8574(6) 0.048(4) Uani 1 1 d . . . H48 H 0.3609 0.5970 0.8757 0.057 Uiso 1 1 calc R . . C49 C 0.2626(11) 0.5543(6) 0.7964(6) 0.037(3) Uani 1 1 d . . . C50 C 0.4568(10) 0.5129(7) 0.7663(6) 0.039(3) Uani 1 1 d . . . H50A H 0.4745 0.4877 0.8092 0.058 Uiso 1 1 calc R . . H50B H 0.4881 0.5572 0.7717 0.058 Uiso 1 1 calc R . . H50C H 0.4878 0.4907 0.7271 0.058 Uiso 1 1 calc R . . C51 C 0.2708(9) 0.4918(6) 0.6986(5) 0.029(3) Uani 1 1 d . . . C52 C 0.3089(8) 0.4521(6) 0.6402(6) 0.026(2) Uani 1 1 d . . . H52A H 0.3731 0.4254 0.6577 0.031 Uiso 1 1 calc R . . H52B H 0.3329 0.4821 0.6038 0.031 Uiso 1 1 calc R . . C53 C 0.3429(9) 0.2868(6) 0.5967(6) 0.031(2) Uani 1 1 d . . . H53A H 0.3191 0.2788 0.5470 0.037 Uiso 1 1 calc R . . H53B H 0.4052 0.3180 0.5983 0.037 Uiso 1 1 calc R . . C54 C 0.3819(8) 0.2238(6) 0.6289(6) 0.033(3) Uani 1 1 d . . . C55 C 0.4719(11) 0.2335(11) 0.6931(6) 0.069(6) Uani 1 1 d . . . C56 C 0.5258(11) 0.1584(7) 0.7011(6) 0.047(3) Uani 1 1 d . . . H56A H 0.6064 0.1591 0.6987 0.056 Uiso 1 1 calc R . . H56B H 0.5081 0.1370 0.7451 0.056 Uiso 1 1 calc R . . C57 C 0.4698(12) 0.1258(7) 0.6397(7) 0.052(4) Uani 1 1 d . . . H57 H 0.5142 0.0878 0.6245 0.063 Uiso 1 1 calc R . . C58 C 0.3509(10) 0.1028(7) 0.6544(7) 0.045(3) Uani 1 1 d . . . H58A H 0.3182 0.0737 0.6170 0.054 Uiso 1 1 calc R . . H58B H 0.3501 0.0802 0.7000 0.054 Uiso 1 1 calc R . . C59 C 0.2927(10) 0.1698(7) 0.6545(7) 0.042(3) Uani 1 1 d . . . H59A H 0.2720 0.1806 0.7019 0.050 Uiso 1 1 calc R . . H59B H 0.2256 0.1694 0.6220 0.050 Uiso 1 1 calc R . . C60 C 0.4515(9) 0.1786(6) 0.5787(5) 0.034(3) Uani 1 1 d . . . C61 C 0.5547(10) 0.2118(7) 0.5583(6) 0.037(3) Uani 1 1 d . . . H61A H 0.6045 0.1787 0.5414 0.055 Uiso 1 1 calc R . . H61B H 0.5908 0.2343 0.5990 0.055 Uiso 1 1 calc R . . H61C H 0.5358 0.2439 0.5212 0.055 Uiso 1 1 calc R . . C62 C 0.3807(10) 0.1546(6) 0.5130(6) 0.038(3) Uani 1 1 d . . . H62A H 0.3802 0.1883 0.4765 0.057 Uiso 1 1 calc R . . H62B H 0.3055 0.1465 0.5250 0.057 Uiso 1 1 calc R . . H62C H 0.4118 0.1138 0.4960 0.057 Uiso 1 1 calc R . . C65 C -0.1662(11) 0.5486(7) 0.6547(6) 0.036(3) Uani 1 1 d . . . C66 C -0.2663(12) 0.5881(10) 0.6605(9) 0.069(5) Uani 1 1 d . . . H66A H -0.3120 0.5864 0.6163 0.104 Uiso 1 1 calc R . . H66B H -0.2459 0.6338 0.6713 0.104 Uiso 1 1 calc R . . H66C H -0.3075 0.5703 0.6979 0.104 Uiso 1 1 calc R . . C67 C -0.1237(10) 0.3590(7) 0.5417(6) 0.041(3) Uani 1 1 d . . . C68 C -0.2060(13) 0.3143(9) 0.5129(8) 0.069(3) Uani 1 1 d . . . H68A H -0.2106 0.2765 0.5441 0.104 Uiso 1 1 calc R . . H68B H -0.1865 0.2992 0.4671 0.104 Uiso 1 1 calc R . . H68C H -0.2771 0.3368 0.5077 0.104 Uiso 1 1 calc R . . N9 N 0.0955(7) 0.5089(5) 0.5436(4) 0.029(2) Uani 1 1 d . . . N10 N 0.1868(8) 0.5096(5) 0.4460(4) 0.027(2) Uani 1 1 d . . . N11 N 0.2178(7) 0.4059(4) 0.6073(5) 0.025(2) Uani 1 1 d . . . N12 N 0.1613(8) 0.5047(5) 0.7033(4) 0.029(2) Uani 1 1 d . . . N13 N 0.3358(8) 0.5178(5) 0.7525(5) 0.030(2) Uani 1 1 d . . . N15 N -0.0901(8) 0.5172(5) 0.6484(5) 0.032(2) Uani 1 1 d . . . N16 N -0.0523(7) 0.3959(5) 0.5662(5) 0.031(2) Uani 1 1 d . . . S2 S 0.2276(2) 0.32620(15) 0.63886(14) 0.0300(6) Uani 1 1 d . . . O4 O 0.1272(6) 0.2938(4) 0.6124(4) 0.0341(18) Uani 1 1 d . . . O5 O 0.2514(6) 0.3334(4) 0.7139(4) 0.0364(19) Uani 1 1 d . . . O6 O 0.4965(7) 0.2771(5) 0.7283(4) 0.043(2) Uani 1 1 d . . . Cl1 Cl 0.2186(3) 0.29066(16) 0.37060(15) 0.0413(7) Uani 1 1 d . . . O7 O 0.2348(11) 0.2608(7) 0.3041(5) 0.079(4) Uani 1 1 d . . . O8 O 0.3206(8) 0.3134(6) 0.4072(5) 0.064(3) Uani 1 1 d . . . O9 O 0.1410(8) 0.3457(5) 0.3642(5) 0.066(3) Uani 1 1 d . . . O10 O 0.1739(9) 0.2392(6) 0.4134(6) 0.078(4) Uani 1 1 d . . . Cl2 Cl 0.5534(2) 0.46178(17) 0.53253(15) 0.0395(7) Uani 1 1 d . . . O11 O 0.5670(8) 0.4856(6) 0.6052(4) 0.069(3) Uani 1 1 d . . . O12 O 0.6523(8) 0.4713(5) 0.5007(5) 0.058(3) Uani 1 1 d . . . O13 O 0.4606(8) 0.4992(6) 0.4974(6) 0.069(3) Uani 1 1 d . . . O14 O 0.5252(8) 0.3934(5) 0.5340(5) 0.054(2) Uani 1 1 d . . . Cl3 Cl 0.0626(3) 0.3096(2) 0.02701(19) 0.0594(10) Uani 1 1 d . . . O15 O 0.0733(19) 0.3298(18) 0.1030(12) 0.038(12) Uiso 0.35(6) 1 d P A 1 O15A O 0.062(3) 0.291(3) 0.1006(17) 0.136(12) Uiso 0.65(6) 1 d P A 2 O16 O 0.0377(17) 0.3750(8) 0.0072(9) 0.134(7) Uani 1 1 d . A . O17 O -0.007(2) 0.2573(16) 0.037(2) 0.110(12) Uiso 0.56(5) 1 d P A 3 O17A O -0.0176(15) 0.2741(11) -0.0069(13) 0.041(9) Uiso 0.44(5) 1 d P A 4 O18 O 0.194(5) 0.296(2) 0.023(4) 0.083(15) Uiso 0.39(10) 1 d P A 5 O18A O 0.164(2) 0.2896(10) -0.0018(17) 0.051(9) Uiso 0.61(10) 1 d P A 6 Cl4 Cl 0.7590(3) 0.4967(2) 0.86903(17) 0.0578(10) Uani 1 1 d . . . O19 O 0.7339(16) 0.4982(13) 0.8032(6) 0.163(9) Uani 1 1 d . B . O20A O 0.833(3) 0.475(2) 0.917(2) 0.120(16) Uiso 0.46(4) 1 d P B 7 O20 O 0.802(2) 0.4252(16) 0.8623(15) 0.110(13) Uiso 0.54(4) 1 d P B 8 O21A O 0.6899(16) 0.5025(12) 0.9197(11) 0.061(5) Uiso 0.50 1 d P B 9 O21 O 0.677(2) 0.5303(15) 0.8815(14) 0.085(7) Uiso 0.50 1 d P B 10 O22 O 0.8623(16) 0.5352(11) 0.8881(10) 0.148(6) Uiso 1 1 d . B . C69 C 0.8582(14) 0.4095(9) 0.3628(9) 0.070(4) Uiso 1 1 d . . . C70 C 0.9152(16) 0.4707(10) 0.3738(10) 0.082(5) Uiso 1 1 d . . . H70A H 0.8773 0.4978 0.4064 0.123 Uiso 1 1 calc R . . H70B H 0.9167 0.4939 0.3292 0.123 Uiso 1 1 calc R . . H70C H 0.9905 0.4622 0.3931 0.123 Uiso 1 1 calc R . . N17 N 0.8050(15) 0.3590(9) 0.3551(10) 0.100(5) Uani 1 1 d . . . C71 C 0.7092(13) 0.9667(8) 0.7938(7) 0.053(4) Uani 1 1 d . . . C72 C 0.7542(13) 0.9019(9) 0.8014(9) 0.065(5) Uani 1 1 d . . . H72A H 0.8118 0.8962 0.7693 0.097 Uiso 1 1 calc R . . H72B H 0.6961 0.8694 0.7907 0.097 Uiso 1 1 calc R . . H72C H 0.7856 0.8957 0.8495 0.097 Uiso 1 1 calc R . . N18 N 0.6796(11) 1.0249(7) 0.7846(7) 0.067(4) Uani 1 1 d . . . C73 C 0.4285(12) 0.3258(9) 0.8796(6) 0.054(4) Uani 1 1 d . . . C74 C 0.3557(10) 0.2705(7) 0.8734(7) 0.049(3) Uani 1 1 d . . . H74A H 0.3095 0.2701 0.9128 0.074 Uiso 1 1 calc R . . H74B H 0.3987 0.2298 0.8735 0.074 Uiso 1 1 calc R . . H74C H 0.3090 0.2737 0.8296 0.074 Uiso 1 1 calc R . . N19 N 0.4887(12) 0.3723(8) 0.8846(7) 0.071(3) Uani 1 1 d . . . C75 C 0.7633(11) 0.2997(10) 0.7072(7) 0.049(4) Uani 1 1 d . . . C76 C 0.7091(14) 0.3643(10) 0.6948(11) 0.082(6) Uani 1 1 d . . . H76A H 0.7641 0.3993 0.7005 0.124 Uiso 1 1 calc R . . H76B H 0.6539 0.3706 0.7284 0.124 Uiso 1 1 calc R . . H76C H 0.6736 0.3656 0.6473 0.124 Uiso 1 1 calc R . . N20 N 0.8056(14) 0.2583(8) 0.7136(8) 0.071(3) Uani 1 1 d . . . N14 N 0.0108(8) 0.3983(6) 0.7150(5) 0.037(3) Uani 1 1 d . . . C63 C 0.0131(11) 0.3767(9) 0.7663(9) 0.056(4) Uani 1 