Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author ; Shie-Ming Peng Department of Chemistry, National Taiwan University, Taipei 402, Taiwan ; _publ_contact_author_email smpeng@ntu.edu.tw _publ_section_title ; Control of Magnetic Spin States by Various Mixed Anionic Ligands in Trinickel Complexes: Synthesis, Crystal Structures and Physical Properties ; _publ_contact_author_name 'Shie-Ming Peng' loop_ _publ_author_name 'Ming-Yi Huang.' 'Chen-Yu Yeh.' 'Gene-Hsiang Lee.' 'Shie-Ming Peng.' data_ic10780(comp1) _database_code_depnum_ccdc_archive 'CCDC 618763' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 N12 Ni3 O8 S4' _chemical_formula_weight 1347.47 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 24.6279(4) _cell_length_b 29.1485(4) _cell_length_c 15.3707(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11034.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description dark-brown _exptl_crystal_colour block _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5552 _exptl_absorpt_coefficient_mu 1.235 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.609 _exptl_absorpt_correction_T_max 0.792 _exptl_absorpt_process_details ? _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20507 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5489 _reflns_number_gt 4664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0516P)^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 onstr _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 -0.013(12) _refine_ls_number_reflns 5489 _refine_ls_number_parameters 385 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.2500 0.2500 0.39154(4) 0.03476(15) Uani 1 2 d S . . Ni2 Ni 0.2500 0.2500 0.54491(4) 0.02765(11) Uani 1 2 d S . . Ni3 Ni 0.2500 0.2500 0.69790(3) 0.02951(13) Uani 1 2 d S . . S1 S 0.33707(3) 0.19743(4) 0.30429(6) 0.0541(2) Uani 1 1 d . . . S2 S 0.35843(3) 0.26104(2) 0.78344(6) 0.03748(18) Uani 1 1 d . . . O1 O 0.29344(10) 0.20829(10) 0.24565(17) 0.0631(7) Uani 1 1 d . . . O2 O 0.39092(10) 0.21172(11) 0.2789(2) 0.0768(9) Uani 1 1 d . . . O3 O 0.39446(9) 0.22391(7) 0.80540(17) 0.0473(6) Uani 1 1 d . . . O4 O 0.31419(9) 0.26987(8) 0.84290(15) 0.0448(5) Uani 1 1 d . . . N1 N 0.21048(10) 0.19341(8) 0.39898(18) 0.0379(6) Uani 1 1 d . . . N2 N 0.23308(9) 0.18686(7) 0.54537(18) 0.0301(5) Uani 1 1 d . . . N3 N 0.25559(9) 0.18455(8) 0.69233(18) 0.0325(5) Uani 1 1 d . . . N4 N 0.31816(10) 0.21861(9) 0.39749(18) 0.0394(6) Uani 1 1 d . . . N5 N 0.32780(8) 0.23671(7) 0.54331(19) 0.0314(5) Uani 1 1 d . . . N6 N 0.32843(10) 0.25442(8) 0.69058(18) 0.0318(5) Uani 1 1 d . . . C1 C 0.18371(14) 0.17966(12) 0.3267(2) 0.0483(8) Uani 1 1 d . . . H1A H 0.1890 0.1960 0.2739 0.058 Uiso 1 1 calc R . . C2 C 0.14907(15) 0.14264(13) 0.3274(3) 0.0550(10) Uani 1 1 d . . . H2A H 0.1319 0.1326 0.2754 0.066 Uiso 1 1 calc R . . C3 C 0.13973(14) 0.12044(11) 0.4052(3) 0.0496(9) Uani 1 1 d . . . H3A H 0.1146 0.0958 0.4077 0.060 Uiso 1 1 calc R . . C4 C 0.16676(11) 0.13391(10) 0.4793(2) 0.0414(7) Uani 1 1 d . . . H4A H 0.1603 0.1186 0.5329 0.050 Uiso 1 1 calc R . . C5 C 0.20373(11) 0.17009(9) 0.4753(2) 0.0358(7) Uani 1 1 d . . . C6 C 0.24521(11) 0.16082(9) 0.6168(2) 0.0339(6) Uani 1 1 d . . . C7 C 0.24950(12) 0.11226(9) 0.6177(3) 0.0392(7) Uani 1 1 d . . . H7A H 0.2433 0.0954 0.5658 0.047 Uiso 1 1 calc R . . C8 C 0.26243(14) 0.08977(10) 0.6922(3) 0.0463(8) Uani 1 1 d . . . H8A H 0.2651 0.0573 0.6922 0.056 Uiso 1 1 calc R . . C9 C 0.27182(14) 0.11419(10) 0.7688(2) 0.0471(9) Uani 1 1 d . . . H9A H 0.2798 0.0988 0.8217 0.057 Uiso 1 1 calc R . . C10 C 0.26916(13) 0.16140(10) 0.7651(2) 0.0401(7) Uani 1 1 d . . . H10A H 0.2773 0.1784 0.8162 0.048 Uiso 1 1 calc R . . C11 C 0.33906(14) 0.13731(14) 0.3178(2) 0.0534(10) Uani 1 1 d . . . C12 C 0.36467(19) 0.11063(19) 0.2554(3) 0.0834(14) Uani 1 1 d . . . H12A H 0.3836 0.1246 0.2084 0.100 Uiso 1 1 calc R . . C13 C 0.3622(2) 0.06232(19) 0.2628(4) 0.0916(18) Uani 1 1 d . . . H13A H 0.3784 0.0442 0.2186 0.110 Uiso 1 1 calc R . . C14 C 0.33788(19) 0.04099(16) 0.3299(3) 0.0706(14) Uani 1 1 d . . . C15 C 0.31450(16) 0.06818(14) 0.3927(3) 0.0654(11) Uani 1 1 d . . . H15A H 0.2978 0.0540 0.4415 0.078 Uiso 1 1 calc R . . C16 C 0.31455(14) 0.11580(12) 0.3872(3) 0.0545(9) Uani 1 1 d . . . H16A H 0.2976 0.1335 0.4314 0.065 Uiso 1 1 calc R . . C17 C 0.3364(2) -0.01037(16) 0.3317(4) 0.098(2) Uani 1 1 d . . . H17A H 0.3555 -0.0225 0.2807 0.147 Uiso 1 1 calc R . . H17B H 0.2986 -0.0208 0.3309 0.147 Uiso 1 1 calc R . . H17C H 0.3541 -0.0214 0.3848 0.147 Uiso 1 1 calc R . . C18 C 0.35255(12) 0.22355(10) 0.4675(2) 0.0372(7) Uani 1 1 d . . . C19 C 0.40871(13) 0.21658(10) 0.4647(2) 0.0421(8) Uani 1 1 d . . . H19A H 0.4258 0.2063 0.4129 0.050 Uiso 1 1 calc R . . C20 C 0.43820(11) 0.22484(10) 0.5377(3) 0.0445(8) Uani 1 1 d . . . H20A H 0.4765 0.2211 0.5358 0.053 Uiso 1 1 calc R . . C21 C 0.41430(12) 0.23847(10) 0.6142(2) 0.0424(8) Uani 1 1 d . . . H21A H 0.4356 0.2444 0.6645 0.051 Uiso 1 1 calc R . . C22 C 0.35776(11) 0.24342(9) 0.6161(2) 0.0315(6) Uani 1 1 d . . . C23 C 0.39878(12) 0.31104(10) 0.7743(2) 0.0397(7) Uani 1 1 d . . . C24 C 0.37652(13) 0.35047(10) 0.7385(2) 0.0434(7) Uani 1 1 d . . . H24A H 0.3408 0.3498 0.7151 0.052 Uiso 1 1 calc R . . C25 C 0.40623(13) 0.39080(10) 0.7368(2) 0.0445(8) Uani 1 1 d . . . H25A H 0.3908 0.4175 0.7113 0.053 Uiso 1 1 calc R . . C26 C 0.45738(13) 0.39300(12) 0.7711(2) 0.0491(9) Uani 1 1 d . . . C27 C 0.47971(14) 0.35301(14) 0.8052(3) 0.0706(13) Uani 1 1 d . . . H27A H 0.5156 0.3537 0.8279 0.085 Uiso 1 1 calc R . . C28 C 0.45103(13) 0.31214(13) 0.8069(3) 0.0632(11) Uani 1 1 d . . . H28A H 0.4671 0.2852 0.8301 0.076 Uiso 1 1 calc R . . C29 C 0.48841(16) 0.43785(13) 0.7745(3) 0.0647(12) Uani 1 1 d . . . H29A H 0.4666 0.4622 0.7476 0.097 Uiso 1 1 calc R . . H29B H 0.5227 0.4346 0.7428 0.097 Uiso 1 1 calc R . . H29C H 0.4959 0.4458 0.8352 0.097 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 0.0334(3) 0.0378(3) 0.0331(3) 0.000 0.000 -0.0007(2) Ni2 0.0264(2) 0.0236(2) 0.0330(3) 0.000 0.000 0.00032(18) Ni3 0.0294(3) 0.0260(3) 0.0332(3) 0.000 0.000 0.00087(19) S1 0.0450(4) 0.0782(6) 0.0390(5) -0.0058(4) 0.0095(4) 0.0066(4) S2 0.0356(4) 0.0370(3) 0.0398(5) 0.0051(3) -0.0069(3) -0.0018(3) O1 0.0606(16) 0.0889(19) 0.0397(15) -0.0026(14) 0.0014(12) 0.0153(13) O2 0.0538(15) 0.120(3) 0.056(2) -0.0020(18) 0.0213(14) -0.0054(15) O3 0.0443(12) 0.0435(12) 0.0539(16) 0.0136(11) -0.0131(11) 0.0001(9) O4 0.0438(12) 0.0528(13) 0.0378(14) 0.0003(11) -0.0005(10) -0.0053(10) N1 0.0354(13) 0.0405(14) 0.0379(16) -0.0089(11) 0.0015(11) -0.0023(10) N2 0.0318(11) 0.0268(10) 0.0316(13) -0.0034(11) 0.0002(12) -0.0004(8) N3 0.0300(12) 0.0310(11) 0.0365(15) 0.0043(11) 0.0030(10) 0.0003(10) N4 0.0355(13) 0.0468(14) 0.0358(16) -0.0007(12) 0.0069(11) 0.0058(11) N5 0.0284(10) 0.0282(10) 0.0377(14) 0.0021(12) 0.0014(12) 0.0000(8) N6 0.0321(12) 0.0290(12) 0.0343(15) 0.0014(10) -0.0036(11) -0.0005(9) C1 0.0485(18) 0.054(2) 0.042(2) -0.0133(16) -0.0001(15) -0.0002(16) C2 0.053(2) 0.050(2) 0.063(3) -0.0226(18) -0.0083(18) -0.0055(16) C3 0.0415(17) 0.0414(17) 0.066(3) -0.0216(17) -0.0016(17) -0.0045(14) C4 0.0396(16) 0.0323(14) 0.052(2) -0.0066(14) 0.0032(15) -0.0023(13) C5 0.0323(14) 0.0314(14) 0.044(2) -0.0087(13) 0.0031(14) 0.0030(11) C6 0.0299(14) 0.0300(13) 0.0417(18) 0.0024(14) 0.0082(12) 0.0008(11) C7 0.0407(15) 0.0253(13) 0.052(2) -0.0024(14) 0.0076(13) 0.0014(12) C8 0.0517(19) 0.0272(15) 0.060(2) 0.0069(15) 0.0071(17) 0.0025(13) C9 0.0497(18) 0.0354(16) 0.056(2) 0.0174(15) 0.0053(16) 0.0025(14) C10 0.0409(16) 0.0357(15) 0.044(2) 0.0048(13) 0.0057(14) 0.0028(13) C11 0.0416(17) 0.071(2) 0.047(2) -0.0232(18) 0.0000(15) 0.0154(16) C12 0.076(3) 0.113(4) 0.061(3) -0.030(3) 0.006(2) 0.034(3) C13 0.089(3) 0.102(4) 0.085(4) -0.058(3) -0.016(3) 0.053(3) C14 0.074(3) 0.072(3) 0.066(3) -0.035(2) -0.028(2) 0.040(2) C15 0.065(2) 0.062(2) 0.070(3) -0.024(2) -0.015(2) 0.022(2) C16 0.052(2) 0.053(2) 0.058(3) -0.0197(18) 0.0022(18) 0.0194(17) C17 0.118(4) 0.077(3) 0.099(4) -0.053(3) -0.057(3) 0.055(3) C18 0.0340(15) 0.0345(14) 0.0431(19) 0.0012(14) 0.0056(14) 0.0019(12) C19 0.0382(16) 0.0372(16) 0.051(2) 0.0042(15) 0.0059(15) 0.0067(13) C20 0.0274(13) 0.0449(16) 0.061(2) 