1 d . . . C64 C 0.0111(14) 0.3393(9) 0.8341(8) 0.069(3) Uani 1 1 d . . . H64A H 0.0182 0.3703 0.8733 0.104 Uiso 1 1 calc R . . H64B H 0.0723 0.3081 0.8384 0.104 Uiso 1 1 calc R . . H64C H -0.0584 0.3154 0.8347 0.104 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0332(8) 0.0472(11) 0.0240(7) 0.0040(7) -0.0017(6) 0.0003(7) C1 0.057(8) 0.027(7) 0.016(5) 0.011(5) -0.006(5) 0.004(6) C2 0.035(6) 0.055(9) 0.029(6) -0.012(6) 0.007(5) -0.007(6) C3 0.062(8) 0.038(8) 0.032(7) -0.002(6) 0.011(6) -0.003(6) C4 0.050(7) 0.034(7) 0.021(5) -0.005(5) 0.004(5) -0.007(6) C5 0.050(8) 0.052(9) 0.040(7) -0.017(6) -0.009(6) 0.025(7) C6 0.027(6) 0.058(9) 0.025(6) -0.004(6) -0.009(5) 0.004(6) C7 0.030(6) 0.058(9) 0.056(8) -0.003(7) -0.002(5) 0.012(6) C8 0.040(7) 0.024(6) 0.028(6) 0.002(5) 0.003(5) 0.007(5) C9 0.040(7) 0.061(10) 0.042(7) -0.013(7) 0.009(5) -0.002(6) C10 0.033(6) 0.061(9) 0.020(6) 0.003(6) -0.006(4) 0.009(6) C11 0.032(6) 0.043(8) 0.029(6) 0.004(6) -0.005(5) -0.017(6) C12 0.034(6) 0.039(8) 0.035(6) -0.002(6) -0.004(5) -0.001(5) C13 0.031(6) 0.048(9) 0.049(8) -0.011(7) -0.008(5) -0.001(6) C14 0.039(7) 0.060(9) 0.017(5) -0.018(6) -0.007(4) 0.006(6) C15 0.023(6) 0.096(13) 0.027(6) 0.014(7) 0.002(5) 0.014(7) C16 0.084(11) 0.062(10) 0.042(8) 0.013(8) 0.028(7) -0.010(9) C17 0.042(7) 0.051(9) 0.037(7) 0.010(6) 0.002(5) -0.005(6) C18 0.070(9) 0.092(13) 0.023(6) 0.003(7) 0.016(6) -0.017(9) C19 0.060(8) 0.032(7) 0.027(5) 0.000(5) 0.003(5) 0.003(6) C20 0.047(7) 0.048(8) 0.038(6) 0.002(6) 0.001(5) -0.004(6) C21 0.054(8) 0.053(9) 0.045(7) 0.018(7) 0.002(6) 0.011(7) C22 0.052(8) 0.066(10) 0.036(7) -0.016(7) -0.009(6) -0.003(7) C23 0.036(8) 0.16(2) 0.067(10) -0.011(12) 0.010(7) -0.032(10) C24 0.033(7) 0.074(10) 0.056(8) 0.006(7) 0.005(6) -0.005(7) C25 0.024(6) 0.075(11) 0.074(9) 0.013(8) 0.016(6) -0.003(6) C26 0.042(7) 0.054(9) 0.033(6) -0.004(6) -0.005(5) -0.004(6) C27 0.056(8) 0.059(10) 0.046(8) -0.014(7) 0.001(6) 0.005(7) C28 0.049(8) 0.062(10) 0.051(8) 0.008(7) 0.014(6) 0.014(7) C29 0.061(9) 0.050(9) 0.057(9) 0.000(8) 0.017(7) 0.005(7) C30 0.106(14) 0.055(11) 0.085(12) 0.026(10) 0.008(10) 0.023(10) C31 0.025(6) 0.058(9) 0.033(7) -0.001(6) -0.002(5) -0.011(6) C32 0.050(8) 0.099(14) 0.044(8) -0.006(8) 0.002(6) -0.053(9) C33 0.052(7) 0.030(7) 0.025(6) 0.003(5) 0.005(5) 0.001(6) C34 0.066(10) 0.16(2) 0.037(8) -0.012(10) 0.007(7) 0.028(11) N1 0.017(5) 0.047(7) 0.035(5) 0.011(5) 0.002(4) 0.005(4) N2 0.025(5) 0.047(6) 0.031(5) -0.006(5) -0.007(4) 0.010(4) N3 0.041(6) 0.044(7) 0.032(5) 0.013(5) 0.005(4) -0.003(5) N4 0.038(6) 0.069(8) 0.023(5) 0.000(5) 0.004(4) 0.008(6) N5 0.039(6) 0.049(7) 0.034(6) 0.013(5) 0.003(4) 0.006(5) N6 0.060(7) 0.046(7) 0.027(5) 0.016(5) -0.006(5) 0.005(6) N7 0.037(6) 0.080(9) 0.023(5) -0.011(5) -0.002(4) 0.003(6) N8 0.036(5) 0.050(7) 0.043(6) 0.012(6) 0.003(4) 0.004(5) S1 0.0434(17) 0.0365(19) 0.0325(15) 0.0010(13) 0.0015(12) -0.0004(13) O1 0.040(5) 0.045(6) 0.036(4) 0.003(4) 0.010(3) -0.007(4) O2 0.061(6) 0.051(7) 0.055(6) 0.003(5) 0.002(4) 0.007(5) O3 0.057(5) 0.058(7) 0.061(6) 0.002(5) 0.017(4) 0.008(5) Ni2 0.0338(8) 0.0231(8) 0.0232(7) -0.0021(6) 0.0001(5) 0.0013(6) C35 0.027(5) 0.014(5) 0.027(5) 0.009(4) -0.010(4) -0.002(4) C36 0.031(6) 0.041(8) 0.028(6) -0.005(5) 0.004(5) -0.010(5) C37 0.033(6) 0.027(7) 0.041(7) 0.004(5) -0.009(5) 0.002(5) C38 0.038(7) 0.037(7) 0.032(6) 0.001(6) -0.004(5) 0.006(6) C39 0.034(6) 0.028(6) 0.032(6) -0.005(5) 0.002(5) -0.004(5) C40 0.029(5) 0.005(5) 0.030(6) -0.001(4) -0.007(4) 0.005(4) C41 0.046(7) 0.043(8) 0.034(6) 0.000(6) 0.009(5) 0.000(6) C42 0.039(6) 0.024(7) 0.022(5) -0.003(5) -0.005(4) 0.000(5) C43 0.039(6) 0.019(6) 0.023(5) -0.007(4) 0.008(4) -0.002(5) C44 0.043(7) 0.039(8) 0.029(6) -0.003(6) -0.003(5) -0.006(6) C45 0.043(7) 0.034(7) 0.039(7) -0.013(6) -0.004(5) -0.007(6) C46 0.086(10) 0.040(8) 0.017(6) -0.006(6) 0.005(6) 0.000(7) C47 0.088(11) 0.037(8) 0.022(6) -0.001(6) -0.011(6) -0.021(7) C48 0.060(8) 0.065(10) 0.017(6) -0.018(6) 0.001(5) -0.022(7) C49 0.054(7) 0.037(7) 0.019(5) 0.000(5) -0.003(5) -0.011(6) C50 0.053(7) 0.037(7) 0.024(5) 0.008(5) -0.007(5) 0.000(6) C51 0.030(6) 0.039(7) 0.017(5) 0.004(5) -0.001(4) 0.002(5) C52 0.021(5) 0.019(6) 0.037(6) -0.020(5) 0.005(4) -0.011(4) C53 0.041(6) 0.024(6) 0.029(5) -0.001(5) 0.011(4) 0.004(5) C54 0.021(5) 0.048(8) 0.031(6) -0.003(5) 0.002(4) -0.002(5) C55 0.037(7) 0.151(18) 0.017(6) 0.003(8) -0.002(5) 0.050(9) C56 0.055(8) 0.061(9) 0.021(5) -0.010(6) -0.014(5) 0.023(7) C57 0.065(9) 0.042(8) 0.049(8) 0.009(6) 0.000(6) 0.044(7) C58 0.047(7) 0.049(8) 0.040(6) 0.013(6) 0.009(5) 0.000(6) C59 0.032(6) 0.049(8) 0.045(7) -0.008(6) 0.006(5) 0.002(6) C60 0.044(6) 0.036(7) 0.024(5) 0.005(5) 0.005(4) 0.016(5) C61 0.050(7) 0.042(8) 0.019(5) 0.008(5) 0.008(5) 0.004(6) C62 0.045(7) 0.033(7) 0.036(6) 0.005(5) 0.003(5) 0.000(5) C65 0.043(7) 0.035(7) 0.031(6) -0.006(5) 0.007(5) -0.012(6) C66 0.047(9) 0.094(14) 0.069(10) -0.003(10) 0.019(7) -0.005(9) C67 0.032(6) 0.051(8) 0.039(7) -0.002(6) -0.005(5) 0.018(6) C68 0.078(7) 0.071(8) 0.056(6) 0.024(6) -0.012(5) -0.005(6) N9 0.033(5) 0.034(6) 0.020(4) 0.000(4) -0.003(4) 0.002(4) N10 0.047(5) 0.016(5) 0.020(4) 0.000(4) 0.005(4) 0.007(4) N11 0.020(4) 0.018(5) 0.036(5) -0.008(4) -0.002(4) 0.003(4) N12 0.044(5) 0.025(5) 0.016(4) 0.000(4) -0.003(4) 0.001(4) N13 0.043(5) 0.016(5) 0.030(5) -0.001(4) 0.004(4) 0.006(4) N15 0.044(6) 0.019(5) 0.033(5) -0.008(4) 0.000(4) 0.003(5) N16 0.031(5) 0.025(5) 0.034(5) 0.006(4) -0.009(4) -0.005(4) S2 0.0363(14) 0.0227(15) 0.0308(14) -0.0011(12) 0.0014(11) 0.0030(12) O4 0.041(4) 0.021(4) 0.039(4) 0.006(3) 0.002(3) 0.006(3) O5 0.045(4) 0.037(5) 0.027(4) 0.003(4) 0.001(3) 0.002(4) O6 0.059(5) 0.039(5) 0.028(4) -0.018(4) -0.005(4) -0.008(4) Cl1 0.0549(17) 0.0385(18) 0.0283(13) 0.0012(12) -0.0090(12) -0.0062(14) O7 0.117(10) 0.088(9) 0.032(5) -0.006(6) 0.013(5) 0.009(7) O8 0.065(6) 0.065(7) 0.060(6) -0.030(6) -0.020(4) -0.001(5) O9 0.075(6) 0.036(5) 0.080(7) -0.020(5) -0.036(5) 0.006(5) O10 0.069(7) 0.076(8) 0.093(8) 0.065(7) 0.040(6) 0.024(6) Cl2 0.0474(16) 0.0339(16) 0.0366(14) -0.0001(14) 0.0002(12) -0.0098(14) O11 0.060(6) 0.116(10) 0.029(4) -0.015(5) -0.006(4) -0.009(6) O12 0.065(6) 0.034(5) 0.079(7) -0.012(5) 0.028(5) -0.021(5) O13 0.045(5) 0.075(8) 0.086(7) 0.043(6) 0.002(5) 0.010(5) O14 0.077(6) 0.026(5) 0.060(6) 0.009(4) 0.020(5) -0.007(4) Cl3 0.063(2) 0.064(3) 0.051(2) -0.001(2) -0.0001(16) 0.012(2) O16 0.203(18) 0.094(12) 0.113(12) -0.004(10) 0.057(12) 0.060(12) Cl4 0.060(2) 0.077(3) 0.0370(17) -0.0007(17) 0.0075(14) 