0.0066(17) 0.0041(17) 0.0063(12) C21 0.0334(15) 0.0418(16) 0.052(2) 0.0027(16) -0.0045(15) 0.0026(12) C22 0.0316(13) 0.0271(13) 0.0358(17) 0.0060(12) -0.0003(13) 0.0008(11) C23 0.0377(14) 0.0398(16) 0.042(2) 0.0008(13) -0.0082(13) -0.0010(12) C24 0.0400(16) 0.0370(15) 0.053(2) -0.0048(15) -0.0092(15) 0.0021(13) C25 0.0453(18) 0.0323(15) 0.056(2) -0.0013(15) -0.0004(16) 0.0011(13) C26 0.0436(17) 0.0512(18) 0.053(2) -0.0004(15) 0.0003(16) -0.0165(14) C27 0.0421(17) 0.069(2) 0.101(4) 0.031(2) -0.026(2) -0.0169(17) C28 0.0420(17) 0.062(2) 0.086(3) 0.022(2) -0.023(2) -0.0071(16) C29 0.058(2) 0.060(2) 0.076(3) 0.009(2) -0.009(2) -0.0246(18) _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 N4 1.914(2) . ? Ni1 N4 1.914(2) 14 ? Ni1 N1 1.919(2) 14 ? Ni1 N1 1.919(2) . ? Ni1 Ni2 2.3573(8) . ? Ni2 N2 1.887(2) 14 ? Ni2 N2 1.887(2) . ? Ni2 N5 1.955(2) . ? Ni2 N5 1.955(2) 14 ? Ni2 Ni3 2.3516(8) . ? Ni3 N3 1.915(2) 14 ? Ni3 N3 1.915(2) . ? Ni3 N6 1.939(2) . ? Ni3 N6 1.939(2) 14 ? S1 O1 1.438(3) . ? S1 O2 1.444(3) . ? S1 N4 1.628(3) . ? S1 C11 1.765(4) . ? S2 O3 1.440(2) . ? S2 O4 1.445(2) . ? S2 N6 1.619(3) . ? S2 C23 1.770(3) . ? N1 C1 1.353(4) . ? N1 C5 1.365(4) . ? N2 C6 1.367(4) . ? N2 C5 1.387(4) . ? N3 C10 1.349(4) . ? N3 C6 1.376(4) . ? N4 C18 1.377(4) . ? N5 C22 1.354(4) . ? N5 C18 1.370(4) . ? N6 C22 1.391(4) . ? C1 C2 1.376(5) . ? C1 H1A 0.9500 . ? C2 C3 1.379(6) . ? C2 H2A 0.9500 . ? C3 C4 1.376(5) . ? C3 H3A 0.9500 . ? C4 C5 1.395(4) . ? C4 H4A 0.9500 . ? C6 C7 1.420(4) . ? C7 C8 1.357(5) . ? C7 H7A 0.9500 . ? C8 C9 1.395(5) . ? C8 H8A 0.9500 . ? C9 C10 1.379(4) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C16 1.376(6) . ? C11 C12 1.387(5) . ? C12 C13 1.414(8) . ? C12 H12A 0.9500 . ? C13 C14 1.344(8) . ? C13 H13A 0.9500 . ? C14 C15 1.376(6) . ? C14 C17 1.498(6) . ? C15 C16 1.391(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.399(4) . ? C19 C20 1.359(5) . ? C19 H19A 0.9500 . ? C20 C21 1.373(5) . ? C20 H20A 0.9500 . ? C21 C22 1.400(4) . ? C21 H21A 0.9500 . ? C23 C28 1.381(4) . ? C23 C24 1.387(4) . ? C24 C25 1.385(4) . ? C24 H24A 0.9500 . ? C25 C26 1.367(5) . ? C25 H25A 0.9500 . ? C26 C27 1.391(5) . ? C26 C29 1.515(5) . ? C27 C28 1.385(5) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ni1 N4 174.52(17) . 14 ? N4 Ni1 N1 87.89(10) . 14 ? N4 Ni1 N1 91.78(10) 14 14 ? N4 Ni1 N1 91.78(10) . . ? N4 Ni1 N1 87.89(10) 14 . ? N1 Ni1 N1 173.17(17) 14 . ? N4 Ni1 Ni2 87.26(8) . . ? N4 Ni1 Ni2 87.26(8) 14 . ? N1 Ni1 Ni2 86.58(9) 14 . ? N1 Ni1 Ni2 86.58(9) . . ? N2 Ni2 N2 179.57(17) 14 . ? N2 Ni2 N5 88.67(9) 14 . ? N2 Ni2 N5 91.33(9) . . ? N2 Ni2 N5 91.33(9) 14 14 ? N2 Ni2 N5 88.67(9) . 14 ? N5 Ni2 N5 178.56(17) . 14 ? N2 Ni2 Ni3 89.79(9) 14 . ? N2 Ni2 Ni3 89.79(9) . . ? N5 Ni2 Ni3 90.72(9) . . ? N5 Ni2 Ni3 90.72(9) 14 . ? N2 Ni2 Ni1 90.21(9) 14 . ? N2 Ni2 Ni1 90.21(9) . . ? N5 Ni2 Ni1 89.28(9) . . ? N5 Ni2 Ni1 89.28(9) 14 . ? Ni3 Ni2 Ni1 180.0 . . ? N3 Ni3 N3 174.87(17) 14 . ? N3 Ni3 N6 90.16(9) 14 . ? N3 Ni3 N6 89.54(9) . . ? N3 Ni3 N6 89.54(9) 14 14 ? N3 Ni3 N6 90.16(9) . 14 ? N6 Ni3 N6 173.35(16) . 14 ? N3 Ni3 Ni2 87.44(8) 14 . ? N3 Ni3 Ni2 87.44(8) . . ? N6 Ni3 Ni2 86.67(8) . . ? N6 Ni3 Ni2 86.67(8) 14 . ? O1 S1 O2 116.96(18) . . ? O1 S1 N4 104.74(15) . . ? O2 S1 N4 113.03(17) . . ? O1 S1 C11 108.26(17) . . ? O2 S1 C11 107.02(18) . . ? N4 S1 C11 106.30(16) . . ? O3 S2 O4 116.77(15) . . ? O3 S2 N6 113.48(14) . . ? O4 S2 N6 103.57(13) . . ? O3 S2 C23 106.96(13) . . ? O4 S2 C23 109.06(14) . . ? N6 S2 C23 106.53(14) . . ? C1 N1 C5 119.9(3) . . ? C1 N1 Ni1 116.9(2) . . ? C5 N1 Ni1 122.7(2) . . ? C6 N2 C5 122.8(2) . . ? C6 N2 Ni2 119.7(2) . . ? C5 N2 Ni2 117.13(19) . . ? C10 N3 C6 119.7(3) . . ? C10 N3 Ni3 118.6(2) . . ? C6 N3 Ni3 121.7(2) . . ? C18 N4 S1 123.5(2) . . ? C18 N4 Ni1 121.8(2) . . ? S1 N4 Ni1 112.96(15) . . ? C22 N5 C18 120.0(2) . . ? C22 N5 Ni2 119.7(2) . . ? C18 N5 Ni2 120.2(2) . . ? C22 N6 S2 121.1(2) . . ? C22 N6 Ni3 123.3(2) . . ? S2 N6 Ni3 114.29(15) . . ? N1 C1 C2 121.8(4) . . ? N1 C1 H1A 119.1 . . ? C2 C1 H1A 119.1 . . ? C1 C2 C3 118.6(3) . . ? C1 C2 H2A 120.7 . . ? C3 C2 H2A 120.7 . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N1 C5 N2 115.4(2) . . ? N1 C5 C4 119.6(3) . . ? N2 C5 C4 124.9(3) . . ? N2 C6 N3 116.0(2) . . ? N2 C6 C7 125.3(3) . . ? N3 C6 C7 118.6(3) . . ? C8 C7 C6 120.5(3) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C7 C8 C9 120.3(3) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C10 C9 C8 117.8(3) . . ? C10 C9 H9A 121.1 . . ? C8 C9 H9A 121.1 . . ? N3 C10 C9 123.0(3) . . ? N3 C10 H10A 118.5 . . ? C9 C10 H10A 118.5 . . ? C16 C11 C12 118.7(4) . . ? C16 C11 S1 122.1(3) . . ? C12 C11 S1 119.2(4) . . ? C11 C12 C13 118.9(5) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C14 C13 C12 122.8(4) . . ? C14 C13 H13A 118.6 . . ? C12 C13 H13A 118.6 . . ? C13 C14 C15 117.3(5) . . ? C13 C14 C17 119.2(4) . . ? C15 C14 C17 123.5(5) . . ? C14 C15 C16 122.1(5) . . ? C14 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? C11 C16 C15 120.2(4) . . ? C11 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 N4 114.9(2) . . ? N5 C18 C19 120.5(3) . . ? N4 C18 C19 124.7(3) . . ? C20 C19 C18 118.5(3) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? C19 C20 C21 122.0(3) . . ? C19 C20 H20A 119.0 . . ? C21 C20 H20A 119.0 . . ? C20 C21 C22 118.3(3) . . ? C20 C21 H21A 120.9 . . ? C22 C21 H21A 120.9 . . ? N5 C22 N6 115.5(2) . . ? N5 C22 C21 120.7(3) . . ? N6 C22 C21 123.9(3) . . ? C28 C23 C24 119.5(3) . . ? C28 C23 S2 120.9(2) . . ? C24 C23 S2 119.5(2) . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C26 C25 C24 121.3(3) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C25 C26 C27 118.0(3) . . ? C25 C26 C29 121.2(3) . . ? C27 C26 C29 120.7(3) . . ? C28 C27 C26 121.7(3) . . ? C28 C27 H27A 119.1 . . ? C26 C27 H27A 119.1 . . ? C23 C28 C27 119.2(3) . . ? C23 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.427 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.083 #===END data_ic11202(comp2) _database_code_depnum_ccdc_archive 'CCDC 618764' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.50 H39 Cl3 N12 Ni3 O9 S4' _chemical_formula_weight 1188.51 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' 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 15.8040(7) _cell_length_b 17.4684(8) _cell_length_c 19.0282(9) _cell_angle_alpha 70.131(1) _cell_angle_beta 67.748(1) _cell_angle_gamma 87.126(1) _cell_volume 4553.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6134 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.40 _exptl_crystal_description plate _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2428 _exptl_absorpt_coefficient_mu 1.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3906 _exptl_absorpt_correction_T_max 0.7332 _exptl_absorpt_process_details ? _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 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59043 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 27.50 _reflns_number_total 20856 _reflns_number_gt 17724 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0559P)^2^+19.2394P] 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 20856 _refine_ls_number_parameters 1199 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1633 _refine_ls_wR_factor_gt 0.1559 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.135 _refine_ls_shift/su_max 0.011 _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 0.00795(4) 0.33851(4) 0.17140(4) 0.01436(13) Uani 1 1 d . . . Ni2 Ni 0.10693(4) 0.27094(4) 0.23376(4) 0.01235(13) Uani 1 1 d . . . Ni3 Ni 0.20900(4) 0.20122(4) 0.29495(4) 0.01402(13) Uani 1 1 d . . . S1 S -0.07084(10) 0.47990(8) 0.21456(9) 0.0253(3) Uani 1 1 d . . . S2 S 0.08388(8) 0.12824(8) 0.48779(7) 0.0187(2) Uani 1 1 d . . . S3 S -0.02492(9) 0.26485(8) 0.06200(8) 0.0204(3) Uani 1 1 d . . . S4 S 0.40493(8) 0.23415(9) 0.14916(8) 0.0217(3) Uani 1 1 d . . . O1 O -0.0821(3) 0.4766(2) 0.1444(2) 0.0280(9) Uani 1 1 d . . . O2 O -0.1519(3) 0.4881(3) 0.2786(3) 0.0447(12) Uani 1 1 d . . . O3 O 0.0910(3) 0.1583(3) 0.5477(2) 0.0315(9) Uani 1 1 d . . . O4 O 0.1434(2) 0.0645(2) 0.4734(2) 0.0232(8) Uani 1 1 d . . . O5 O -0.1010(3) 0.3090(3) 0.0917(3) 0.0361(11) Uani 1 1 d . . . O6 O 0.0204(3) 