0.0072(19) O19 0.175(16) 0.28(3) 0.026(6) -0.003(10) -0.020(7) 0.046(17) N17 0.110(12) 0.069(11) 0.117(13) -0.009(10) -0.008(10) -0.013(9) C71 0.075(9) 0.051(10) 0.036(7) -0.008(7) 0.031(6) -0.033(8) C72 0.058(9) 0.067(12) 0.069(10) 0.016(9) 0.004(7) -0.037(8) N18 0.093(10) 0.036(7) 0.077(9) 0.018(6) 0.038(7) 0.014(7) C73 0.065(9) 0.067(11) 0.029(6) 0.013(7) -0.003(6) 0.032(9) C74 0.036(7) 0.062(9) 0.048(7) 0.018(7) -0.001(5) 0.005(6) N19 0.080(7) 0.062(7) 0.070(6) -0.021(5) 0.000(5) -0.008(6) C75 0.036(7) 0.079(12) 0.031(6) -0.009(7) 0.006(5) -0.014(7) C76 0.057(10) 0.079(14) 0.105(14) 0.015(11) -0.028(9) -0.020(9) N20 0.080(7) 0.062(7) 0.070(6) -0.021(5) 0.000(5) -0.008(6) N14 0.051(6) 0.042(7) 0.020(5) 0.021(5) 0.006(4) -0.001(5) C63 0.031(7) 0.065(11) 0.072(11) 0.001(9) 0.015(7) 0.004(7) C64 0.078(7) 0.071(8) 0.056(6) 0.024(6) -0.012(5) -0.005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.999(9) . ? Ni1 N6 2.052(11) . ? Ni1 N8 2.058(12) . ? Ni1 N5 2.059(11) . ? Ni1 N7 2.080(12) . ? Ni1 N3 2.405(10) . ? C1 C2 1.417(17) . ? C1 C6 1.422(16) . ? C1 N1 1.434(14) . ? C2 C3 1.358(18) . ? C2 H2 0.9300 . ? C3 C4 1.420(18) . ? C3 H3 0.9300 . ? C4 C5 1.384(19) . ? C4 H4 0.9300 . ? C5 C6 1.386(19) . ? C5 H5 0.9300 . ? C6 N2 1.323(16) . ? C7 N2 1.464(15) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N1 1.261(14) . ? C8 N2 1.382(14) . ? C8 C9 1.540(17) . ? C9 N3 1.547(17) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.347(18) . ? C10 C15 1.398(16) . ? C10 N5 1.442(18) . ? C11 C12 1.386(17) . ? C11 H11 0.9300 . ? C12 C13 1.412(17) . ? C12 H12 0.9300 . ? C13 C14 1.290(19) . ? C13 H13 0.9300 . ? C14 C15 1.45(2) . ? C14 H14 0.9300 . ? C15 N4 1.287(19) . ? C16 N4 1.510(16) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N4 1.345(17) . ? C17 N5 1.347(16) . ? C17 C18 1.48(2) . ? C18 N3 1.501(15) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.534(18) . ? C19 S1 1.802(12) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.540(18) . ? C20 C26 1.555(19) . ? C20 C25 1.618(17) . ? C21 O3 1.289(17) . ? C21 C22 1.42(2) . ? C22 C23 1.63(2) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.55(2) . ? C23 C26 1.60(2) . ? C23 H23 0.9800 . ? C24 C25 1.67(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.533(18) . ? C26 C28 1.548(17) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N6 1.167(18) . ? C29 C30 1.56(2) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N7 1.112(16) . ? C31 C32 1.471(18) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 N8 1.165(15) . ? C33 C34 1.404(18) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? N3 S1 1.684(12) . ? S1 O1 1.414(8) . ? S1 O2 1.454(10) . ? Ni2 N12 2.045(9) . ? Ni2 N14 2.047(9) . ? Ni2 N15 2.058(10) . ? Ni2 N9 2.064(9) . ? Ni2 N16 2.075(10) . ? Ni2 N11 2.377(8) . ? C35 C36 1.348(16) . ? C35 N9 1.380(14) . ? C35 C40 1.413(15) . ? C36 C37 1.396(17) . ? C36 H36 0.9300 . ? C37 C38 1.365(16) . ? C37 H37 0.9300 . ? C38 C39 1.446(17) . ? C38 H38 0.9300 . ? C39 C40 1.382(16) . ? C39 H39 0.9300 . ? C40 N10 1.441(13) . ? C41 N10 1.454(14) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 N9 1.312(14) . ? C42 N10 1.340(14) . ? C42 C43 1.494(16) . ? C43 N11 1.520(13) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.361(17) . ? C44 C49 1.401(17) . ? C44 N12 1.408(14) . ? C45 C46 1.428(17) . ? C45 H45 0.9300 . ? C46 C47 1.41(2) . ? C46 H46 0.9300 . ? C47 C48 1.29(2) . ? C47 H47 0.9300 . ? C48 C49 1.359(16) . ? C48 H48 0.9300 . ? C49 N13 1.448(15) . ? C50 N13 1.455(15) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 N13 1.332(14) . ? C51 N12 1.347(14) . ? C51 C52 1.457(15) . ? C52 N11 1.521(13) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.455(17) . ? C53 S2 1.823(10) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.565(17) . ? C54 C60 1.589(15) . ? C54 C59 1.617(17) . ? C55 O6 1.12(2) . ? C55 C56 1.63(2) . ? C56 C57 1.443(18) . ? C56 H56A 0.9700 . ? C56 H56B 0.9700 . ? C57 C58 1.543(19) . ? C57 C60 1.561(16) . ? C57 H57 0.9800 . ? C58 C59 1.506(19) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 C61 1.479(16) . ? C60 C62 1.518(15) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C65 N15 1.120(15) . ? C65 C66 1.45(2) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 N16 1.192(16) . ? C67 C68 1.40(2) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? N11 S2 1.696(9) . ? S2 O4 1.419(8) . ? S2 O5 1.427(8) . ? Cl1 O7 1.415(10) . ? Cl1 O8 1.428(9) . ? Cl1 O10 1.435(10) . ? Cl1 O9 1.436(10) . ? Cl2 O12 1.383(9) . ? Cl2 O14 1.405(10) . ? Cl2 O11 1.445(9) . ? Cl2 O13 1.452(10) . ? Cl3 O17A 1.32(2) . ? Cl3 O17 1.36(3) . ? Cl3 O16 1.380(17) . ? Cl3 O18A 1.421(18) . ? Cl3 O15A 1.44(3) . ? Cl3 O15 1.48(2) . ? Cl3 O18 1.61(5) . ? Cl4 O21 1.23(3) . ? Cl4 O19 1.251(12) . ? Cl4 O20A 1.28(4) . ? Cl4 O21A 1.32(2) . ? Cl4 O22 1.48(2) . ? Cl4 O20 1.52(3) . ? O19 O21 1.79(3) . ? O20A O22 1.37(4) . ? C69 N17 1.19(2) . ? C69 C70 1.40(3) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 N18 1.22(2) . ? C71 C72 1.40(2) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 N19 1.17(2) . ? C73 C74 1.40(2) . ? C74 H74A 0.9600 . ? C74 H74B 0.9600 . ? C74 H74C 0.9600 . ? C75 N20 0.972(19) . ? C75 C76 1.45(3) . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? N14 C63 1.057(17) . ? C63 C64 1.48(2) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? 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 N6 168.3(4) . . ? N1 Ni1 N8 86.6(4) . . ? N6 Ni1 N8 86.2(4) . . ? N1 Ni1 N5 93.9(4) . . ? N6 Ni1 N5 92.3(4) . . ? N8 Ni1 N5 174.1(4) . . ? N1 Ni1 N7 100.3(4) . . ? N6 Ni1 N7 89.2(4) . . ? N8 Ni1 N7 92.1(4) . . ? N5 Ni1 N7 93.7(4) . . ? N1 Ni1 N3 77.6(4) . . ? N6 Ni1 N3 94.2(4) . . ? N8 Ni1 N3 97.7(4) . . ? N5 Ni1 N3 76.6(4) . . ? N7 Ni1 N3 169.8(4) . . ? C2 C1 C6 122.1(11) . . ? C2 C1 N1 131.8(10) . . ? C6 C1 N1 106.1(10) . . ? C3 C2 C1 115.7(12) . . ? C3 C2 H2 122.1 . . ? C1 C2 H2 122.1 . . ? C2 C3 C4 123.9(12) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? C5 C4 C3 118.8(11) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 119.8(11) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? N2 C6 C5 133.0(11) . . ? N2 C6 C1 107.8(10) . . ? C5 C6 C1 119.2(11) . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 N2 115.0(10) . . ? N1 C8 C9 126.4(11) . . ? N2 C8 C9 118.6(10) . . ? C8 C9 N3 105.8(9) . . ? C8 C9 H9A 110.6 . . ? N3 C9 H9A 110.6 . . ? C8 C9 H9B 110.6 . . ? N3 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? C11 C10 C15 123.8(14) . . ? C11 C10 N5 132.0(11) . . ? C15 C10 N5 104.2(12) . . ? C10 C11 C12 118.7(11) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C11 C12 C13 118.2(12) . . ? C11 C12 H12 120.9 . . ? C13 C12 H12 120.9 . . ? C14 C13 C12 123.6(13) . . ? C14 C13 H13 118.2 . . ? C12 C13 H13 118.2 . . ? C13 C14 C15 119.7(12) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N4 C15 C10 111.6(14) . . ? N4 C15 C14 132.1(11) . . ? C10 C15 C14 115.8(14) . . ? N4 C16 H16A 109.5 . . ? N4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 N5 112.6(12) . . ? N4 C17 C18 127.6(12) . . ? N5 C17 C18 119.8(12) . . ? C17 C18 N3 111.3(11) . . ? C17 C18 H18A 109.4 . . ? N3 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? N3 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C20 C19 S1 117.8(8) . . ? C20 C19 H19A 107.9 . . ? S1 C19 H19A 107.9 . . ? C20 C19 H19B 107.9 . . ? S1 C19 H19B 107.9 . . ? H19A C19 H19B 107.2 . . ? C19 C20 C21 119.6(11) . . ? C19 C20 C26 124.4(10) . . ? C21 C20 C26 98.5(10) . . ? C19 C20 C25 105.4(10) . . ? C21 C20 C25 102.8(10) . . ? C26 C20 C25 103.4(10) . . ? O3 C21 C22 130.5(13) . . ? O3 C21 C20 117.7(13) . . ? C22 C21 C20 110.8(12) . . ? C21 C22 C23 104.6(12) . . ? C21 C22 H22A 110.8 . . ? C23 C22 H22A 110.8 . . ? C21 C22 H22B 110.8 . . ? C23 C22 H22B 110.8 . . ? H22A C22 H22B 108.9 . . ? C24 C23 C26 100.0(13) . . ? C24 C23 C22 103.9(15) . . ? C26 C23 C22 97.2(13) . . ? C24 C23 H23 117.5 . . ? C26 C23 H23 117.5 . . ? C22 C23 H23 117.5 . . ? C23 C24 C25 106.3(12) . . ? C23 C24 H24A 110.5 . . ? C25 C24 H24A 110.5 . . ? C23 C24 H24B 110.5 . . ? C25 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? C20 C25 C24 99.6(11) . . ? C20 C25 H25A 111.8 . . ? C24 C25 H25A 111.8 . . ? C20 C25 H25B 111.8 . . ? C24 C25 H25B 111.8 . . ? H25A C25 H25B 109.6 . . ? C27 C26 C28 110.1(10) . . ? C27 C26 C20 111.7(11) . . ? C28 C26 C20 114.0(10) . . ? C27 C26 C23 112.3(11) . . ? C28 C26 C23 110.7(12) . . ? C20 C26 C23 97.7(12) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N6 C29 C30 173.8(17) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N7 C31 C32 173.9(16) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N8 C33 C34 174.7(16) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C8 N1 C1 105.0(9) . . ? C8 N1 Ni1 119.8(8) . . ? C1 N1 Ni1 134.9(7) . . ? C6 N2 C8 106.0(9) . . ? C6 N2 C7 126.3(10) . . ? C8 N2 C7 127.2(11) . . ? C18 N3 C9 110.3(11) . . ? C18 N3 S1 113.1(9) . . ? C9 N3 S1 112.5(8) . . ? C18 N3 Ni1 99.9(7) . . ? C9 N3 Ni1 106.6(7) . . ? S1 N3 Ni1 113.7(5) . . ? C15 N4 C17 107.1(11) . . ? C15 N4 C16 128.5(12) . . ? C17 N4 C16 123.0(13) . . ? C17 N5 C10 104.2(10) . . ? C17 N5 Ni1 116.2(9) . . ? C10 N5 Ni1 139.5(8) . . ? C29 N6 Ni1 173.1(12) . . ? C31 N7 Ni1 175.7(10) . . ? C33 N8 Ni1 157.9(10) . . ? O1 S1 O2 119.5(5) . . ? O1 S1 N3 106.6(5) . . ? O2 S1 N3 106.7(6) . . ? O1 S1 C19 111.5(5) . . ? O2 S1 C19 109.5(6) . . ? N3 S1 C19 101.3(5) . . ? N12 Ni2 N14 86.4(4) . . ? N12 Ni2 N15 98.7(4) . . ? N14 Ni2 N15 89.8(4) . . ? N12 Ni2 N9 95.7(4) . . ? N14 Ni2 N9 172.3(4) . . ? N15 Ni2 N9 97.2(4) . . ? N12 Ni2 N16 169.2(4) . . ? N14 Ni2 N16 87.2(4) . . ? N15 Ni2 N16 90.0(4) . . ? N9 Ni2 N16 89.5(4) . . ? N12 Ni2 N11 77.9(3) . . ? N14 Ni2 N11 97.4(4) . . ? N15 Ni2 N11 171.8(4) . . ? N9 Ni2 N11 75.9(3) . . ? N16 Ni2 N11 94.3(3) . . ? C36 C35 N9 132.8(10) . . ? C36 C35 C40 118.2(10) . . ? N9 C35 C40 108.8(9) . . ? C35 C36 C37 117.8(10) . . ? C35 C36 H36 121.1 . . ? C37 C36 H36 121.1 . . ? C38 C37 C36 124.2(11) . . ? C38 C37 H37 117.9 . . ? C36 C37 H37 117.9 . . ? C37 C38 C39 120.3(12) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 112.7(10) . . ? C40 C39 H39 123.7 . . ? C38 C39 H39 123.7 . . ? C39 C40 C35 126.7(9) . . ? C39 C40 N10 129.1(10) . . ? C35 C40 N10 104.2(8) . . ? N10 C41 H41A 109.5 . . ? N10 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N10 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N9 C42 N10 113.2(10) . . ? N9 C42 C43 122.6(10) . . ? N10 C42 C43 124.1(10) . . ? C42 C43 N11 107.4(8) . . ? C42 C43 H43A 110.2 . . ? N11 C43 H43A 110.2 . . ? C42 C43 H43B 110.2 . . ? N11 C43 H43B 110.2 . . ? H43A C43 H43B 108.5 . . ? C45 C44 C49 119.4(11) . . ? C45 C44 N12 132.0(10) . . ? C49 C44 N12 108.2(10) . . ? C44 C45 C46 116.5(12) . . ? C44 C45 H45 121.8 . . ? C46 C45 H45 121.8 . . ? C47 C46 C45 118.6(13) . . ? C47 C46 H46 120.7 . . ? C45 C46 H46 120.7 . . ? C48 C47 C46 124.6(12) . . ? C48 C47 H47 117.7 . . ? C46 C47 H47 117.7 . . ? C47 C48 C49 115.8(13) . . ? C47 C48 H48 122.1 . . ? C49 C48 H48 122.1 . . ? C48 C49 C44 124.5(13) . . ? C48 C49 N13 129.9(12) . . ? C44 C49 N13 105.6(10) . . ? N13 C50 H50A 109.5 . . ? N13 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N13 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N13 C51 N12 112.8(9) . . ? N13 C51 C52 125.9(10) . . ? N12 C51 C52 121.3(9) . . ? C51 C52 N11 112.1(8) . . ? C51 C52 H52A 109.2 . . ? N11 C52 H52A 109.2 . . ? C51 C52 H52B 109.2 . . ? N11 C52 H52B 109.2 . . ? H52A C52 H52B 107.9 . . ? C54 C53 S2 114.7(8) . . ? C54 C53 H53A 108.6 . . ? S2 C53 H53A 108.6 . . ? C54 C53 H53B 108.6 . . ? S2 C53 H53B 108.6 . . ? H53A C53 H53B 107.6 . . ? C53 C54 C55 113.2(12) . . ? C53 C54 C60 114.0(9) . . ? C55 C54 C60 99.7(9) . . ? C53 C54 C59 120.1(9) . . ? C55 C54 C59 106.4(11) . . ? C60 C54 C59 101.0(9) . . ? O6 C55 C54 133.3(15) . . ? O6 C55 C56 125.1(11) . . ? C54 C55 C56 101.6(14) . . ? C57 C56 C55 100.6(10) . . ? C57 C56 H56A 111.6 . . ? C55 C56 H56A 111.6 . . ? C57 C56 H56B 111.6 . . ? C55 C56 H56B 111.6 . . ? H56A C56 H56B 109.4 . . ? C56 C57 C58 111.4(11) . . ? C56 C57 C60 108.4(12) . . ? C58 C57 C60 104.8(9) . . ? C56 C57 H57 110.7 . . ? C58 C57 H57 110.7 . . ? C60 C57 H57 110.7 . . ? C59 C58 C57 99.8(10) . . ? C59 C58 H58A 111.8 . . ? C57 C58 H58A 111.8 . . ? C59 C58 H58B 111.8 . . ? C57 C58 H58B 111.8 . . ? H58A C58 H58B 109.5 . . ? C58 C59 C54 105.9(9) . . ? C58 C59 H59A 110.6 . . ? C54 C59 H59A 110.6 . . ? C58 C59 H59B 110.6 . . ? C54 C59 H59B 110.6 . . ? H59A C59 H59B 108.7 . . ? C61 C60 C62 110.6(9) . . ? C61 C60 C57 114.9(10) . . ? C62 C60 C57 115.0(11) . . ? C61 C60 C54 113.0(10) . . ? C62 C60 C54 112.3(9) . . ? C57 C60 C54 89.6(8) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N15 C65 C66 177.9(14) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N16 C67 C68 178.8(14) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C42 N9 C35 107.3(9) . . ? C42 N9 Ni2 116.0(8) . . ? C35 N9 Ni2 136.6(7) . . ? C42 N10 C40 106.4(9) . . ? C42 N10 C41 130.3(10) . . ? C40 N10 C41 123.2(9) . . ? C43 N11 C52 109.9(8) . . ? C43 N11 S2 113.3(7) . . ? C52 