0.2865(2) -0.0241(2) 0.0290(9) Uani 1 1 d . . . O7 O 0.4228(2) 0.2522(2) 0.2110(2) 0.0257(8) Uani 1 1 d . . . O8 O 0.4511(3) 0.1682(3) 0.1273(3) 0.0422(12) Uani 1 1 d . . . O17 O 0.2949(2) 0.1320(2) 0.3425(2) 0.0203(7) Uani 1 1 d . . . H17 H 0.2628 0.1041 0.3877 0.030 Uiso 1 1 d R . . H17' H 0.3412 0.1569 0.3338 0.030 Uiso 1 1 d R . . N1 N 0.1123(3) 0.4156(2) 0.0969(2) 0.0161(8) Uani 1 1 d . . . N2 N 0.1820(3) 0.3695(2) 0.1897(2) 0.0162(8) Uani 1 1 d . . . N3 N 0.2413(3) 0.3196(3) 0.2881(2) 0.0163(8) Uani 1 1 d . . . N4 N -0.0210(3) 0.3982(2) 0.2435(2) 0.0175(8) Uani 1 1 d . . . N5 N 0.0381(3) 0.3014(3) 0.3272(2) 0.0164(8) Uani 1 1 d . . . N6 N 0.1007(3) 0.1974(3) 0.4020(2) 0.0168(8) Uani 1 1 d . . . N7 N -0.0855(3) 0.2558(2) 0.2544(2) 0.0157(8) Uani 1 1 d . . . N8 N 0.0278(3) 0.1744(2) 0.2778(2) 0.0150(8) Uani 1 1 d . . . N9 N 0.1500(3) 0.0996(2) 0.2874(2) 0.0164(8) Uani 1 1 d . . . N10 N 0.0444(3) 0.2729(2) 0.1047(2) 0.0159(8) Uani 1 1 d . . . N11 N 0.1724(3) 0.2426(2) 0.1377(2) 0.0143(8) Uani 1 1 d . . . N12 N 0.2957(3) 0.2237(2) 0.1771(2) 0.0152(8) Uani 1 1 d . . . C1 C 0.1130(4) 0.4639(3) 0.0240(3) 0.0197(10) Uani 1 1 d . . . H1A H 0.0651 0.4544 0.0085 0.024 Uiso 1 1 calc R . . C2 C 0.1800(4) 0.5257(3) -0.0282(3) 0.0247(11) Uani 1 1 d . . . H2A H 0.1777 0.5597 -0.0783 0.030 Uiso 1 1 calc R . . C3 C 0.2516(4) 0.5381(3) -0.0066(3) 0.0270(12) Uani 1 1 d . . . H3A H 0.2985 0.5813 -0.0414 0.032 Uiso 1 1 calc R . . C4 C 0.2538(4) 0.4868(3) 0.0658(3) 0.0250(11) Uani 1 1 d . . . H4A H 0.3036 0.4934 0.0801 0.030 Uiso 1 1 calc R . . C5 C 0.1834(3) 0.4254(3) 0.1180(3) 0.0153(9) Uani 1 1 d . . . C6 C 0.2225(3) 0.3856(3) 0.2366(3) 0.0183(10) Uani 1 1 d . . . C7 C 0.2357(4) 0.4643(3) 0.2375(4) 0.0275(12) Uani 1 1 d . . . H7A H 0.2225 0.5107 0.2005 0.033 Uiso 1 1 calc R . . C8 C 0.2677(5) 0.4735(4) 0.2917(4) 0.0387(16) Uani 1 1 d . . . H8A H 0.2769 0.5264 0.2928 0.046 Uiso 1 1 calc R . . C9 C 0.2865(4) 0.4055(4) 0.3449(4) 0.0346(14) Uani 1 1 d . . . H9A H 0.3090 0.4108 0.3829 0.041 Uiso 1 1 calc R . . C10 C 0.2721(3) 0.3297(3) 0.3420(3) 0.0229(11) Uani 1 1 d . . . H10A H 0.2842 0.2828 0.3792 0.027 Uiso 1 1 calc R . . C11 C 0.0096(5) 0.5627(4) 0.1827(5) 0.0446(18) Uani 1 1 d . . . H11A H -0.0154 0.6138 0.1610 0.067 Uiso 1 1 calc R . . H11B H 0.0663 0.5569 0.1405 0.067 Uiso 1 1 calc R . . H11C H 0.0227 0.5636 0.2288 0.067 Uiso 1 1 calc R . . C12 C -0.0147(4) 0.3662(3) 0.3180(3) 0.0215(11) Uani 1 1 d . . . C13 C -0.0597(5) 0.3933(4) 0.3829(4) 0.0413(17) Uani 1 1 d . . . H13A H -0.0966 0.4379 0.3769 0.050 Uiso 1 1 calc R . . C14 C -0.0503(5) 0.3550(5) 0.4552(4) 0.0459(19) Uani 1 1 d . . . H14A H -0.0812 0.3730 0.4996 0.055 Uiso 1 1 calc R . . C15 C 0.0034(4) 0.2909(4) 0.4640(3) 0.0326(14) Uani 1 1 d . . . H15A H 0.0111 0.2656 0.5137 0.039 Uiso 1 1 calc R . . C16 C 0.0466(3) 0.2632(3) 0.3995(3) 0.0175(10) Uani 1 1 d . . . C17 C -0.0295(3) 0.0860(4) 0.5251(4) 0.0291(12) Uani 1 1 d . . . H17A H -0.0419 0.0393 0.5753 0.044 Uiso 1 1 calc R . . H17B H -0.0383 0.0677 0.4848 0.044 Uiso 1 1 calc R . . H17C H -0.0718 0.1274 0.5361 0.044 Uiso 1 1 calc R . . C18 C -0.1744(3) 0.2719(3) 0.2752(3) 0.0234(11) Uani 1 1 d . . . H18A H -0.1884 0.3242 0.2477 0.028 Uiso 1 1 calc R . . C19 C -0.2448(4) 0.2164(4) 0.3339(4) 0.0291(13) Uani 1 1 d . . . H19A H -0.3065 0.2301 0.3475 0.035 Uiso 1 1 calc R . . C20 C -0.2241(4) 0.1388(3) 0.3738(3) 0.0249(11) Uani 1 1 d . . . H20A H -0.2719 0.0983 0.4139 0.030 Uiso 1 1 calc R . . C21 C -0.1339(3) 0.1221(3) 0.3542(3) 0.0200(10) Uani 1 1 d . . . H21A H -0.1190 0.0698 0.3809 0.024 Uiso 1 1 calc R . . C22 C -0.0635(3) 0.1825(3) 0.2946(3) 0.0151(9) Uani 1 1 d . . . C23 C 0.0675(3) 0.1019(3) 0.2804(3) 0.0158(9) Uani 1 1 d . . . C24 C 0.0325(3) 0.0375(3) 0.2676(3) 0.0199(10) Uani 1 1 d . . . H24A H -0.0262 0.0387 0.2646 0.024 Uiso 1 1 calc R . . C25 C 0.0837(4) -0.0269(3) 0.2596(3) 0.0239(11) Uani 1 1 d . . . H25A H 0.0609 -0.0707 0.2508 0.029 Uiso 1 1 calc R . . C26 C 0.1692(4) -0.0278(3) 0.2645(3) 0.0213(10) Uani 1 1 d . . . H26A H 0.2063 -0.0714 0.2585 0.026 Uiso 1 1 calc R . . C27 C 0.1987(3) 0.0361(3) 0.2783(3) 0.0195(10) Uani 1 1 d . . . H27A H 0.2572 0.0354 0.2816 0.023 Uiso 1 1 calc R . . C28 C -0.0638(4) 0.1606(4) 0.1019(4) 0.0332(14) Uani 1 1 d . . . H28A H -0.1072 0.1517 0.0793 0.050 Uiso 1 1 calc R . . H28B H -0.0945 0.1435 0.1610 0.050 Uiso 1 1 calc R . . H28C H -0.0114 0.1284 0.0878 0.050 Uiso 1 1 calc R . . C29 C 0.1288(3) 0.2417(3) 0.0879(3) 0.0163(9) Uani 1 1 d . . . C30 C 0.1703(4) 0.2109(3) 0.0252(3) 0.0239(11) Uani 1 1 d . . . H30A H 0.1401 0.2097 -0.0092 0.029 Uiso 1 1 calc R . . C31 C 0.2554(4) 0.1825(4) 0.0138(3) 0.0268(12) Uani 1 1 d . . . H31A H 0.2835 0.1607 -0.0283 0.032 Uiso 1 1 calc R . . C32 C 0.3005(4) 0.1850(3) 0.0626(3) 0.0212(10) Uani 1 1 d . . . H32A H 0.3594 0.1655 0.0543 0.025 Uiso 1 1 calc R . . C33 C 0.2583(3) 0.2168(3) 0.1241(3) 0.0167(9) Uani 1 1 d . . . C34 C 0.4422(5) 0.3227(5) 0.0613(4) 0.0445(18) Uani 1 1 d . . . H34A H 0.5081 0.3362 0.0439 0.067 Uiso 1 1 calc R . . H34B H 0.4086 0.3684 0.0733 0.067 Uiso 1 1 calc R . . H34C H 0.4305 0.3127 0.0180 0.067 Uiso 1 1 calc R . . Ni4 Ni 0.49156(4) 0.76539(4) 0.26642(4) 0.01587(14) Uani 1 1 d . . . Ni5 Ni 0.59750(4) 0.81399(4) 0.30472(4) 0.01352(13) Uani 1 1 d . . . Ni6 Ni 0.70591(4) 0.86577(4) 0.34128(4) 0.01476(13) Uani 1 1 d . . . S5 S 0.40275(11) 0.59717(8) 0.36940(9) 0.0297(3) Uani 1 1 d . . . S6 S 0.58593(8) 0.86894(8) 0.52307(7) 0.0180(2) Uani 1 1 d . . . S7 S 0.45636(9) 0.88612(8) 0.12874(8) 0.0212(3) Uani 1 1 d . . . S8 S 0.89968(8) 0.89249(8) 0.19163(8) 0.0213(3) Uani 1 1 d . . . O9 O 0.4045(3) 0.6150(3) 0.2899(3) 0.0433(12) Uani 1 1 d . . . O10 O 0.3138(3) 0.5768(3) 0.4339(3) 0.0486(13) Uani 1 1 d . . . O11 O 0.6475(2) 0.9428(2) 0.4838(2) 0.0224(8) Uani 1 1 d . . . O12 O 0.5940(3) 0.8135(3) 0.5962(2) 0.0309(9) Uani 1 1 d . . . O13 O 0.3810(3) 0.8240(3) 0.1768(3) 0.0331(10) Uani 1 1 d . . . O14 O 0.4984(3) 0.8989(2) 0.0433(2) 0.0286(9) Uani 1 1 d . . . O15 O 0.9205(2) 0.8508(3) 0.2619(2) 0.0282(9) Uani 1 1 d . . . O16 O 0.9438(3) 0.9734(3) 0.1454(3) 0.0435(12) Uani 1 1 d . . . O18 O 0.7969(2) 0.9203(2) 0.3661(2) 0.0208(7) Uani 1 1 d . . . H18 H 0.7686 0.9335 0.4047 0.031 Uiso 1 1 d R . . H18' H 0.8435 0.8984 0.3637 0.031 Uiso 1 1 d R . . N13 N 0.4037(3) 0.8221(2) 0.3270(2) 0.0173(8) Uani 1 1 d . . . N14 N 0.5231(3) 0.9003(2) 0.3193(2) 0.0148(8) Uani 1 1 d . . . N15 N 0.6502(3) 0.9759(2) 0.3013(2) 0.0150(8) Uani 1 1 d . . . N16 N 0.4593(3) 0.6746(3) 0.3648(3) 0.0194(9) Uani 1 1 d . . . N17 N 0.5273(3) 0.7459(2) 0.4164(3) 0.0176(8) Uani 1 1 d . . . N18 N 0.5982(3) 0.8286(3) 0.4565(2) 0.0172(8) Uani 1 1 d . . . N19 N 0.5902(3) 0.7099(3) 0.2130(3) 0.0194(9) Uani 1 1 d . . . N20 N 0.6677(3) 0.7264(2) 0.2903(3) 0.0179(8) Uani 1 1 d . . . N21 N 0.7373(3) 0.7451(3) 0.3708(2) 0.0170(8) Uani 1 1 d . . . N22 N 0.5293(3) 0.8611(3) 0.1729(2) 0.0168(8) Uani 1 1 d . . . N23 N 0.6612(3) 0.8824(2) 0.1921(2) 0.0161(8) Uani 1 1 d . . . N24 N 0.7897(3) 0.8875(3) 0.2214(3) 0.0190(9) Uani 1 1 d . . . C35 C 0.3140(3) 0.7963(3) 0.3582(3) 0.0232(11) Uani 1 1 d . . . H35A H 0.2964 0.7515 0.3475 0.028 Uiso 1 1 calc R . . C36 C 0.2469(4) 0.8313(4) 0.4044(4) 0.0292(13) Uani 1 1 d . . . H36A H 0.1843 0.8108 0.4262 0.035 Uiso 1 1 calc R . . C37 C 0.2730(4) 0.8978(4) 0.4187(3) 0.0264(12) Uani 1 1 d . . . H37A H 0.2278 0.9245 0.4493 0.032 Uiso 1 1 calc R . . C38 C 0.3637(3) 0.9245(3) 0.3885(3) 0.0209(10) Uani 1 1 d . . . H38A H 0.3816 0.9700 0.3980 0.025 Uiso 1 1 calc R . . C39 C 0.4310(3) 0.8847(3) 0.3434(3) 0.0173(10) Uani 1 1 d . . . C40 C 0.5668(3) 0.9766(3) 0.2970(3) 0.0162(9) Uani 1 1 d . . . C41 C 0.5324(3) 1.0505(3) 0.2647(3) 0.0206(10) Uani 1 1 d . . . H41A H 0.4729 1.0505 0.2636 0.025 Uiso 1 1 calc R . . C42 C 0.5861(4) 1.1228(3) 0.2349(3) 0.0215(11) Uani 1 1 d . . . H42A H 0.5638 1.1732 0.2133 0.026 Uiso 1 1 calc R . . C43 C 0.6738(4) 1.1215(3) 0.2365(3) 0.0236(11) Uani 1 1 d . . . H43A H 0.7128 1.1705 0.2150 0.028 Uiso 1 1 calc R . . C44 C 0.7017(3) 1.0469(3) 0.2705(3) 0.0194(10) Uani 1 1 d . . . H44A H 0.7611 1.0458 0.2722 0.023 Uiso 1 1 calc R . . C45 C 0.4700(6) 0.5154(4) 0.3885(7) 0.068(3) Uani 1 1 d . . . H45A H 0.4415 0.4662 0.3897 0.102 