N11 S2 113.4(7) . . ? C43 N11 Ni2 102.3(6) . . ? C52 N11 Ni2 104.5(6) . . ? S2 N11 Ni2 112.6(4) . . ? C51 N12 C44 106.6(9) . . ? C51 N12 Ni2 118.2(7) . . ? C44 N12 Ni2 134.8(8) . . ? C51 N13 C49 106.7(9) . . ? C51 N13 C50 128.5(9) . . ? C49 N13 C50 124.8(9) . . ? C65 N15 Ni2 177.6(10) . . ? C67 N16 Ni2 164.8(9) . . ? O4 S2 O5 119.2(5) . . ? O4 S2 N11 105.6(4) . . ? O5 S2 N11 104.8(5) . . ? O4 S2 C53 107.6(5) . . ? O5 S2 C53 112.2(5) . . ? N11 S2 C53 106.5(5) . . ? O7 Cl1 O8 112.8(7) . . ? O7 Cl1 O10 106.3(8) . . ? O8 Cl1 O10 107.4(7) . . ? O7 Cl1 O9 112.5(7) . . ? O8 Cl1 O9 108.7(6) . . ? O10 Cl1 O9 109.0(6) . . ? O12 Cl2 O14 111.0(6) . . ? O12 Cl2 O11 109.3(6) . . ? O14 Cl2 O11 108.0(7) . . ? O12 Cl2 O13 112.5(6) . . ? O14 Cl2 O13 109.3(7) . . ? O11 Cl2 O13 106.6(7) . . ? O17A Cl3 O17 39.2(14) . . ? O17A Cl3 O16 104.1(14) . . ? O17 Cl3 O16 129.8(16) . . ? O17A Cl3 O18A 105.9(17) . . ? O17 Cl3 O18A 113.0(16) . . ? O16 Cl3 O18A 109.5(11) . . ? O17A Cl3 O15A 105(2) . . ? O17 Cl3 O15A 67(2) . . ? O16 Cl3 O15A 119(2) . . ? O18A Cl3 O15A 111.5(18) . . ? O17A Cl3 O15 128.1(14) . . ? O17 Cl3 O15 94(2) . . ? O16 Cl3 O15 90.3(15) . . ? O18A Cl3 O15 115.8(18) . . ? O15A Cl3 O15 31.6(17) . . ? O17A Cl3 O18 124(3) . . ? O17 Cl3 O18 119.5(19) . . ? O16 Cl3 O18 109.8(16) . . ? O18A Cl3 O18 20.9(18) . . ? O15A Cl3 O18 95(3) . . ? O15 Cl3 O18 95(3) . . ? O21 Cl4 O19 92.5(15) . . ? O21 Cl4 O20A 125(2) . . ? O19 Cl4 O20A 142.8(19) . . ? O21 Cl4 O21A 41.8(13) . . ? O19 Cl4 O21A 126.9(13) . . ? O20A Cl4 O21A 87.8(19) . . ? O21 Cl4 O22 109.9(15) . . ? O19 Cl4 O22 111.0(14) . . ? O20A Cl4 O22 59.1(18) . . ? O21A Cl4 O22 110.0(12) . . ? O21 Cl4 O20 143.7(17) . . ? O19 Cl4 O20 89.7(15) . . ? O20A Cl4 O20 61.6(19) . . ? O21A Cl4 O20 112.2(15) . . ? O22 Cl4 O20 103.0(14) . . ? Cl4 O19 O21 43.3(10) . . ? Cl4 O20A O22 68(2) . . ? Cl4 O21 O19 44.2(10) . . ? O20A O22 Cl4 53.3(19) . . ? N17 C69 C70 176(2) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N18 C71 C72 173.8(14) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N19 C73 C74 179.6(16) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N20 C75 C76 174.6(19) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C63 N14 Ni2 161.0(12) . . ? N14 C63 C64 173.4(18) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.121 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.226 # Attachment 'WZL002.cif' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 634029' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H54 Cl4 N10 Ni2 O4' _chemical_formula_sum 'C40 H54 Cl4 N10 Ni2 O4' _chemical_formula_weight 998.15 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' Ni Ni 0.3393 1.1124 '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' _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 8.4850(2) _cell_length_b 11.8690(3) _cell_length_c 12.9820(4) _cell_angle_alpha 113.6570(10) _cell_angle_beta 99.9230(10) _cell_angle_gamma 100.4470(10) _cell_volume 1133.25(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 23359 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7273 _exptl_absorpt_correction_T_max 0.8003 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17699 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4000 _reflns_number_gt 3328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & M 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0854P)^2^+0.6869P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.024(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4000 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.53111(5) 0.15566(4) 0.11005(4) 0.0353(2) Uani 1 1 d . . . Cl1 Cl 0.82600(11) 0.20240(9) 0.14692(8) 0.0481(3) Uani 1 1 d . . . Cl2 Cl 0.49395(11) 0.05793(8) -0.10239(7) 0.0402(3) Uani 1 1 d . . . O1 O 0.1728(6) 0.7951(5) 0.1390(6) 0.1136(16) Uani 1 1 d . . . H1 H 0.2327 0.8306 0.1113 0.170 Uiso 1 1 calc R . . O2 O 0.8459(8) 0.0312(6) 0.3226(7) 0.168(3) Uani 1 1 d . . . H2' H 0.7798 0.0378 0.2726 0.252 Uiso 1 1 calc R . . N1 N 0.4970(4) 0.3216(3) 0.1093(2) 0.0387(7) Uani 1 1 d . . . N2 N 0.3200(4) 0.4306(3) 0.0817(3) 0.0489(8) Uani 1 1 d . . . N3 N 0.2630(4) 0.1088(3) 0.0693(3) 0.0398(7) Uani 1 1 d . . . H3' H 0.233(6) 0.035(4) 0.017(4) 0.055(13) Uiso 1 1 d . . . N4 N 0.3364(4) 0.2581(3) 0.3913(3) 0.0489(8) Uani 1 1 d . . . N5 N 0.5066(4) 0.2239(3) 0.2771(2) 0.0378(7) Uani 1 1 d . . . C1 C 0.5858(5) 0.4483(4) 0.1501(3) 0.0457(9) Uani 1 1 d . . . C2 C 0.7552(6) 0.5088(4) 0.2050(4) 0.0562(11) Uani 1 1 d . . . H2 H 0.8287 0.4604 0.2182 0.067 Uiso 1 1 d R . . C3 C 0.8088(7) 0.6392(5) 0.2391(4) 0.0712(14) Uani 1 1 d . . . H3 H 0.9239 0.6853 0.2775 0.085 Uiso 1 1 d R . . C4 C 0.6962(9) 0.7068(5) 0.2160(4) 0.0760(16) Uani 1 1 d . . . H4 H 0.7372 0.7970 0.2402 0.091 Uiso 1 1 d R . . C5 C 0.5315(8) 0.6470(5) 0.1626(4) 0.0696(14) Uani 1 1 d . . . H5 H 0.4544 0.6917 0.1464 0.084 Uiso 1 1 d R . . C6 C 0.4747(6) 0.5169(4) 0.1314(3) 0.0517(10) Uani 1 1 d . . . C7 C 0.1623(6) 0.4587(5) 0.0500(4) 0.0662(13) Uani 1 1 d . . . H7A H 0.1854 0.5475 0.0670 0.079 Uiso 1 1 d R . . H7B H 0.0902 0.4413 0.0945 0.079 Uiso 1 1 d R . . H7C H 0.1090 0.4067 -0.0319 0.079 Uiso 1 1 d R . . C8 C 0.3406(5) 0.3154(4) 0.0708(3) 0.0425(9) Uani 1 1 d . . . C9 C 0.2055(5) 0.1925(4) 0.0213(4) 0.0480(10) Uani 1 1 d . . . H9A H 0.1802 0.1511 -0.0624 0.058 Uiso 1 1 d R . . H9B H 0.1071 0.2092 0.0441 0.058 Uiso 1 1 d R . . C10 C 0.2104(5) 0.1171(4) 0.1740(4) 0.0471(9) Uani 1 1 d . . . H10A H 0.1184 0.1538 0.1775 0.057 Uiso 1 1 d R . . H10B H 0.1764 0.0331 0.1694 0.057 Uiso 1 1 d R . . C11 C 0.3508(4) 0.2006(3) 0.2810(3) 0.0408(8) Uani 1 1 d . . . C12 C 0.1840(7) 0.2527(6) 0.4289(5) 0.0750(15) Uani 1 1 d . . . H12A H 0.2120 0.3023 0.5122 0.090 Uiso 1 1 d R . . H12B H 0.1290 0.1654 0.4081 0.090 Uiso 1 1 d R . . H12C H 0.1113 0.2869 0.3918 0.090 Uiso 1 1 d R . . C13 C 0.4955(5) 0.3254(4) 0.4635(4) 0.0497(10) Uani 1 1 d . . . C14 C 0.5549(7) 0.4029(5) 0.5834(4) 0.0695(13) Uani 1 1 d . . . H14 H 0.4793 0.4169 0.6314 0.083 Uiso 1 1 d R . . C15 C 0.7255(8) 0.4566(5) 0.6269(4) 0.0798(16) Uani 1 1 d . . . H15 H 0.7703 0.5142 0.7086 0.096 Uiso 1 1 d R . . C16 C 0.8322(7) 0.4323(5) 0.5562(4) 0.0680(13) Uani 1 1 d . . . H16 H 0.9496 0.4685 0.5933 0.082 Uiso 1 1 d R . . C17 C 0.7726(5) 0.3558(4) 0.4368(4) 0.0519(10) Uani 1 1 d . . . H17 H 0.8441 0.3406 0.3857 0.062 Uiso 1 1 d R . . C18 C 0.6022(5) 0.3024(3) 0.3909(3) 0.0407(8) Uani 1 1 d . . . C19 C 0.2339(10) 0.8578(8) 0.2641(8) 0.116(3) Uani 1 1 d . . . H19A H 0.3330 0.9259 0.2873 0.174 Uiso 1 1 calc R . . H19B H 0.2591 0.7972 0.2913 0.174 Uiso 1 1 calc R . . H19C H 0.1506 0.8922 0.2973 0.174 Uiso 1 1 calc R . . C20 C 0.7722(18) 0.0429(9) 0.4237(10) 0.195(6) Uani 1 1 d . . . H20A H 0.8536 0.0433 0.4853 0.292 Uiso 1 1 calc R . . H20B H 0.6760 -0.0284 0.3976 0.292 Uiso 1 1 calc R . . H20C H 0.7405 0.1211 0.4522 0.292 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0277(3) 0.0430(3) 0.0352(3) 0.0131(2) 0.01045(19) 0.0181(2) Cl1 0.0283(5) 0.0593(6) 0.0501(6) 0.0151(5) 0.0115(4) 0.0180(4) Cl2 0.0389(5) 0.0462(5) 0.0378(5) 0.0164(4) 0.0132(4) 0.0201(4) O1 0.077(3) 0.117(4) 0.186(5) 0.096(4) 0.058(3) 0.028(3) O2 0.142(5) 0.096(4) 0.200(7) 0.071(4) -0.081(5) -0.006(3) N1 0.0378(17) 0.0456(17) 0.0361(16) 0.0158(14) 0.0139(13) 0.0214(13) N2 0.062(2) 0.059(2) 0.0450(18) 0.0268(17) 0.0257(16) 0.0412(18) N3 0.0303(16) 0.0442(18) 0.0435(18) 0.0145(16) 0.0107(13) 0.0184(14) N4 0.050(2) 0.067(2) 0.0475(19) 0.0302(17) 0.0294(16) 0.0320(17) N5 0.0337(16) 0.0429(16) 0.0370(16) 0.0136(14) 0.0136(13) 0.0177(13) C1 0.058(2) 0.049(2) 0.0334(19) 0.0160(17) 0.0208(18) 0.0212(19) C2 0.067(3) 0.051(2) 0.046(2) 0.0175(19) 0.020(2) 0.012(2) C3 0.090(4) 0.053(3) 0.058(3) 0.016(2) 0.030(3) 0.004(3) C4 0.121(5) 0.049(3) 0.060(3) 0.022(2) 0.041(3) 0.018(3) C5 0.120(5) 0.058(3) 0.054(3) 0.030(2) 0.045(3) 0.045(3) C6 0.081(3) 0.053(2) 0.037(2) 0.0220(19) 0.030(2) 0.039(2) C7 0.081(3) 0.086(3) 0.054(3) 0.034(2) 0.024(2) 0.062(3) C8 0.047(2) 0.055(2) 0.0370(19) 0.0201(17) 0.0197(16) 0.0319(18) C9 0.035(2) 0.065(3) 0.047(2) 0.023(2) 0.0110(17) 0.0253(18) C10 0.0318(19) 0.060(2) 0.059(2) 0.029(2) 0.0204(18) 0.0215(17) C11 0.039(2) 0.047(2) 0.045(2) 0.0213(17) 0.0207(16) 0.0230(16) C12 0.069(3) 0.107(4) 0.080(3) 0.052(3) 0.052(3) 0.044(3) C13 0.063(3) 0.055(2) 0.043(2) 0.0233(19) 0.026(2) 0.027(2) C14 0.086(4) 0.085(3) 0.041(2) 0.023(2) 0.030(2) 0.032(3) C15 0.104(5) 0.080(4) 0.035(2) 0.014(2) 0.012(3) 0.014(3) C16 0.070(3) 0.071(3) 0.045(2) 0.019(2) 0.005(2) 0.005(2) C17 0.048(2) 0.059(2) 0.041(2) 0.0180(19) 0.0092(18) 0.0112(19) C18 0.047(2) 0.044(2) 0.0369(19) 0.0183(17) 0.0159(16) 0.0196(17) C19 0.117(6) 0.119(6) 0.161(8) 0.089(6) 0.073(6) 0.047(5) C20 0.34(2) 0.082(6) 0.129(8) 0.034(6) 0.031(10) 0.034(8) _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 2.046(3) . ? Ni1 N5 2.051(3) . ? Ni1 N3 2.157(3) . ? Ni1 Cl1 2.3809(9) . ? Ni1 Cl2 2.4600(10) . ? Ni1 Cl2 2.4651(10) 2_655 ? Cl2 Ni1 2.4650(10) 2_655 ? O1 C19 1.435(9) . ? O1 H1 0.8200 . ? O2 C20 1.517(13) . ? O2 H2' 0.8200 . ? N1 C8 1.312(5) . ? N1 C1 1.386(5) . ? N2 C8 1.365(5) . ? N2 C6 1.371(6) . ? N2 C7 1.467(5) . ? N3 C10 1.475(5) . ? N3 C9 1.477(5) . ? N3 H3' 0.82(5) . ? N4 C11 1.355(5) . ? N4 C13 1.383(6) . ? N4 C12 1.458(5) . ? N5 C11 1.315(5) . ? N5 C18 1.385(5) . ? C1 C2 1.397(6) . ? C1 C6 1.404(6) . ? C2 C3 1.387(6) . ? C2 H2 0.9594 . ? C3 C4 1.421(8) . ? C3 H3 0.9598 . ? C4 C5 1.359(8) . ? C4 H4 0.9608 . ? C5 C6 1.393(7) . ? C5 H5 0.9601 . ? C7 H7A 0.9599 . ? C7 H7B 0.9604 . ? C7 H7C 0.9604 . ? C8 C9 1.497(6) . ? C9 H9A 0.9597 . ? C9 H9B 0.9603 . ? C10 C11 1.492(5) . ? C10 H10A 0.9596 . ? C10 H10B 0.9606 . ? C12 H12A 0.9603 . ? C12 H12B 0.9597 . ? C12 H12C 0.9605 . ? C13 C14 1.391(6) . ? C13 C18 1.399(5) . ? C14 C15 1.384(8) . ? C14 H14 0.9595 . ? C15 C16 1.384(7) . ? C15 H15 0.9601 . ? C16 C17 1.384(6) . ? C16 H16 0.9603 . ? C17 C18 1.384(6) . ? C17 H17 0.9607 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? 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 87.96(11) . . ? N1 Ni1 N3 80.39(12) . . ? N5 Ni1 N3 81.22(12) . . ? N1 Ni1 Cl1 100.04(9) . . ? N5 Ni1 Cl1 101.06(8) . . ? N3 Ni1 Cl1 177.69(9) . . ? N1 Ni1 Cl2 90.89(8) . . ? N5 Ni1 Cl2 167.51(8) . . ? N3 Ni1 Cl2 86.33(9) . . ? Cl1 Ni1 Cl2 91.39(3) . . ? N1 Ni1 Cl2 167.57(9) . 2_655 ? N5 Ni1 Cl2 89.72(9) . 2_655 ? N3 Ni1 Cl2 87.18(9) . 2_655 ? Cl1 Ni1 Cl2 92.39(3) . 2_655 ? Cl2 Ni1 Cl2 88.73(3) . 2_655 ? Ni1 Cl2 Ni1 91.27(3) . 2_655 ? C19 O1 H1 109.5 . . ? C20 O2 H2' 109.5 . . ? C8 N1 C1 106.0(3) . . ? C8 N1 Ni1 113.7(3) . . ? C1 N1 Ni1 139.7(3) . . ? C8 N2 C6 106.9(3) . . ? C8 N2 C7 126.9(4) . . ? C6 N2 C7 126.2(4) . . ? C10 N3 C9 114.2(3) . . ? C10 N3 Ni1 109.4(2) . . ? C9 N3 Ni1 108.9(2) . . ? C10 N3 H3' 112(3) . . ? C9 N3 H3' 109(3) . . ? Ni1 N3 H3' 103(3) . . ? C11 N4 C13 106.9(3) . . ? C11 N4 C12 127.5(4) . . ? C13 N4 C12 125.6(4) . . ? C11 N5 C18 106.4(3) . . ? C11 N5 Ni1 113.3(2) . . ? C18 N5 Ni1 139.7(2) . . ? N1 C1 C2 130.0(4) . . ? N1 C1 C6 108.7(4) . . ? C2 C1 C6 121.3(4) . . ? C3 C2 C1 117.1(5) . . ? C3 C2 H2 122.9 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 121.1(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 118.6 . . ? C5 C4 C3 121.4(5) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 118.3(5) . . ? C4 C5 H5 122.0 . . ? C6 C5 H5 119.7 . . ? N2 C6 C5 133.2(4) . . ? N2 C6 C1 106.0(4) . . ? C5 C6 C1 120.8(5) . . ? N2 C7 H7A 108.7 . . ? N2 C7 H7B 109.8 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.8 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 N2 112.4(4) . . ? N1 C8 C9 121.5(3) . . ? N2 C8 C9 126.1(3) . . ? N3 C9 C8 108.4(3) . . ? N3 C9 H9A 110.0 . . ? C8 C9 H9A 110.4 . . ? N3 C9 H9B 108.7 . . ? C8 C9 H9B 109.9 . . ? H9A C9 H9B 109.5 . . ? N3 C10 C11 109.8(3) . . ? N3 C10 H10A 108.5 . . ? C11 C10 H10A 109.3 . . ? N3 C10 H10B 109.9 . . ? C11 C10 H10B 109.8 . . ? H10A C10 H10B 109.5 . . ? N5 C11 N4 112.3(3) . . ? N5 C11 C10 122.0(3) . . ? N4 C11 C10 125.7(3) . . ? N4 C12 H12A 109.0 . . ? N4 C12 H12B 109.4 . . ? H12A C12 H12B 109.5 . . ? N4 C12 H12C 109.9 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C14 132.0(4) . . ? N4 C13 C18 106.0(3) . . ? C14 C13 C18 121.9(4) . . ? C15 C14 C13 116.3(4) . . ? C15 C14 H14 123.3 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 122.1(4) . . ? C14 C15 H15 118.5 . . ? C16 C15 H15 119.3 . . ? C17 C16 C15 121.4(5) . . ? C17 C16 H16 121.1 . . ? C15 C16 H16 117.5 . . ? C18 C17 C16 117.5(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 122.7 . . ? C17 C18 N5 130.9(3) . . ? C17 C18 C13 120.7(4) . . ? N5 C18 C13 108.4(3) . . ? O1 C19 H19A 109.5 . . ? O1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2 C20 H20A 109.5 . . ? O2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.670 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.165 data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 634030' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H33 Cl2 N5 Ni O3 S' _chemical_formula_sum 'C28 H33 Cl2 N5 Ni O3 S' _chemical_formula_weight 649.26 _chemical_absolute_configuration unk 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.3810(6) _cell_length_b 14.6380(7) _cell_length_c 15.5530(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2818.