Uiso 1 1 calc R . . H45B H 0.4743 0.5054 0.4409 0.102 Uiso 1 1 calc R . . H45C H 0.5316 0.5289 0.3457 0.102 Uiso 1 1 calc R . . C46 C 0.4652(3) 0.6835(3) 0.4325(3) 0.0187(10) Uani 1 1 d . . . C47 C 0.4120(4) 0.6358(3) 0.5118(3) 0.0276(12) Uani 1 1 d . . . H47A H 0.3670 0.5946 0.5227 0.033 Uiso 1 1 calc R . . C48 C 0.4253(4) 0.6490(3) 0.5742(3) 0.0290(12) Uani 1 1 d . . . H48A H 0.3901 0.6158 0.6284 0.035 Uiso 1 1 calc R . . C49 C 0.4889(4) 0.7097(3) 0.5591(3) 0.0241(11) Uani 1 1 d . . . H49A H 0.4994 0.7170 0.6025 0.029 Uiso 1 1 calc R . . C50 C 0.5379(3) 0.7606(3) 0.4790(3) 0.0165(9) Uani 1 1 d . . . C51 C 0.4731(4) 0.8984(4) 0.5513(3) 0.0267(12) Uani 1 1 d . . . H51A H 0.4628 0.9263 0.5903 0.040 Uiso 1 1 calc R . . H51B H 0.4294 0.8497 0.5762 0.040 Uiso 1 1 calc R . . H51C H 0.4642 0.9354 0.5033 0.040 Uiso 1 1 calc R . . C52 C 0.5833(4) 0.6818(3) 0.1572(3) 0.0266(12) Uani 1 1 d . . . H52A H 0.5322 0.6940 0.1419 0.032 Uiso 1 1 calc R . . C53 C 0.6471(4) 0.6365(4) 0.1221(4) 0.0298(13) Uani 1 1 d . . . H53A H 0.6391 0.6156 0.0848 0.036 Uiso 1 1 calc R . . C54 C 0.7241(4) 0.6212(4) 0.1416(4) 0.0315(13) Uani 1 1 d . . . H54A H 0.7696 0.5903 0.1172 0.038 Uiso 1 1 calc R . . C55 C 0.7337(4) 0.6511(3) 0.1961(3) 0.0243(11) Uani 1 1 d . . . H55A H 0.7872 0.6426 0.2082 0.029 Uiso 1 1 calc R . . C56 C 0.6642(3) 0.6946(3) 0.2346(3) 0.0189(10) Uani 1 1 d . . . C57 C 0.7161(3) 0.6941(3) 0.3393(3) 0.0166(9) Uani 1 1 d . . . C58 C 0.7368(4) 0.6121(3) 0.3617(3) 0.0207(10) Uani 1 1 d . . . H58A H 0.7191 0.5754 0.3415 0.025 Uiso 1 1 calc R . . C59 C 0.7829(4) 0.5855(3) 0.4132(3) 0.0248(11) Uani 1 1 d . . . H59A H 0.7981 0.5305 0.4279 0.030 Uiso 1 1 calc R . . C60 C 0.8072(4) 0.6391(4) 0.4435(3) 0.0275(12) Uani 1 1 d . . . H60A H 0.8406 0.6224 0.4777 0.033 Uiso 1 1 calc R . . C61 C 0.7812(4) 0.7170(3) 0.4221(3) 0.0219(11) Uani 1 1 d . . . H61A H 0.7948 0.7534 0.4446 0.026 Uiso 1 1 calc R . . C62 C 0.4179(4) 0.9795(4) 0.1398(3) 0.0296(13) Uani 1 1 d . . . H62A H 0.3736 0.9975 0.1142 0.044 Uiso 1 1 calc R . . H62B H 0.4703 1.0209 0.1140 0.044 Uiso 1 1 calc R . . H62C H 0.3884 0.9720 0.1975 0.044 Uiso 1 1 calc R . . C63 C 0.6130(3) 0.9055(3) 0.1428(3) 0.0177(10) Uani 1 1 d . . . C64 C 0.6498(4) 0.9679(3) 0.0675(3) 0.0238(11) Uani 1 1 d . . . H64A H 0.6153 0.9858 0.0344 0.029 Uiso 1 1 calc R . . C65 C 0.7379(4) 1.0032(3) 0.0420(3) 0.0273(12) Uani 1 1 d . . . H65A H 0.7634 1.0463 -0.0087 0.033 Uiso 1 1 calc R . . C66 C 0.7892(4) 0.9766(3) 0.0894(3) 0.0261(12) Uani 1 1 d . . . H66A H 0.8506 0.9992 0.0704 0.031 Uiso 1 1 calc R . . C67 C 0.7491(3) 0.9158(3) 0.1658(3) 0.0179(10) Uani 1 1 d . . . C68 C 0.9365(5) 0.8341(5) 0.1278(5) 0.052(2) Uani 1 1 d . . . H68A H 1.0035 0.8346 0.1076 0.077 Uiso 1 1 calc R . . H68B H 0.9175 0.8574 0.0820 0.077 Uiso 1 1 calc R . . H68C H 0.9089 0.7777 0.1582 0.077 Uiso 1 1 calc R . . C69 C 0.6679(8) 0.2349(5) -0.0488(7) 0.076(3) Uani 1 1 d . . . H69A H 0.6093 0.2084 -0.0037 0.092 Uiso 1 1 calc R . . H69B H 0.6893 0.2001 -0.0827 0.092 Uiso 1 1 calc R . . Cl1 Cl 0.64986(17) 0.33252(14) -0.10791(15) 0.0691(6) Uani 1 1 d . . . Cl2 Cl 0.7483(4) 0.2438(2) -0.0104(4) 0.178(2) Uani 1 1 d . . . C70 C 0.4987(8) 0.5791(11) 0.7913(9) 0.153(8) Uani 1 1 d . . . H70A H 0.5406 0.6287 0.7719 0.183 Uiso 1 1 calc R . . H70B H 0.5258 0.5485 0.7539 0.183 Uiso 1 1 calc R . . Cl3 Cl 0.3934(3) 0.6088(3) 0.78706(16) 0.167(2) Uani 1 1 d . . . Cl4 Cl 0.49244(18) 0.5183(2) 0.8879(3) 0.1151(13) Uani 1 1 d . . . C71 C -0.0461(7) 0.2913(5) 0.6961(7) 0.105(4) Uiso 1 1 d D . . H71A H 0.0010 0.2687 0.6586 0.127 Uiso 0.80 1 calc PR A 1 H71B H -0.0290 0.2844 0.7428 0.127 Uiso 0.80 1 calc PR A 1 H71C H -0.0117 0.3330 0.7020 0.127 Uiso 0.20 1 calc PR A 2 H71D H -0.0028 0.2534 0.6761 0.127 Uiso 0.20 1 calc PR A 2 Cl5 Cl -0.0513(3) 0.3975(2) 0.6454(2) 0.0915(10) Uiso 0.80 1 d PD B 1 Cl6 Cl -0.1516(4) 0.2403(4) 0.7291(4) 0.165(2) Uiso 0.80 1 d PD B 1 Cl5' Cl -0.0997(16) 0.3365(15) 0.6310(13) 0.153(8) Uiso 0.20 1 d PD B 2 Cl6' Cl -0.1346(13) 0.2377(14) 0.7891(10) 0.147(8) Uiso 0.20 1 d PD B 2 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 0.0170(3) 0.0146(3) 0.0164(3) -0.0076(2) -0.0102(2) 0.0054(2) Ni2 0.0132(3) 0.0126(3) 0.0133(3) -0.0052(2) -0.0068(2) 0.0024(2) Ni3 0.0126(3) 0.0161(3) 0.0134(3) -0.0037(2) -0.0065(2) 0.0025(2) S1 0.0359(7) 0.0241(7) 0.0307(7) -0.0169(6) -0.0238(6) 0.0192(6) S2 0.0158(6) 0.0245(6) 0.0138(6) -0.0016(5) -0.0079(5) 0.0006(5) S3 0.0260(6) 0.0210(6) 0.0252(7) -0.0124(5) -0.0184(5) 0.0079(5) S4 0.0141(6) 0.0317(7) 0.0180(6) -0.0071(5) -0.0063(5) 0.0032(5) O1 0.036(2) 0.030(2) 0.035(2) -0.0180(18) -0.0264(19) 0.0170(18) O2 0.053(3) 0.058(3) 0.043(3) -0.033(2) -0.030(2) 0.044(3) O3 0.047(3) 0.037(2) 0.021(2) -0.0096(18) -0.0245(19) 0.0065(19) O4 0.0161(17) 0.0220(19) 0.0227(19) 0.0018(15) -0.0067(15) 0.0031(14) O5 0.039(2) 0.052(3) 0.045(3) -0.034(2) -0.033(2) 0.030(2) O6 0.041(2) 0.030(2) 0.026(2) -0.0119(18) -0.0229(19) 0.0079(18) O7 0.0145(17) 0.037(2) 0.026(2) -0.0107(18) -0.0089(15) 0.0038(16) O8 0.034(2) 0.062(3) 0.056(3) -0.041(3) -0.029(2) 0.028(2) O17 0.0150(16) 0.0264(19) 0.0184(18) -0.0021(15) -0.0103(14) 0.0015(14) N1 0.021(2) 0.0135(19) 0.018(2) -0.0065(16) -0.0107(17) 0.0041(16) N2 0.018(2) 0.015(2) 0.0134(19) -0.0021(16) -0.0065(16) -0.0017(16) N3 0.0135(19) 0.020(2) 0.017(2) -0.0057(17) -0.0081(16) 0.0008(16) N4 0.023(2) 0.017(2) 0.018(2) -0.0099(17) -0.0116(18) 0.0093(17) N5 0.0150(19) 0.020(2) 0.017(2) -0.0082(17) -0.0079(16) 0.0056(16) N6 0.0141(19) 0.019(2) 0.014(2) -0.0033(17) -0.0042(16) 0.0035(16) N7 0.0142(19) 0.017(2) 0.018(2) -0.0071(17) -0.0078(16) 0.0026(16) N8 0.0133(19) 0.0134(19) 0.018(2) -0.0024(16) -0.0075(16) -0.0009(15) N9 0.017(2) 0.0141(19) 0.016(2) -0.0018(16) -0.0071(16) 0.0018(16) N10 0.021(2) 0.019(2) 0.018(2) -0.0118(17) -0.0136(17) 0.0066(17) N11 0.0171(19) 0.0121(19) 0.0119(19) -0.0040(15) -0.0038(16) 0.0014(15) N12 0.0124(18) 0.020(2) 0.0114(19) -0.0024(16) -0.0054(15) 0.0030(16) C1 0.026(3) 0.017(2) 0.019(2) -0.006(2) -0.012(2) 0.006(2) C2 0.036(3) 0.020(3) 0.019(3) -0.005(2) -0.015(2) 0.008(2) C3 0.035(3) 0.022(3) 0.018(3) 0.001(2) -0.010(2) -0.005(2) C4 0.026(3) 0.023(3) 0.028(3) -0.005(2) -0.015(2) -0.001(2) C5 0.022(2) 0.012(2) 0.014(2) -0.0049(18) -0.0093(19) 0.0058(18) C6 0.016(2) 0.022(3) 0.017(2) -0.006(2) -0.0074(19) -0.0002(19) C7 0.037(3) 0.020(3) 0.030(3) -0.005(2) -0.019(3) -0.005(2) C8 0.066(5) 0.024(3) 0.039(4) -0.010(3) -0.033(3) -0.008(3) C9 0.044(4) 0.036(3) 0.033(3) -0.010(3) -0.025(3) -0.007(3) C10 0.021(3) 0.029(3) 0.022(3) -0.007(2) -0.012(2) 0.001(2) C11 0.074(5) 0.017(3) 0.064(5) -0.017(3) -0.048(4) 0.011(3) C12 0.023(3) 0.027(3) 0.020(3) -0.011(2) -0.012(2) 0.006(2) C13 0.059(4) 0.048(4) 0.036(3) -0.030(3) -0.029(3) 0.037(3) C14 0.063(5) 0.059(5) 0.032(3) -0.032(3) -0.025(3) 0.039(4) C15 0.043(3) 0.044(4) 0.016(3) -0.013(3) -0.016(3) 0.021(3) C16 0.016(2) 0.020(2) 0.016(2) -0.006(2) -0.0072(19) 0.0039(19) C17 0.013(2) 0.031(3) 0.034(3) -0.008(3) -0.002(2) -0.002(2) C18 0.016(2) 0.025(3) 0.032(3) -0.011(2) -0.012(2) 0.008(2) C19 0.014(2) 0.036(3) 0.038(3) -0.014(3) -0.011(2) 0.008(2) C20 0.015(2) 0.031(3) 0.029(3) -0.013(2) -0.006(2) -0.005(2) C21 0.021(2) 0.021(3) 0.021(3) -0.005(2) -0.013(2) 0.002(2) C22 0.015(2) 0.021(2) 0.014(2) -0.0086(19) -0.0084(18) 0.0024(18) C23 0.016(2) 0.014(2) 0.015(2) -0.0036(19) -0.0056(19) 0.0009(18) C24 0.020(2) 0.018(2) 0.024(3) -0.003(2) -0.014(2) 0.0023(19) C25 0.029(3) 0.018(3) 0.026(3) -0.008(2) -0.012(2) 0.000(2) C26 0.024(3) 0.013(2) 0.026(3) -0.006(2) -0.012(2) 0.007(2) C27 0.014(2) 0.023(3) 0.018(2) -0.004(2) -0.0060(19) 0.0026(19) C28 0.040(3) 0.025(3) 0.041(4) -0.009(3) -0.023(3) -0.009(3) C29 0.017(2) 0.012(2) 0.020(2) -0.0053(19) -0.0069(19) 0.0017(18) C30 0.025(3) 0.028(3) 0.025(3) -0.015(2) -0.012(2) 0.004(2) C31 0.029(3) 0.036(3) 0.020(3) -0.019(2) -0.006(2) 0.005(2) C32 0.020(2) 0.024(3) 0.017(2) -0.008(2) -0.005(2) 0.006(2) C33 0.018(2) 0.011(2) 0.019(2) -0.0029(19) -0.0066(19) -0.0003(18) C34 0.037(4) 0.053(4) 0.027(3) 0.008(3) -0.011(3) -0.022(3) Ni4 0.0172(3) 0.0150(3) 0.0180(3) -0.0057(3) -0.0096(3) 0.0020(2) Ni5 0.0138(3) 0.0139(3) 0.0153(3) -0.0066(2) -0.0070(2) 0.0038(2) Ni6 0.0138(3) 0.0168(3) 0.0175(3) -0.0085(3) -0.0081(2) 0.0041(2) S5 0.0384(8) 0.0190(6) 0.0367(8) -0.0027(6) -0.0246(7) -0.0075(6) S6 0.0166(6) 0.0241(6) 0.0188(6) -0.0117(5) -0.0093(5) 0.0054(5) S7 0.0236(6) 0.0238(6) 0.0198(6) -0.0062(5) -0.0134(5) 0.0018(5) S8 0.0144(6) 0.0271(7) 0.0262(7) -0.0150(6) -0.0069(5) 0.0019(5) O9 0.054(3) 0.046(3) 0.035(2) -0.008(2) -0.025(2) -0.021(2) O10 0.047(3) 0.048(3) 0.040(3) 0.005(2) -0.019(2) -0.029(2) O11 0.0200(18) 0.029(2) 0.0257(19) -0.0182(17) -0.0093(15) 0.0038(15) O12 0.042(2) 0.034(2) 0.026(2) -0.0104(18) -0.0246(19) 0.0058(19) O13 0.033(2) 0.038(2) 0.032(2) -0.0045(19) -0.0225(19) -0.0084(18) O14 0.039(2) 0.031(2) 0.023(2) -0.0097(17) -0.0195(18) 0.0021(18) O15 0.0163(18) 0.038(2) 0.033(2) -0.0152(19) -0.0103(16) 0.0061(16) O16 0.030(2) 0.036(3) 0.057(3) -0.001(2) -0.021(2) -0.0112(19) O18 0.0167(17) 0.0259(19) 0.028(2) -0.0148(16) -0.0132(15) 0.0068(15) N13 0.017(2) 0.016(2) 0.018(2) -0.0023(17) -0.0095(17) 0.0011(16) N14 0.0117(18) 0.016(2) 0.019(2) -0.0088(17) -0.0065(16) 0.0046(15) N15 0.0151(19) 0.017(2) 0.016(2) -0.0091(17) -0.0073(16) 0.0042(16) N16 0.022(2) 0.015(2) 0.023(2) -0.0047(17) -0.0110(18) 0.0002(17) N17 0.017(2) 0.015(2) 0.020(2) -0.0034(17) -0.0093(17) 0.0041(16) N18 0.018(2) 0.018(2) 0.018(2) -0.0095(17) -0.0072(17) 0.0032(16) N19 0.023(2) 0.015(2) 0.023(2) -0.0068(18) -0.0111(18) 0.0013(17) N20 0.021(2) 0.016(2) 0.022(2) -0.0097(17) -0.0119(18) 0.0063(17) N21 0.0146(19) 0.019(2) 0.018(2) -0.0070(17) -0.0071(17) 0.0054(16) N22 0.017(2) 0.019(2) 0.0138(19) -0.0045(17) -0.0063(16) 0.0016(16) N23 0.017(2) 0.018(2) 0.0138(19) -0.0090(17) -0.0046(16) 0.0055(16) N24 0.018(2) 0.021(2) 0.018(2) -0.0079(18) -0.0076(17) 0.0022(17) C35 0.019(2) 0.020(3) 0.030(3) -0.005(2) -0.011(2) -0.001(2) C36 0.014(2) 0.036(3) 0.032(3) -0.006(3) -0.007(2) 0.003(2) C37 0.019(3) 0.036(3) 0.025(3) -0.012(2) -0.009(2) 0.011(2) C38 0.020(2) 0.027(3) 0.016(2) -0.009(2) -0.008(2) 0.007(2) C39 0.021(2) 0.018(2) 0.014(2) -0.0034(19) -0.010(2) 0.0042(19) C40 0.019(2) 0.017(2) 0.016(2) -0.0096(19) -0.0079(19) 0.0035(19) C41 0.017(2) 0.022(3) 0.029(3) -0.013(2) -0.013(2) 0.007(2) C42 0.028(3) 0.015(2) 0.024(3) -0.007(2) -0.014(2) 0.006(2) C43 0.025(3) 0.017(2) 0.031(3) -0.009(2) -0.012(2) -0.002(2) C44 0.020(2) 0.024(3) 0.020(2) -0.010(2) -0.012(2) 0.003(2) C45 0.089(6) 0.027(4) 0.133(9) -0.039(5) -0.082(7) 0.021(4) C46 0.017(2) 0.019(2) 0.023(3) -0.007(2) -0.012(2) 0.0050(19) C47 0.033(3) 0.020(3) 0.023(3) -0.002(2) -0.009(2) -0.003(2) C48 0.035(3) 0.022(3) 0.020(3) 0.000(2) -0.007(2) -0.001(2) C49 0.033(3) 0.021(3) 0.015(2) -0.005(2) -0.007(2) 0.004(2) C50 0.016(2) 0.018(2) 0.019(2) -0.008(2) -0.0102(19) 0.0083(19) C51 0.019(3) 0.029(3) 0.029(3) -0.015(2) -0.002(2) 0.005(2) C52 0.035(3) 0.023(3) 0.030(3) -0.012(2) -0.019(3) 0.002(2) C53 0.045(3) 0.028(3) 0.032(3) -0.020(3) -0.023(3) 0.009(3) C54 0.038(3) 0.031(3) 0.033(3) -0.020(3) -0.016(3) 0.017(3) C55 0.029(3) 0.026(3) 0.027(3) -0.017(2) -0.015(2) 0.012(2) C56 0.024(3) 0.012(2) 0.021(2) -0.005(2) -0.010(2) 0.0033(19) C57 0.016(2) 0.018(2) 0.017(2) -0.0082(19) -0.0049(19) 0.0037(18) C58 0.026(3) 0.018(2) 0.021(3) -0.010(2) -0.010(2) 0.004(2) C59 0.029(3) 0.017(2) 0.024(3) -0.004(2) -0.008(2) 0.008(2) C60 0.026(3) 0.033(3) 0.028(3) -0.007(2) -0.018(2) 0.011(2) C61 0.022(3) 0.022(3) 0.026(3) -0.008(2) -0.015(2) 0.006(2) C62 0.032(3) 0.035(3) 0.025(3) -0.012(3) -0.015(2) 0.014(3) C63 0.020(2) 0.019(2) 0.017(2) -0.010(2) -0.007(2) 0.0057(19) C64 0.028(3) 0.025(3) 0.020(3) -0.008(2) -0.011(2) 0.003(2) C65 0.031(3) 0.025(3) 0.020(3) -0.002(2) -0.009(2) -0.002(2) C66 0.022(3) 0.027(3) 0.025(3) -0.006(2) -0.007(2) -0.004(2) C67 0.019(2) 0.019(2) 0.020(2) -0.013(2) -0.007(2) 0.0049(19) C68 0.033(3) 0.084(6) 0.066(5) -0.061(5) -0.022(4) 0.027(4) C69 0.105(8) 0.047(5) 0.091(7) -0.017(5) -0.057(7) 0.003(5) Cl1 0.0767(15) 0.0534(12) 0.0648(14) -0.0117(11) -0.0212(12) 0.0001(11) Cl2 0.284(6) 0.096(3) 0.271(6) -0.052(3) -0.240(6) 0.021(3) C70 0.073(8) 0.240(18) 0.139(12) -0.143(13) 0.047(8) -0.097(10) Cl3 0.131(3) 0.299(6) 0.0298(12) -0.015(2) -0.0068(15) -0.110(4) Cl4 0.0535(14) 0.136(3) 0.171(4) -0.100(3) -0.0141(18) -0.0238(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N10 1.904(4) . ? Ni1 N4 1.905(4) . ? Ni1 N7 1.913(4) . ? Ni1 N1 1.922(4) . ? Ni1 Ni2 2.3488(8) . ? Ni2 N2 1.883(4) . ? Ni2 N8 1.889(4) . ? Ni2 N5 1.935(4) . ? Ni2 N11 1.946(4) . ? Ni2 Ni3 2.3880(8) . ? Ni3 O17 2.036(3) . ? Ni3 N12 2.046(4) . ? Ni3 N6 2.088(4) . ? Ni3 N3 2.104(4) . ? Ni3 N9 2.117(4) . ? S1 O1 1.433(4) . ? S1 O2 1.437(5) . ? S1 N4 1.625(4) . ? S1 C11 1.754(7) . ? S2 O3 1.449(4) . ? S2 O4 1.451(4) . ? S2 N6 1.600(4) . ? S2 C17 1.753(5) . ? S3 O5 1.431(4) . ? S3 O6 1.435(4) . ? S3 N10 1.626(4) . ? S3 C28 1.758(6) . ? S4 O8 1.430(4) . ? S4 O7 1.440(4) . ? S4 N12 1.601(4) . ? S4 C34 1.767(6) . ? O17 H17 0.8021 . ? O17 H17' 0.8023 . ? N1 C1 1.353(6) . ? N1 C5 1.365(6) . ? N2 C5 1.374(6) . ? N2 C6 1.380(6) . ? N3 C6 1.341(6) . ? N3 C10 1.351(6) . ? N4 C12 1.376(6) . ? N5 C16 1.366(6) . ? N5 C12 1.374(6) . ? N6 C16 1.395(6) . ? N7 C18 1.349(6) . ? N7 C22 1.356(6) . ? N8 C22 1.365(6) . ? N8 C23 1.379(6) . ? N9 C27 1.339(6) . ? N9 C23 1.359(6) . ? N10 C29 1.379(6) . ? N11 C33 1.367(6) . ? N11 C29 1.370(6) . ? N12 C33 1.388(6) . ? C1 C2 1.365(8) . ? C1 H1A 0.9500 . ? C2 C3 1.390(8) . ? C2 H2A 0.9500 . ? C3 C4 1.376(7) . ? C3 H3A 0.9500 . ? C4 C5 1.391(7) . ? C4 H4A 0.9500 . ? C6 C7 1.408(7) . ? C7 C8 1.365(8) . ? C7 H7A 0.9500 . ? C8 C9 1.379(9) . ? C8 H8A 0.9500 . ? C9 C10 1.377(8) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.398(7) . ? C13 C14 1.373(9) . ? C13 H13A 0.9500 . ? C14 C15 1.375(8) . ? C14 H14A 0.9500 . ? C15 C16 1.394(7) . ? C15 H15A 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.362(8) . ? C18 H18A 0.9500 . ? C19 C20 1.401(8) . ? C19 H19A 0.9500 . ? C20 C21 1.374(7) . ? C20 H20A 0.9500 . ? C21 C22 1.410(7) . ? C21 H21A 0.9500 . ? C23 C24 1.407(7) . ? C24 C25 1.370(7) . ? C24 H24A 0.9500 . ? C25 C26 1.388(7) . ? C25 H25A 0.9500 . ? C26 C27 1.369(7) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.398(7) . ? C30 C31 1.373(8) . ? C30 H30A 0.9500 . ? C31 C32 1.381(7) . ? C31 H31A 0.9500 . ? C32 C33 1.390(7) . ? C32 H32A 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? Ni4 N22 1.895(4) . ? Ni4 N16 1.902(4) . ? Ni4 N13 1.914(4) . ? Ni4 N19 1.930(4) . ? Ni4 Ni5 2.3542(8) . ? Ni5 N20 1.880(4) . ? Ni5 N14 1.896(4) . ? Ni5 N23 1.945(4) . ? Ni5 N17 1.946(4) . ? Ni5 Ni6 2.3924(8) . ? Ni6 O18 2.038(3) . ? Ni6 N24 2.067(4) . ? Ni6 N21 2.074(4) . ? Ni6 N15 2.097(4) . ? Ni6 N18 2.108(4) . ? S5 O9 1.427(4) . ? S5 O10 1.434(5) . ? S5 N16 1.618(4) . ? S5 C45 1.758(7) . ? S6 O11 1.445(4) . ? S6 O12 1.448(4) . ? S6 N18 1.595(4) . ? S6 C51 1.762(5) . ? S7 O13 1.437(4) . ? S7 O14 1.443(4) . ? S7 N22 1.631(4) . ? S7 C62 1.765(6) . ? S8 O16 1.431(4) . ? S8 O15 1.440(4) . ? S8 N24 1.607(4) . ? S8 C68 1.762(6) . ? O18 H18 0.8057 . ? O18 H18' 0.8052 . ? N13 C35 1.346(6) . ? N13 C39 1.365(6) . ? N14 C39 1.361(6) . ? N14 C40 1.385(6) . ? N15 C44 1.338(6) . ? N15 C40 1.351(6) . ? N16 C46 1.387(6) . ? N17 C50 1.371(6) . ? N17 C46 1.376(6) . ? N18 C50 1.401(6) . ? N19 C52 1.352(7) . ? N19 C56 1.366(6) . ? N20 C56 1.373(6) . ? N20 C57 1.381(6) . ? N21 C57 1.346(6) . ? N21 C61 1.353(6) . ? N22 C63 1.381(6) . ? N23 C63 1.369(6) . ? N23 C67 1.370(6) . ? N24 C67 1.379(6) . ? C35 C36 1.365(8) . ? C35 H35A 0.9500 . ? C36 C37 1.393(8) . ? C36 H36A 0.9500 . ? C37 C38 1.365(7) . ? C37 H37A 0.9500 . ? C38 C39 1.411(7) . ? C38 H38A 0.9500 . ? C40 C41 1.408(7) . ? C41 C42 1.375(7) . ? C41 H41A 0.9500 . ? C42 C43 1.396(7) . ? C42 H42A 0.9500 . ? C43 C44 1.377(7) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.390(7) . ? C47 C48 1.373(8) . ? C47 H47A 0.9500 . ? C48 C49 1.379(8) . ? C48 H48A 0.9500 . ? C49 C50 1.402(7) . ? C49 H49A 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.363(8) . ? C52 H52A 0.9500 . ? C53 C54 1.388(8) . ? C53 H53A 0.9500 . ? C54 C55 1.366(8) . ? C54 H54A 0.9500 . ? C55 C56 1.417(7) . ? C55 H55A 0.9500 . ? C57 C58 1.408(7) . ? C58 C59 1.381(7) . ? C58 H58A 0.9500 . ? C59 C60 1.388(8) . ? C59 H59A 0.9500 . ? C60 C61 1.373(7) . ? C60 H60A 0.9500 . ? C61 H61A 0.9500 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.397(7) . ? C64 C65 1.387(8) . ? C64 H64A 0.9500 . ? C65 C66 1.386(8) . ? C65 H65A 0.9500 . ? C66 C67 1.402(7) . ? C66 H66A 0.9500 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 Cl2 1.724(10) . ? C69 Cl1 1.773(9) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 Cl3 1.742(16) . ? C70 Cl4 1.750(18) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 Cl5' 1.715(10) . ? C71 Cl6 1.716(8) . ? C71 Cl6' 1.759(10) . ? C71 Cl5 1.791(8) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C71 H71C 0.9900 . ? C71 H71D 0.9900 . ? 