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 27459 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.028 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.993 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13794 _diffrn_reflns_av_R_equivalents 0.0960 _diffrn_reflns_av_sigmaI/netI 0.1120 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4891 _reflns_number_gt 3576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (O & M 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0823P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0017(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 4891 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.24169(7) 0.00280(6) 0.01968(5) 0.0245(3) Uani 1 1 d . . . Cl1 Cl 0.15449(15) 0.01178(13) 0.14652(11) 0.0334(5) Uani 1 1 d . . . Cl2 Cl 0.13152(15) -0.01500(12) -0.09489(11) 0.0313(5) Uani 1 1 d . . . S1 S 0.60388(15) 0.02386(11) 0.18170(11) 0.0234(4) Uani 1 1 d . . . O1 O 0.6434(5) 0.1093(3) 0.1511(3) 0.0314(13) Uani 1 1 d . . . O2 O 0.6450(4) -0.0594(3) 0.1472(3) 0.0241(12) Uani 1 1 d . . . O3 O 0.6635(5) -0.1734(3) 0.3160(3) 0.0328(13) Uani 1 1 d . . . N1 N 0.3398(6) 0.1104(4) 0.0102(4) 0.0259(15) Uani 1 1 d . . . N2 N 0.4589(6) 0.2203(4) 0.0401(4) 0.0258(15) Uani 1 1 d . . . N3 N 0.4737(5) 0.0235(4) 0.1634(3) 0.0224(13) Uani 1 1 d . . . N4 N 0.4723(6) -0.1942(4) 0.0783(4) 0.0250(15) Uani 1 1 d . . . N5 N 0.3501(5) -0.0987(3) 0.0261(4) 0.0213(14) Uani 1 1 d . . . C1 C 0.3568(7) 0.1635(4) -0.0649(5) 0.0224(17) Uani 1 1 d . . . C2 C 0.3187(7) 0.1537(5) -0.1471(6) 0.033(2) Uani 1 1 d . . . H2 H 0.2687 0.1054 -0.1594 0.040 Uiso 1 1 d R . . C3 C 0.3543(8) 0.2157(5) -0.2082(5) 0.037(2) Uani 1 1 d . . . H3 H 0.3283 0.2093 -0.2660 0.044 Uiso 1 1 d R . . C4 C 0.4239(8) 0.2843(5) -0.1876(5) 0.037(2) Uani 1 1 d . . . H4 H 0.4479 0.3242 -0.2327 0.044 Uiso 1 1 d R . . C5 C 0.4620(8) 0.2963(5) -0.1068(6) 0.036(2) Uani 1 1 d . . . H5 H 0.5070 0.3459 -0.0883 0.043 Uiso 1 1 d R . . C6 C 0.4321(7) 0.2325(5) -0.0448(5) 0.0261(18) Uani 1 1 d . . . C7 C 0.5381(7) 0.2783(5) 0.0830(5) 0.033(2) Uani 1 1 d . . . H7A H 0.5632 0.3251 0.0447 0.040 Uiso 1 1 d R . . H7B H 0.5981 0.2416 0.1012 0.040 Uiso 1 1 d R . . H7C H 0.5048 0.3060 0.1323 0.040 Uiso 1 1 d R . . C8 C 0.4039(7) 0.1473(4) 0.0711(5) 0.0240(18) Uani 1 1 d . . . C9 C 0.4127(7) 0.1101(4) 0.1600(5) 0.0271(18) Uani 1 1 d . . . H9A H 0.3412 0.0996 0.1817 0.033 Uiso 1 1 d R . . H9B H 0.4484 0.1545 0.1954 0.033 Uiso 1 1 d R . . C10 C 0.4164(6) -0.0637(4) 0.1738(4) 0.0232(17) Uani 1 1 d . . . H10A H 0.4505 -0.0988 0.2183 0.028 Uiso 1 1 d R . . H10B H 0.3431 -0.0509 0.1898 0.028 Uiso 1 1 d R . . C11 C 0.4131(6) -0.1195(4) 0.0936(4) 0.0214(17) Uani 1 1 d . . . C12 C 0.5493(7) -0.2417(5) 0.1346(5) 0.0262(18) Uani 1 1 d . . . H12A H 0.5535 -0.2097 0.1884 0.031 Uiso 1 1 d R . . H12B H 0.6192 -0.2422 0.1079 0.031 Uiso 1 1 d R . . H12C H 0.5260 -0.3033 0.1445 0.031 Uiso 1 1 d R . . C13 C 0.4503(7) -0.2250(4) -0.0040(4) 0.0247(18) Uani 1 1 d . . . C14 C 0.4894(7) -0.2985(5) -0.0507(5) 0.0278(19) Uani 1 1 d . . . H14 H 0.5416 -0.3385 -0.0247 0.033 Uiso 1 1 d R . . C15 C 0.4483(8) -0.3103(5) -0.1316(5) 0.034(2) Uani 1 1 d . . . H15 H 0.4722 -0.3601 -0.1669 0.041 Uiso 1 1 d R . . C16 C 0.3732(8) -0.2498(5) -0.1665(5) 0.033(2) Uani 1 1 d . . . H16 H 0.3482 -0.2601 -0.2241 0.039 Uiso 1 1 d R . . C17 C 0.3344(7) -0.1757(5) -0.1205(5) 0.0276(19) Uani 1 1 d . . . H17 H 0.2820 -0.1334 -0.1425 0.033 Uiso 1 1 d R . . C18 C 0.3739(6) -0.1639(4) -0.0373(4) 0.0208(17) Uani 1 1 d . . . C19 C 0.6195(6) 0.0212(5) 0.2955(4) 0.0285(17) Uani 1 1 d . . . H19A H 0.6128 0.0822 0.3177 0.034 Uiso 1 1 d R . . H19B H 0.5638 -0.0166 0.3196 0.034 Uiso 1 1 d R . . C20 C 0.7248(6) -0.0160(4) 0.3292(4) 0.0216(16) Uani 1 1 d . . . C21 C 0.7272(7) -0.1174(5) 0.3448(4) 0.0281(18) Uani 1 1 d . . . C22 C 0.8182(8) -0.1360(5) 0.4052(5) 0.036(2) Uani 1 1 d . . . H22A H 0.7913 -0.1664 0.4555 0.043 Uiso 1 1 d R . . H22B H 0.8695 -0.1747 0.3766 0.043 Uiso 1 1 d R . . C23 C 0.8607(6) -0.0407(5) 0.4233(5) 0.0300(18) Uani 1 1 d . . . H23 H 0.9080 -0.0338 0.4718 0.036 Uiso 1 1 d R . . C24 C 0.9212(6) -0.0106(6) 0.3417(4) 0.0350(19) Uani 1 1 d . . . H24A H 0.9692 -0.0571 0.3208 0.042 Uiso 1 1 d R . . H24B H 0.9603 0.0456 0.3487 0.042 Uiso 1 1 d R . . C25 C 0.8278(6) 0.0038(5) 0.2761(4) 0.0262(15) Uani 1 1 d . . . H25A H 0.8308 -0.0386 0.2290 0.031 Uiso 1 1 d R . . H25B H 0.8252 0.0651 0.2541 0.031 Uiso 1 1 d R . . C26 C 0.7583(6) 0.0186(4) 0.4213(4) 0.0238(16) Uani 1 1 d . . . C27 C 0.7782(7) 0.1203(5) 0.4277(5) 0.036(2) Uani 1 1 d . . . H27A H 0.7979 0.1361 0.4855 0.043 Uiso 1 1 d R . . H27B H 0.7137 0.1525 0.4118 0.043 Uiso 1 1 d R . . H27C H 0.8357 0.1367 0.3893 0.043 Uiso 1 1 d R . . C28 C 0.6730(6) -0.0084(6) 0.4901(4) 0.0295(17) Uani 1 1 d . . . H28A H 0.6956 0.0134 0.5455 0.035 Uiso 1 1 d R . . H28B H 0.6660 -0.0737 0.4918 0.035 Uiso 1 1 d R . . H28C H 0.6047 0.0184 0.4754 0.035 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0236(5) 0.0226(4) 0.0274(5) 0.0001(4) -0.0035(4) 0.0005(4) Cl1 0.0248(10) 0.0384(11) 0.0370(10) 0.0020(9) 0.0044(8) 0.0026(9) Cl2 0.0296(11) 0.0285(10) 0.0358(10) -0.0023(8) -0.0106(8) 0.0014(9) S1 0.0250(11) 0.0253(10) 0.0198(9) -0.0003(7) -0.0017(8) 0.0016(8) O1 0.033(4) 0.029(3) 0.032(3) 0.006(2) -0.006(3) -0.005(2) O2 0.026(3) 0.025(3) 0.021(3) -0.004(2) 0.002(2) -0.003(2) O3 0.043(4) 0.030(3) 0.026(3) 0.003(2) 0.007(3) -0.003(3) N1 0.026(4) 0.028(3) 0.024(3) -0.001(3) -0.004(3) 0.003(3) N2 0.024(4) 0.024(3) 0.030(4) -0.001(3) 0.004(3) 0.001(3) N3 0.024(3) 0.023(3) 0.020(3) -0.001(2) -0.003(3) 0.003(3) N4 0.029(4) 0.029(3) 0.017(3) -0.002(2) -0.004(3) 0.005(3) N5 0.013(4) 0.024(3) 0.027(3) -0.004(3) -0.004(3) -0.002(2) C1 0.021(5) 0.024(4) 0.023(4) 0.001(3) 0.002(4) 0.003(3) C2 0.024(5) 0.029(4) 0.046(5) -0.001(4) -0.002(4) 0.007(3) C3 0.046(6) 0.035(5) 0.030(5) 0.010(4) 0.005(4) 0.011(4) C4 0.042(6) 0.038(5) 0.030(5) 0.013(4) 0.009(4) 0.015(4) C5 0.032(6) 0.024(4) 0.053(6) 0.001(4) 0.016(5) 0.003(4) C6 0.029(5) 0.022(4) 0.027(4) -0.001(3) 0.003(4) 0.006(3) C7 0.033(5) 0.022(4) 0.045(5) -0.006(3) 0.001(4) -0.006(4) C8 0.030(5) 0.015(4) 0.027(4) -0.001(3) 0.005(4) 0.007(3) C9 0.030(5) 0.016(4) 0.036(5) -0.003(3) -0.007(4) 0.000(3) C10 0.022(5) 0.020(4) 0.027(4) 0.008(3) 0.002(4) -0.001(3) C11 0.025(5) 0.020(4) 0.019(4) -0.001(3) 