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 N10 Ni1 N4 174.32(17) . . ? N10 Ni1 N7 91.49(18) . . ? N4 Ni1 N7 87.85(18) . . ? N10 Ni1 N1 89.70(17) . . ? N4 Ni1 N1 90.17(18) . . ? N7 Ni1 N1 171.91(17) . . ? N10 Ni1 Ni2 87.76(12) . . ? N4 Ni1 Ni2 86.57(12) . . ? N7 Ni1 Ni2 86.22(12) . . ? N1 Ni1 Ni2 85.84(12) . . ? N2 Ni2 N8 177.81(17) . . ? N2 Ni2 N5 88.33(18) . . ? N8 Ni2 N5 90.68(18) . . ? N2 Ni2 N11 91.74(17) . . ? N8 Ni2 N11 89.16(17) . . ? N5 Ni2 N11 177.47(17) . . ? N2 Ni2 Ni1 89.47(12) . . ? N8 Ni2 Ni1 88.56(12) . . ? N5 Ni2 Ni1 89.39(12) . . ? N11 Ni2 Ni1 88.08(12) . . ? N2 Ni2 Ni3 90.70(12) . . ? N8 Ni2 Ni3 91.29(12) . . ? N5 Ni2 Ni3 91.78(12) . . ? N11 Ni2 Ni3 90.75(12) . . ? Ni1 Ni2 Ni3 178.83(4) . . ? O17 Ni3 N12 94.71(15) . . ? O17 Ni3 N6 99.44(15) . . ? N12 Ni3 N6 165.83(15) . . ? O17 Ni3 N3 103.71(15) . . ? N12 Ni3 N3 91.82(16) . . ? N6 Ni3 N3 84.02(16) . . ? O17 Ni3 N9 92.55(15) . . ? N12 Ni3 N9 86.63(16) . . ? N6 Ni3 N9 93.57(16) . . ? N3 Ni3 N9 163.73(15) . . ? O17 Ni3 Ni2 173.79(11) . . ? N12 Ni3 Ni2 82.81(11) . . ? N6 Ni3 Ni2 83.20(11) . . ? N3 Ni3 Ni2 82.10(11) . . ? N9 Ni3 Ni2 81.64(11) . . ? O1 S1 O2 116.8(3) . . ? O1 S1 N4 104.5(2) . . ? O2 S1 N4 113.0(2) . . ? O1 S1 C11 107.7(3) . . ? O2 S1 C11 108.4(3) . . ? N4 S1 C11 105.9(3) . . ? O3 S2 O4 114.1(2) . . ? O3 S2 N6 114.5(2) . . ? O4 S2 N6 107.8(2) . . ? O3 S2 C17 106.8(3) . . ? O4 S2 C17 107.3(3) . . ? N6 S2 C17 105.8(3) . . ? O5 S3 O6 117.5(2) . . ? O5 S3 N10 105.2(2) . . ? O6 S3 N10 112.7(2) . . ? O5 S3 C28 108.0(3) . . ? O6 S3 C28 107.3(3) . . ? N10 S3 C28 105.4(3) . . ? O8 S4 O7 115.2(2) . . ? O8 S4 N12 114.3(3) . . ? O7 S4 N12 107.0(2) . . ? O8 S4 C34 107.3(3) . . ? O7 S4 C34 107.3(3) . . ? N12 S4 C34 105.0(3) . . ? Ni3 O17 H17 105.7 . . ? Ni3 O17 H17' 114.2 . . ? H17 O17 H17' 120.8 . . ? C1 N1 C5 119.4(4) . . ? C1 N1 Ni1 119.5(3) . . ? C5 N1 Ni1 121.0(3) . . ? C5 N2 C6 123.8(4) . . ? C5 N2 Ni2 118.0(3) . . ? C6 N2 Ni2 117.6(3) . . ? C6 N3 C10 118.9(4) . . ? C6 N3 Ni3 120.7(3) . . ? C10 N3 Ni3 120.0(3) . . ? C12 N4 S1 124.9(3) . . ? C12 N4 Ni1 121.8(3) . . ? S1 N4 Ni1 112.3(2) . . ? C16 N5 C12 120.3(4) . . ? C16 N5 Ni2 120.8(3) . . ? C12 N5 Ni2 118.7(3) . . ? C16 N6 S2 118.6(3) . . ? C16 N6 Ni3 117.9(3) . . ? S2 N6 Ni3 123.2(2) . . ? C18 N7 C22 119.6(4) . . ? C18 N7 Ni1 119.5(3) . . ? C22 N7 Ni1 120.8(3) . . ? C22 N8 C23 124.3(4) . . ? C22 N8 Ni2 117.5(3) . . ? C23 N8 Ni2 117.6(3) . . ? C27 N9 C23 118.0(4) . . ? C27 N9 Ni3 120.5(3) . . ? C23 N9 Ni3 120.9(3) . . ? C29 N10 S3 122.8(3) . . ? C29 N10 Ni1 121.0(3) . . ? S3 N10 Ni1 115.8(2) . . ? C33 N11 C29 120.2(4) . . ? C33 N11 Ni2 119.9(3) . . ? C29 N11 Ni2 119.6(3) . . ? C33 N12 S4 119.7(3) . . ? C33 N12 Ni3 117.7(3) . . ? S4 N12 Ni3 121.8(2) . . ? N1 C1 C2 122.5(5) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C1 C2 C3 118.8(5) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C4 C3 C2 119.1(5) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? N1 C5 N2 116.1(4) . . ? N1 C5 C4 119.6(4) . . ? N2 C5 C4 124.2(4) . . ? N3 C6 N2 115.4(4) . . ? N3 C6 C7 120.8(5) . . ? N2 C6 C7 123.5(5) . . ? C8 C7 C6 119.6(5) . . ? C8 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? C7 C8 C9 119.4(5) . . ? C7 C8 H8A 120.3 . . ? C9 C8 H8A 120.3 . . ? C10 C9 C8 119.0(5) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? N3 C10 C9 122.4(5) . . ? N3 C10 H10A 118.8 . . ? C9 C10 H10A 118.8 . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 N4 115.4(4) . . ? N5 C12 C13 119.9(5) . . ? N4 C12 C13 124.6(5) . . ? C14 C13 C12 119.5(5) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C13 C14 C15 120.6(6) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C14 C15 C16 119.6(5) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? N5 C16 C15 120.1(4) . . ? N5 C16 N6 115.1(4) . . ? C15 C16 N6 124.7(5) . . ? S2 C17 H17A 109.5 . . ? S2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 123.0(5) . . ? N7 C18 H18A 118.5 . . ? C19 C18 H18A 118.5 . . ? C18 C19 C20 118.5(5) . . ? C18 C19 H19A 120.7 . . ? C20 C19 H19A 120.7 . . ? C21 C20 C19 119.1(5) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C22 120.1(5) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? N7 C22 N8 116.4(4) . . ? N7 C22 C21 119.6(4) . . ? N8 C22 C21 123.9(4) . . ? N9 C23 N8 114.9(4) . . ? N9 C23 C24 120.7(4) . . ? N8 C23 C24 124.0(4) . . ? C25 C24 C23 119.6(5) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 119.4(5) . . ? C24 C25 H25A 120.3 . . ? C26 C25 H25A 120.3 . . ? C27 C26 C25 118.2(5) . . ? C27 C26 H26A 120.9 . . ? C25 C26 H26A 120.9 . . ? N9 C27 C26 124.0(5) . . ? N9 C27 H27A 118.0 . . ? C26 C27 H27A 118.0 . . ? S3 C28 H28A 109.5 . . ? S3 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S3 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N11 C29 N10 115.3(4) . . ? N11 C29 C30 120.1(4) . . ? N10 C29 C30 124.6(5) . . ? C31 C30 C29 119.2(5) . . ? C31 C30 H30A 120.4 . . ? C29 C30 H30A 120.4 . . ? C30 C31 C32 120.9(5) . . ? C30 C31 H31A 119.5 . . ? C32 C31 H31A 119.5 . . ? C31 C32 C33 118.9(5) . . ? C31 C32 H32A 120.5 . . ? C33 C32 H32A 120.5 . . ? N11 C33 N12 114.2(4) . . ? N11 C33 C32 120.6(4) . . ? N12 C33 C32 125.2(4) . . ? S4 C34 H34A 109.5 . . ? S4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? S4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N22 Ni4 N16 174.33(18) . . ? N22 Ni4 N13 90.97(17) . . ? N16 Ni4 N13 87.12(18) . . ? N22 Ni4 N19 90.78(18) . . ? N16 Ni4 N19 90.41(18) . . ? N13 Ni4 N19 172.23(18) . . ? N22 Ni4 Ni5 87.13(13) . . ? N16 Ni4 Ni5 87.41(13) . . ? N13 Ni4 Ni5 86.10(12) . . ? N19 Ni4 Ni5 86.43(13) . . ? N20 Ni5 N14 177.97(18) . . ? N20 Ni5 N23 92.15(17) . . ? N14 Ni5 N23 88.41(17) . . ? N20 Ni5 N17 89.35(18) . . ? N14 Ni5 N17 90.00(17) . . ? N23 Ni5 N17 176.74(17) . . ? N20 Ni5 Ni4 89.39(13) . . ? N14 Ni5 Ni4 88.67(12) . . ? N23 Ni5 Ni4 88.47(12) . . ? N17 Ni5 Ni4 88.64(12) . . ? N20 Ni5 Ni6 91.09(13) . . ? N14 Ni5 Ni6 90.86(12) . . ? N23 Ni5 Ni6 90.47(12) . . ? N17 Ni5 Ni6 92.40(12) . . ? Ni4 Ni5 Ni6 178.86(4) . . ? O18 Ni6 N24 95.44(16) . . ? O18 Ni6 N21 102.57(15) . . ? N24 Ni6 N21 89.94(16) . . ? O18 Ni6 N15 92.74(15) . . ? N24 Ni6 N15 87.36(16) . . ? N21 Ni6 N15 164.64(16) . . ? O18 Ni6 N18 98.90(15) . . ? N24 Ni6 N18 165.64(16) . . ? N21 Ni6 N18 86.43(16) . . ? N15 Ni6 N18 92.48(16) . . ? O18 Ni6 Ni5 174.76(11) . . ? N24 Ni6 Ni5 82.78(12) . . ? N21 Ni6 Ni5 82.39(12) . . ? N15 Ni6 Ni5 82.27(11) . . ? N18 Ni6 Ni5 82.97(11) . . ? O9 S5 O10 116.1(3) . . ? O9 S5 N16 105.6(2) . . ? O10 S5 N16 113.3(3) . . ? O9 S5 C45 108.2(4) . . ? O10 S5 C45 108.4(4) . . ? N16 S5 C45 104.4(3) . . ? O11 S6 O12 114.6(2) . . ? O11 S6 N18 107.5(2) . . ? O12 S6 N18 114.2(2) . . ? O11 S6 C51 107.3(2) . . ? O12 S6 C51 106.7(3) . . ? N18 S6 C51 106.0(2) . . ? O13 S7 O14 116.9(2) . . ? O13 S7 N22 104.7(2) . . ? O14 S7 N22 112.2(2) . . ? O13 S7 C62 108.3(3) . . ? O14 S7 C62 108.1(3) . . ? N22 S7 C62 106.1(2) . . ? O16 S8 O15 115.1(3) . . ? O16 S8 N24 113.9(3) . . ? O15 S8 N24 107.0(2) . . ? O16 S8 C68 107.5(4) . . ? O15 S8 C68 107.1(3) . . ? N24 S8 C68 105.6(3) . . ? Ni6 O18 H18 108.2 . . ? Ni6 O18 H18' 115.6 . . ? H18 O18 H18' 119.6 . . ? C35 N13 C39 119.5(4) . . ? C35 N13 Ni4 119.3(4) . . ? C39 N13 Ni4 121.1(3) . . ? C39 N14 C40 124.6(4) . . ? C39 N14 Ni5 117.3(3) . . ? C40 N14 Ni5 117.7(3) . . ? C44 N15 C40 118.4(4) . . ? C44 N15 Ni6 119.9(3) . . ? C40 N15 Ni6 121.2(3) . . ? C46 N16 S5 122.8(4) . . ? C46 N16 Ni4 120.2(3) . . ? S5 N16 Ni4 115.3(2) . . ? C50 N17 C46 119.8(4) . . ? C50 N17 Ni5 120.5(3) . . ? C46 N17 Ni5 119.7(3) . . ? C50 N18 S6 117.4(3) . . ? C50 N18 Ni6 118.7(3) . . ? S6 N18 Ni6 123.7(2) . . ? C52 N19 C56 119.9(4) . . ? C52 N19 Ni4 119.6(4) . . ? C56 N19 Ni4 120.4(3) . . ? C56 N20 C57 123.1(4) . . ? C56 N20 Ni5 118.1(3) . . ? C57 N20 Ni5 118.7(3) . . ? C57 N21 C61 118.9(4) . . ? C57 N21 Ni6 121.7(3) . . ? C61 N21 Ni6 119.4(3) . . ? C63 N22 S7 122.1(3) . . ? C63 N22 Ni4 123.0(3) . . ? S7 N22 Ni4 114.9(2) . . ? C63 N23 C67 120.5(4) . . ? C63 N23 Ni5 118.9(3) . . ? C67 N23 Ni5 120.0(3) . . ? C67 N24 S8 120.3(4) . . ? C67 N24 Ni6 116.5(3) . . ? S8 N24 Ni6 121.6(2) . . ? N13 C35 C36 123.3(5) . . ? N13 C35 H35A 118.4 . . ? C36 C35 H35A 118.4 . . ? C35 C36 C37 118.0(5) . . ? C35 C36 H36A 121.0 . . ? C37 C36 H36A 121.0 . . ? C38 C37 C36 119.8(5) . . ? C38 C37 H37A 120.1 . . ? C36 C37 H37A 120.1 . . ? C37 C38 C39 120.2(5) . . ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 . . ? N14 C39 N13 116.4(4) . . ? N14 C39 C38 124.4(5) . . ? N13 C39 C38 119.0(5) . . ? N15 C40 N14 115.2(4) . . ? N15 C40 C41 121.1(4) . . ? N14 C40 C41 123.5(4) . . ? C42 C41 C40 119.2(5) . . ? C42 C41 H41A 120.4 . . ? C40 C41 H41A 120.4 . . ? C41 C42 C43 119.5(5) . . ? C41 C42 H42A 120.2 . . ? C43 C42 H42A 120.2 . . ? C44 C43 C42 117.7(5) . . ? C44 C43 H43A 121.1 . . ? C42 C43 H43A 121.1 . . ? N15 C44 C43 124.0(5) . . ? N15 C44 H44A 118.0 . . ? C43 C44 H44A 118.0 . . ? S5 C45 H45A 109.5 . . ? S5 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? S5 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N17 C46 N16 115.0(4) . . ? N17 C46 C47 120.8(5) . . ? N16 C46 C47 124.1(5) . . ? C48 C47 C46 119.0(5) . . ? C48 C47 H47A 120.5 . . ? C46 C47 H47A 120.5 . . ? C47 C48 C49 121.0(5) . . ? C47 C48 H48A 119.5 . . ? C49 C48 H48A 119.5 . . ? C48 C49 C50 119.2(5) . . ? C48 C49 H49A 120.4 . . ? C50 C49 H49A 120.4 . . ? N17 C50 N18 115.4(4) . . ? N17 C50 C49 120.0(5) . . ? N18 C50 C49 124.6(5) . . ? S6 C51 H51A 109.5 . . ? S6 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S6 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N19 C52 C53 122.4(5) . . ? N19 C52 H52A 118.8 . . ? C53 C52 H52A 118.8 . . ? C52 C53 C54 119.2(5) . . ? C52 C53 H53A 120.4 . . ? C54 C53 H53A 120.4 . . ? C55 C54 C53 119.3(5) . . ? C55 C54 H54A 120.3 . . ? C53 C54 H54A 120.3 . . ? C54 C55 C56 120.3(5) . . ? C54 C55 H55A 119.8 . . ? C56 C55 H55A 119.8 . . ? N19 C56 N20 116.8(4) . . ? N19 C56 C55 118.8(5) . . ? N20 C56 C55 124.3(5) . . ? N21 C57 N20 115.3(4) . . ? N21 C57 C58 120.3(4) . . ? N20 C57 C58 124.2(4) . . ? C59 C58 C57 119.5(5) . . ? C59 C58 H58A 120.2 . . ? C57 C58 H58A 120.2 . . ? C58 C59 C60 119.9(5) . . ? C58 C59 H59A 120.0 . . ? C60 C59 H59A 120.0 . . ? C61 C60 C59 117.4(5) . . ? C61 C60 H60A 121.3 . . ? C59 C60 H60A 121.3 . . ? N21 C61 C60 123.8(5) . . ? N21 C61 H61A 118.1 . . ? C60 C61 H61A 118.1 . . ? S7 C62 H62A 109.5 . . ? S7 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? S7 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N23 C63 N22 114.7(4) . . ? N23 C63 C64 120.6(5) . . ? N22 C63 C64 124.6(5) . . ? C65 C64 C63 118.6(5) . . ? C65 C64 H64A 120.7 . . ? C63 C64 H64A 120.7 . . ? C66 C65 C64 121.0(5) . . ? C66 C65 H65A 119.5 . . ? C64 C65 H65A 119.5 . . ? C65 C66 C67 118.9(5) . . ? C65 C66 H66A 120.6 . . ? C67 C66 H66A 120.6 . . ? N23 C67 N24 114.7(4) . . ? N23 C67 C66 120.2(5) . . ? N24 C67 C66 125.1(5) . . ? S8 C68 H68A 109.5 . . ? S8 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? S8 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? Cl2 C69 Cl1 110.4(5) . . ? Cl2 C69 H69A 109.6 . . ? Cl1 C69 H69A 109.6 . . ? Cl2 C69 H69B 109.6 . . ? Cl1 C69 H69B 109.6 . . ? H69A C69 H69B 108.1 . . ? Cl3 C70 Cl4 114.2(6) . . ? Cl3 C70 H70A 108.7 . . ? Cl4 C70 H70A 108.7 . . ? Cl3 C70 H70B 108.7 . . ? Cl4 C70 H70B 108.7 . . ? H70A C70 H70B 107.6 . . ? Cl5' C71 Cl6 69.5(10) . . ? Cl5' C71 Cl6' 105.5(13) . . ? Cl6 C71 Cl6' 42.3(8) . . ? Cl5' C71 Cl5 50.4(9) . . ? Cl6 C71 Cl5 108.8(6) . . ? Cl6' C71 Cl5 120.0(10) . . ? Cl5' C71 H71A 95.3 . . ? Cl6 C71 H71A 109.9 . . ? Cl6' C71 H71A 128.2 . . ? Cl5 C71 H71A 109.9 . . ? Cl5' C71 H71B 154.3 . . ? Cl6 C71 H71B 109.9 . . ? Cl6' C71 H71B 67.8 . . ? Cl5 C71 H71B 109.9 . . ? H71A C71 H71B 108.3 . . ? Cl5' C71 H71C 110.6 . . ? Cl6 C71 H71C 144.9 . . ? Cl6' C71 H71C 110.6 . . ? Cl5 C71 H71C 60.3 . . ? H71A C71 H71C 105.1 . . ? H71B C71 H71C 54.2 . . ? Cl5' C71 H71D 110.6 . . ? Cl6 C71 H71D 103.3 . . ? Cl6' C71 H71D 110.7 . . ? Cl5 C71 H71D 128.8 . . ? H71A C71 H71D 19.5 . . ? H71B C71 H71D 94.7 . . ? H71C C71 H71D 108.8 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.780 _refine_diff_density_min -1.609 _refine_diff_density_rms 0.130 #===END data_ic11181(comp3) _database_code_depnum_ccdc_archive 'CCDC 618765' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H45 N12 Ni3 O4.50' _chemical_formula_weight 1014.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6867(2) _cell_length_b 14.9385(2) _cell_length_c 20.4837(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.5497(8) _cell_angle_gamma 90.00 _cell_volume 4685.38(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour deep-brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2100 _exptl_absorpt_coefficient_mu 1.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.542 _exptl_absorpt_correction_T_max 0.805 _exptl_absorpt_process_details ? _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30002 _diffrn_reflns_av_R_equivalents 0.0910 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10728 _reflns_number_gt 8525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1053P)^2^+7.4812P] 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 10728 _refine_ls_number_parameters 588 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.2013 _refine_ls_wR_factor_gt 0.1888 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.016 _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 0.12687(3) 0.72189(3) 0.32646(2) 0.02681(15) Uani 1 1 d . . . Ni2 Ni 0.25239(3) 0.74124(3) 0.27817(2) 0.02355(14) Uani 1 1 d . . . Ni3 Ni 0.37412(3) 0.75048(3) 0.22479(2) 0.02582(15) Uani 1 1 d . . . N1 N 0.1063(2) 0.8534(2) 0.29838(16) 0.0309(7) Uani 1 1 d . . . N2 N 0.25006(18) 0.8663(2) 0.28973(15) 0.0274(6) Uani 1 1 d . . . N3 N 0.3930(2) 0.8720(2) 0.27661(15) 0.0286(7) Uani 1 1 d . . . N4 N 0.2147(2) 0.7621(2) 0.41370(16) 0.0269(6) Uani 1 1 d . . . N5 N 0.3287(2) 0.7279(2) 0.36248(15) 0.0259(6) Uani 1 1 d . . . N6 N 0.43795(19) 0.6843(2) 0.30985(15) 0.0276(6) Uani 1 1 d . . . N7 N 0.0615(2) 0.5659(2) 0.41584(17) 0.0349(8) Uani 1 1 d . . . N8 N 0.1612(2) 0.5923(2) 0.34238(16) 0.0284(7) Uani 1 1 d . . . N9 N 0.25184(19) 0.6145(2) 0.26692(15) 0.0269(6) Uani 1 1 d . . . N10 N 0.1778(2) 0.7565(2) 0.19249(16) 0.0264(7) Uani 1 1 d . . . N11 N 0.2924(2) 0.8121(2) 0.14801(15) 0.0282(7) Uani 1 1 d . . . N12 N 0.4100(2) 0.8616(2) 0.09695(16) 0.0336(7) Uani 1 1 d . . . O1 O 0.02500(17) 0.7074(2) 0.36622(14) 0.0353(6) Uani 1 1 d . . . O2 O 0.32680(17) 0.62846(18) 0.18470(13) 0.0296(6) Uani 1 1 d . . . O3 O 0.06800(17) 0.6888(2) 0.22868(13) 0.0331(6) Uani 1 1 d . . . O4 O 0.47195(19) 0.7569(2) 0.17978(15) 0.0344(6) Uani 1 1 d . . . C1 C 0.0236(3) 0.8851(3) 0.2884(2) 0.0380(9) Uani 1 1 d . . . H1A H -0.0208 0.8465 0.2970 0.046 Uiso 1 1 calc R . . C2 C 0.0009(3) 0.9711(3) 0.2663(2) 0.0447(11) Uani 1 1 d . . . H2A H -0.0573 0.9922 0.2616 0.054 Uiso 1 1 calc R . . C3 C 0.0653(3) 1.0256(3) 0.2511(2) 0.0434(10) Uani 1 1 d . . . H3A H 0.0515 1.0845 0.2348 0.052 Uiso 1 1 calc R . . C4 C 0.1494(3) 0.9941(3) 0.2596(2) 0.0359(9) Uani 1 1 d . . . H4A H 0.1937 1.0312 0.2490 0.043 Uiso 1 1 calc R . . C5 C 0.1698(2) 0.9074(3) 0.28384(18) 0.0289(8) Uani 1 1 d . . . C6 C 0.3279(2) 0.9133(3) 0.29912(19) 0.0286(8) Uani 1 1 d . . . C7 C 0.3429(3) 0.9963(3) 0.3322(2) 0.0375(9) Uani 1 1 d . . . H7A H 0.2970 1.0252 0.3477 0.045 Uiso 1 1 calc R . . C8 C 0.4238(3) 1.0355(3) 0.3422(2) 0.0462(11) Uani 1 1 d . . . H8A H 0.4340 1.0918 0.3641 0.055 Uiso 1 1 calc R . . C9 C 0.4911(3) 0.9920(3) 0.3201(2) 0.0417(10) Uani 1 1 d . . . H9A H 0.5477 1.0176 0.3267 0.050 Uiso 1 1 calc R . . C10 C 0.4727(3) 0.9111(3) 0.2884(2) 0.0347(9) Uani 1 1 d . . . H10A H 0.5186 0.8809 0.2739 0.042 Uiso 1 1 calc R . . C11 C 0.1851(3) 0.7979(3) 0.46509(19) 0.0311(8) Uani 1 1 d . . . H11A H 0.1239 0.7998 0.4620 0.037 Uiso 1 1 calc R . . C12 