0.007(4) 0.004(3) C12 0.028(5) 0.022(4) 0.028(4) 0.000(3) -0.005(4) 0.006(3) C13 0.027(5) 0.019(4) 0.028(4) 0.002(3) -0.003(4) -0.002(3) C14 0.028(5) 0.020(4) 0.035(5) -0.001(3) 0.007(4) -0.001(3) C15 0.042(6) 0.029(4) 0.033(5) -0.010(3) 0.006(4) 0.001(4) C16 0.047(6) 0.030(4) 0.021(4) -0.006(3) -0.002(4) -0.005(4) C17 0.029(5) 0.019(4) 0.035(5) 0.003(3) -0.001(4) 0.001(3) C18 0.025(5) 0.015(3) 0.022(4) -0.001(3) -0.003(3) -0.005(3) C19 0.027(4) 0.034(4) 0.024(4) 0.000(3) 0.002(3) -0.005(4) C20 0.021(4) 0.023(4) 0.021(4) 0.000(3) -0.011(3) 0.003(3) C21 0.037(5) 0.028(4) 0.019(4) -0.004(3) 0.007(4) 0.001(4) C22 0.048(6) 0.032(5) 0.027(5) 0.003(3) -0.008(4) 0.010(4) C23 0.024(5) 0.047(5) 0.019(4) -0.003(3) -0.009(3) 0.003(4) C24 0.028(4) 0.049(5) 0.028(4) -0.005(4) 0.002(3) -0.002(4) C25 0.027(4) 0.033(4) 0.019(3) -0.001(3) 0.002(3) 0.004(4) C26 0.024(4) 0.033(4) 0.015(3) -0.005(3) 0.003(3) -0.003(4) C27 0.033(6) 0.038(5) 0.036(5) 0.000(4) 0.005(4) -0.003(4) C28 0.024(4) 0.042(4) 0.023(3) -0.005(4) -0.007(3) -0.001(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 Ni1 N1 1.994(6) . ? Ni1 N5 2.005(6) . ? Ni1 Cl1 2.2526(19) . ? Ni1 Cl2 2.2592(19) . ? S1 O1 1.425(5) . ? S1 O2 1.426(5) . ? S1 N3 1.636(6) . ? S1 C19 1.781(7) . ? O3 C21 1.222(9) . ? N1 C8 1.348(10) . ? N1 C1 1.419(9) . ? N2 C8 1.355(9) . ? N2 C6 1.373(10) . ? N2 C7 1.459(10) . ? N3 C10 1.469(8) . ? N3 C9 1.477(9) . ? N4 C11 1.338(9) . ? N4 C13 1.384(9) . ? N4 C12 1.470(9) . ? N5 C11 1.342(9) . ? N5 C18 1.403(9) . ? C1 C2 1.370(11) . ? C1 C6 1.409(11) . ? C2 C3 1.387(11) . ? C2 H2 0.9590 . ? C3 C4 1.361(12) . ? C3 H3 0.9596 . ? C4 C5 1.354(12) . ? C4 H4 0.9599 . ? C5 C6 1.393(11) . ? C5 H5 0.9593 . ? C7 H7A 0.9595 . ? C7 H7B 0.9595 . ? C7 H7C 0.9604 . ? C8 C9 1.490(10) . ? C9 H9A 0.9598 . ? C9 H9B 0.9596 . ? C10 C11 1.492(9) . ? C10 H10A 0.9598 . ? C10 H10B 0.9595 . ? C12 H12A 0.9603 . ? C12 H12B 0.9599 . ? C12 H12C 0.9592 . ? C13 C14 1.386(10) . ? C13 C18 1.401(10) . ? C14 C15 1.368(11) . ? C14 H14 0.9613 . ? C15 C16 1.394(12) . ? C15 H15 0.9594 . ? C16 C17 1.385(11) . ? C16 H16 0.9597 . ? C17 C18 1.394(10) . ? C17 H17 0.9599 . ? C19 C20 1.507(10) . ? C19 H19A 0.9609 . ? C19 H19B 0.9603 . ? C20 C21 1.505(10) . ? C20 C25 1.547(10) . ? C20 C26 1.576(8) . ? C21 C22 1.492(11) . ? C22 C23 1.516(10) . ? C22 H22A 0.9597 . ? C22 H22B 0.9603 . ? C23 C26 1.537(10) . ? C23 C24 1.538(10) . ? C23 H23 0.9603 . ? C24 C25 1.556(10) . ? C24 H24A 0.9603 . ? C24 H24B 0.9607 . ? C25 H25A 0.9608 . ? C25 H25B 0.9609 . ? C26 C27 1.512(10) . ? C26 C28 1.555(9) . ? C27 H27A 0.9597 . ? C27 H27B 0.9597 . ? C27 H27C 0.9598 . ? C28 H28A 0.9605 . ? C28 H28B 0.9601 . ? C28 H28C 0.9598 . ? 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 100.4(2) . . ? N1 Ni1 Cl1 108.08(19) . . ? N5 Ni1 Cl1 108.69(19) . . ? N1 Ni1 Cl2 113.63(19) . . ? N5 Ni1 Cl2 110.99(18) . . ? Cl1 Ni1 Cl2 114.09(8) . . ? O1 S1 O2 120.1(3) . . ? O1 S1 N3 106.4(3) . . ? O2 S1 N3 106.5(3) . . ? O1 S1 C19 108.3(3) . . ? O2 S1 C19 108.5(3) . . ? N3 S1 C19 106.2(3) . . ? C8 N1 C1 105.7(6) . . ? C8 N1 Ni1 128.5(5) . . ? C1 N1 Ni1 125.7(5) . . ? C8 N2 C6 108.8(6) . . ? C8 N2 C7 129.4(6) . . ? C6 N2 C7 121.7(7) . . ? C10 N3 C9 120.2(6) . . ? C10 N3 S1 117.3(4) . . ? C9 N3 S1 120.5(5) . . ? C11 N4 C13 108.8(6) . . ? C11 N4 C12 129.6(6) . . ? C13 N4 C12 121.6(6) . . ? C11 N5 C18 105.9(6) . . ? C11 N5 Ni1 126.6(5) . . ? C18 N5 Ni1 127.5(5) . . ? C2 C1 C6 120.7(7) . . ? C2 C1 N1 131.3(7) . . ? C6 C1 N1 108.0(6) . . ? C1 C2 C3 117.5(8) . . ? C1 C2 H2 119.1 . . ? C3 C2 H2 123.4 . . ? C4 C3 C2 121.5(8) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 118.2 . . ? C5 C4 C3 122.4(7) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 118.2 . . ? C4 C5 C6 117.6(8) . . ? C4 C5 H5 125.4 . . ? C6 C5 H5 117.0 . . ? N2 C6 C5 133.6(8) . . ? N2 C6 C1 106.2(6) . . ? C5 C6 C1 120.2(7) . . ? N2 C7 H7A 110.5 . . ? N2 C7 H7B 109.2 . . ? H7A C7 H7B 109.4 . . ? N2 C7 H7C 108.8 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 N2 111.2(6) . . ? N1 C8 C9 123.3(7) . . ? N2 C8 C9 125.5(7) . . ? N3 C9 C8 112.6(6) . . ? N3 C9 H9A 108.8 . . ? C8 C9 H9A 108.5 . . ? N3 C9 H9B 109.0 . . ? C8 C9 H9B 108.6 . . ? H9A C9 H9B 109.4 . . ? N3 C10 C11 113.4(6) . . ? N3 C10 H10A 109.4 . . ? C11 C10 H10A 108.8 . . ? N3 C10 H10B 108.4 . . ? C11 C10 H10B 107.3 . . ? H10A C10 H10B 109.5 . . ? N4 C11 N5 111.4(6) . . ? N4 C11 C10 125.5(7) . . ? N5 C11 C10 123.1(6) . . ? N4 C12 H12A 108.9 . . ? N4 C12 H12B 109.4 . . ? H12A C12 H12B 109.4 . . ? N4 C12 H12C 110.2 . . ? H12A C12 H12C 109.6 . . ? H12B C12 H12C 109.5 . . ? N4 C13 C14 132.0(7) . . ? N4 C13 C18 105.5(6) . . ? C14 C13 C18 122.6(7) . . ? C15 C14 C13 116.7(8) . . ? C15 C14 H14 124.1 . . ? C13 C14 H14 119.2 . . ? C14 C15 C16 121.7(7) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 117.7 . . ? C17 C16 C15 121.8(7) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 118.6 . . ? C16 C17 C18 117.1(7) . . ? C16 C17 H17 123.7 . . ? C18 C17 H17 119.2 . . ? C17 C18 C13 120.0(7) . . ? C17 C18 N5 131.6(7) . . ? C13 C18 N5 108.4(6) . . ? C20 C19 S1 116.5(5) . . ? C20 C19 H19A 106.6 . . ? S1 C19 H19A 109.1 . . ? C20 C19 H19B 106.1 . . ? S1 C19 H19B 108.8 . . ? H19A C19 H19B 109.5 . . ? C21 C20 C19 115.4(6) . . ? C21 C20 C25 104.8(6) . . ? C19 C20 C25 117.4(5) . . ? C21 C20 C26 99.5(5) . . ? C19 C20 C26 115.3(6) . . ? C25 C20 C26 102.0(5) . . ? O3 C21 C22 126.7(7) . . ? O3 C21 C20 126.1(7) . . ? C22 C21 C20 107.2(6) . . ? C21 C22 C23 102.2(6) . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22A 113.3 . . ? C21 C22 H22B 108.4 . . ? C23 C22 H22B 113.5 . . ? H22A C22 H22B 109.5 . . ? C22 C23 C26 103.3(6) . . ? C22 C23 C24 106.2(6) . . ? C26 C23 C24 102.8(6) . . ? C22 C23 H23 117.0 . . ? C26 C23 H23 117.3 . . ? C24 C23 H23 108.7 . . ? C23 C24 C25 102.6(6) . . ? C23 C24 H24A 112.2 . . ? C25 C24 H24A 109.5 . . ? C23 C24 H24B 113.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 109.5 . . ? C20 C25 C24 103.7(5) . . ? C20 C25 H25A 108.6 . . ? C24 C25 H25A 112.6 . . ? C20 C25 H25B 109.7 . . ? C24 C25 H25B 112.6 . . ? H25A C25 H25B 109.5 . . ? C27 C26 C23 114.9(6) . . ? C27 C26 C28 108.5(6) . . ? C23 C26 C28 113.7(6) . . ? C27 C26 C20 114.8(6) . . ? C23 C26 C20 93.1(5) . . ? C28 C26 C20 111.4(6) . . ? C26 C27 H27A 109.9 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.1 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.4 . . ? C26 C28 H28C 109.3 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.452 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.123