C 0.2390(3) 0.8316(3) 0.5215(2) 0.0335(8) Uani 1 1 d . . . H12A H 0.2154 0.8555 0.5568 0.040 Uiso 1 1 calc R . . C13 C 0.3287(3) 0.8303(3) 0.5261(2) 0.0354(9) Uani 1 1 d . . . H13A H 0.3674 0.8533 0.5647 0.042 Uiso 1 1 calc R . . C14 C 0.3610(3) 0.7953(3) 0.47406(19) 0.0321(8) Uani 1 1 d . . . H14A H 0.4220 0.7947 0.4761 0.038 Uiso 1 1 calc R . . C15 C 0.3025(2) 0.7603(2) 0.41781(18) 0.0255(7) Uani 1 1 d . . . C16 C 0.4058(2) 0.6820(3) 0.36682(18) 0.0265(7) Uani 1 1 d . . . C17 C 0.4463(2) 0.6308(3) 0.4220(2) 0.0323(8) Uani 1 1 d . . . H17A H 0.4241 0.6307 0.4616 0.039 Uiso 1 1 calc R . . C18 C 0.5191(3) 0.5805(3) 0.4184(2) 0.0395(10) Uani 1 1 d . . . H18A H 0.5466 0.5445 0.4552 0.047 Uiso 1 1 calc R . . C19 C 0.5518(3) 0.5832(3) 0.3599(2) 0.0408(10) Uani 1 1 d . . . H19A H 0.6021 0.5497 0.3565 0.049 Uiso 1 1 calc R . . C20 C 0.5098(2) 0.6350(3) 0.3082(2) 0.0334(8) Uani 1 1 d . . . H20A H 0.5323 0.6367 0.2688 0.040 Uiso 1 1 calc R . . C21 C 0.0171(3) 0.6412(3) 0.4044(2) 0.0352(9) Uani 1 1 d . . . C22 C -0.0550(3) 0.6512(4) 0.4423(3) 0.0513(12) Uani 1 1 d . . . H22A H -0.0596 0.7141 0.4546 0.077 Uiso 1 1 calc R . . H22B H -0.0416 0.6144 0.4828 0.077 Uiso 1 1 calc R . . H22C H -0.1104 0.6315 0.4139 0.077 Uiso 1 1 calc R . . C23 C 0.1293(3) 0.5417(3) 0.38651(19) 0.0311(8) Uani 1 1 d . . . C24 C 0.1674(3) 0.4574(3) 0.4059(2) 0.0391(9) Uani 1 1 d . . . H24A H 0.1442 0.4206 0.4357 0.047 Uiso 1 1 calc R . . C25 C 0.2375(3) 0.4285(3) 0.3819(2) 0.0420(10) Uani 1 1 d . . . H25A H 0.2650 0.3733 0.3970 0.050 Uiso 1 1 calc R . . C26 C 0.2681(3) 0.4797(3) 0.3358(2) 0.0372(9) Uani 1 1 d . . . H26A H 0.3170 0.4607 0.3190 0.045 Uiso 1 1 calc R . . C27 C 0.2262(2) 0.5595(3) 0.31460(19) 0.0282(8) Uani 1 1 d . . . C28 C 0.2812(2) 0.5807(3) 0.21486(19) 0.0280(8) Uani 1 1 d . . . C29 C 0.2568(3) 0.4886(3) 0.1864(2) 0.0406(10) Uani 1 1 d . . . H29A H 0.2847 0.4777 0.1498 0.061 Uiso 1 1 d R . . H29B H 0.2756 0.4445 0.2206 0.061 Uiso 1 1 d R . . H29C H 0.1946 0.4850 0.1708 0.061 Uiso 1 1 d R . . C30 C 0.0424(3) 0.7070(4) 0.1116(2) 0.0434(10) Uani 1 1 d . . . H30A H 0.0211 0.6452 0.1063 0.065 Uiso 1 1 calc R . . H30B H 0.0775 0.7196 0.0785 0.065 Uiso 1 1 calc R . . H30C H -0.0074 0.7481 0.1049 0.065 Uiso 1 1 calc R . . C31 C 0.0980(2) 0.7194(3) 0.18138(19) 0.0297(8) Uani 1 1 d . . . C32 C 0.2053(2) 0.8149(3) 0.14704(18) 0.0273(7) Uani 1 1 d . . . C33 C 0.1499(3) 0.8752(3) 0.10785(19) 0.0336(8) Uani 1 1 d . . . H33A H 0.0906 0.8801 0.1112 0.040 Uiso 1 1 calc R . . C34 C 0.1824(3) 0.9283(3) 0.0636(2) 0.0378(9) Uani 1 1 d . . . H34A H 0.1452 0.9691 0.0353 0.045 Uiso 1 1 calc R . . C35 C 0.2691(3) 0.9216(3) 0.0609(2) 0.0359(9) Uani 1 1 d . . . H35A H 0.2914 0.9564 0.0296 0.043 Uiso 1 1 calc R . . C36 C 0.3241(3) 0.8636(3) 0.10406(18) 0.0300(8) Uani 1 1 d . . . C37 C 0.4715(3) 0.8101(3) 0.13042(19) 0.0324(8) Uani 1 1 d . . . C38 C 0.5567(3) 0.8106(4) 0.1073(2) 0.0452(11) Uani 1 1 d . . . H38A H 0.6056 0.8120 0.1463 0.068 Uiso 1 1 calc R . . H38B H 0.5591 0.8636 0.0795 0.068 Uiso 1 1 calc R . . H38C H 0.5606 0.7565 0.0810 0.068 Uiso 1 1 calc R . . C39 C 0.9181(5) 0.9630(5) 0.4881(3) 0.0749(18) Uani 1 1 d . . . H39A H 0.8612 0.9378 0.4800 0.090 Uiso 1 1 calc R . . C40 C 0.9728(5) 0.9458(5) 0.4448(3) 0.0739(18) Uani 1 1 d . . . H40A H 0.9540 0.9083 0.4069 0.089 Uiso 1 1 calc R . . C41 C 1.0534(5) 0.9832(4) 0.4572(3) 0.0690(17) Uani 1 1 d . . . H41A H 1.0910 0.9720 0.4275 0.083 Uiso 1 1 calc R . . C42 C 0.3651(7) 0.1930(8) 0.5606(5) 0.055(2) Uiso 0.50 1 d PD A 1 H42A H 0.4031 0.2107 0.6013 0.066 Uiso 0.50 1 calc PR A 1 C43 C 0.2983(8) 0.2497(9) 0.5265(6) 0.081(4) Uiso 0.50 1 d PD A 1 H43A H 0.2954 0.3102 0.5403 0.098 Uiso 0.50 1 calc PR A 1 C44 C 0.2366(8) 0.2166(8) 0.4724(5) 0.067(3) Uiso 0.50 1 d PD A 1 H44A H 0.1898 0.2536 0.4506 0.081 Uiso 0.50 1 calc PR A 1 C45 C 0.2433(8) 0.1295(7) 0.4502(6) 0.075(3) Uiso 0.50 1 d PD A 1 H45A H 0.2007 0.1058 0.4142 0.090 Uiso 0.50 1 calc PR A 1 C46 C 0.3140(7) 0.0778(9) 0.4820(6) 0.076(3) Uiso 0.50 1 d PD A 1 H46A H 0.3224 0.0182 0.4686 0.091 Uiso 0.50 1 calc PR A 1 C47 C 0.3719(8) 0.1191(10) 0.5350(6) 0.076(3) Uiso 0.50 1 d PD A 1 H47A H 0.4231 0.0861 0.5537 0.091 Uiso 0.50 1 calc PR A 1 C48 C 0.1475(9) 0.2217(12) 0.3298(5) 0.113(6) Uiso 0.50 1 d PD B 2 H48A H 0.1664 0.1886 0.3718 0.169 Uiso 0.50 1 d PR B 2 H48B H 0.0924 0.1966 0.3046 0.169 Uiso 0.50 1 d PR B 2 H48C H 0.1390 0.2848 0.3397 0.169 Uiso 0.50 1 d PR B 2 C49 C 0.2272(5) 0.2058(5) 0.3068(3) 0.0301(15) Uiso 0.50 1 d PD B 2 H49A H 0.2778 0.2365 0.3354 0.036 Uiso 0.50 1 calc PR B 2 H49B H 0.2400 0.1410 0.3050 0.036 Uiso 0.50 1 calc PR B 2 O5 O 0.2051(6) 0.2442(6) 0.2415(4) 0.078(3) Uiso 0.50 1 d PD B 2 C50 C 0.2688(7) 0.2235(8) 0.2024(5) 0.059(3) Uiso 0.50 1 d PD B 2 H50A H 0.2448 0.1707 0.1753 0.071 Uiso 0.50 1 calc PR B 2 H50B H 0.3205 0.2015 0.2352 0.071 Uiso 0.50 1 calc PR B 2 C51 C 0.3044(9) 0.2803(10) 0.1568(7) 0.081(4) Uiso 0.50 1 d PD B 2 H51D H 0.3468 0.2476 0.1389 0.121 Uiso 0.50 1 d PR B 2 H51A H 0.2576 0.2989 0.1210 0.121 Uiso 0.50 1 d PR B 2 H51B H 0.3316 0.3321 0.1803 0.121 Uiso 0.50 1 d PR B 2 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 0.0216(2) 0.0283(3) 0.0310(3) -0.0005(2) 0.00654(18) 0.00035(19) Ni2 0.0211(2) 0.0227(3) 0.0264(3) 0.00021(17) 0.00432(19) 0.00067(17) Ni3 0.0234(3) 0.0254(3) 0.0291(3) 0.00177(18) 0.00670(19) 0.00041(18) N1 0.0261(15) 0.0317(17) 0.0337(16) -0.0013(14) 0.0041(13) 0.0073(13) N2 0.0229(15) 0.0243(16) 0.0333(16) 0.0012(13) 0.0023(12) 0.0021(12) N3 0.0271(15) 0.0274(16) 0.0300(16) 0.0020(13) 0.0033(12) -0.0015(13) N4 0.0242(15) 0.0267(16) 0.0292(16) 0.0009(12) 0.0047(12) 0.0023(12) N5 0.0228(14) 0.0265(16) 0.0276(15) 0.0009(12) 0.0036(12) 0.0026(12) N6 0.0233(14) 0.0277(16) 0.0314(16) 0.0008(13) 0.0049(12) 0.0031(12) N7 0.0304(16) 0.0381(19) 0.0388(18) -0.0003(15) 0.0131(14) -0.0031(15) N8 0.0248(15) 0.0294(17) 0.0311(15) -0.0024(13) 0.0063(12) -0.0025(13) N9 0.0252(15) 0.0248(16) 0.0316(16) -0.0017(13) 0.0082(12) -0.0009(12) N10 0.0216(15) 0.0283(17) 0.0281(15) 0.0015(12) 0.0026(12) 0.0005(12) N11 0.0293(15) 0.0241(16) 0.0301(15) 0.0001(13) 0.0039(12) -0.0008(13) N12 0.0353(17) 0.0314(18) 0.0350(17) 0.0009(14) 0.0095(14) -0.0079(14) O1 0.0269(13) 0.0397(17) 0.0404(15) 0.0022(13) 0.0099(11) 0.0010(12) O2 0.0312(13) 0.0264(14) 0.0321(13) 0.0000(11) 0.0090(11) 0.0012(11) O3 0.0252(13) 0.0374(16) 0.0358(14) -0.0013(12) 0.0044(11) -0.0034(12) O4 0.0323(14) 0.0364(16) 0.0369(15) 0.0060(12) 0.0131(12) 0.0015(12) C1 0.0274(19) 0.049(3) 0.038(2) 0.0049(19) 0.0088(16) 0.0116(18) C2 0.038(2) 0.049(3) 0.048(2) 0.012(2) 0.0114(19) 0.021(2) C3 0.049(3) 0.039(2) 0.043(2) 0.0086(19) 0.0115(19) 0.017(2) C4 0.040(2) 0.029(2) 0.038(2) 0.0024(17) 0.0077(17) 0.0070(17) C5 0.0292(18) 0.0278(19) 0.0284(18) -0.0014(15) 0.0035(14) 0.0041(15) C6 0.0306(18) 0.0220(18) 0.0314(18) 0.0028(15) 0.0024(15) -0.0013(15) C7 0.036(2) 0.029(2) 0.045(2) -0.0059(18) 0.0044(18) -0.0011(17) C8 0.052(3) 0.032(2) 0.053(3) -0.006(2) 0.005(2) -0.012(2) C9 0.040(2) 0.038(2) 0.046(2) 0.0003(19) 0.0071(19) -0.0120(19) C10 0.0295(19) 0.036(2) 0.038(2) 0.0036(17) 0.0070(16) -0.0053(17) C11 0.0317(19) 0.029(2) 0.035(2) 0.0012(16) 0.0116(16) 0.0039(16) C12 0.039(2) 0.029(2) 0.035(2) -0.0001(16) 0.0123(16) 0.0045(17) C13 0.038(2) 0.035(2) 0.0316(19) -0.0044(17) 0.0030(16) 0.0007(18) C14 0.0297(18) 0.032(2) 0.0334(19) 0.0027(16) 0.0046(15) 0.0026(16) C15 0.0261(17) 0.0217(17) 0.0281(18) 0.0011(14) 0.0046(14) 0.0013(14) C16 0.0224(16) 0.0245(18) 0.0324(18) 0.0001(15) 0.0054(14) 0.0001(14) C17 0.0296(18) 0.032(2) 0.036(2) 0.0038(16) 0.0093(16) 0.0049(16) C18 0.037(2) 0.039(2) 0.041(2) 0.0101(19) 0.0064(17) 0.0133(19) C19 0.033(2) 0.040(2) 0.050(2) 0.002(2) 0.0120(18) 0.0119(18) C20 0.0282(18) 0.034(2) 0.039(2) 0.0019(17) 0.0109(16) 0.0064(16) C21 0.0278(18) 0.043(2) 0.035(2) -0.0051(18) 0.0088(16) -0.0088(17) C22 0.039(2) 0.059(3) 0.064(3) 0.002(3) 0.029(2) 0.000(2) C23 0.0326(19) 0.030(2) 0.0318(19) -0.0010(16) 0.0084(15) -0.0047(16) C24 0.045(2) 0.033(2) 0.043(2) 0.0056(18) 0.0178(19) -0.0022(19) C25 0.049(2) 0.030(2) 0.050(2) 0.0086(19) 0.018(2) 0.0087(19) C26 0.040(2) 0.030(2) 0.045(2) 0.0036(18) 0.0180(18) 0.0057(18) C27 0.0261(17) 0.0262(19) 0.0329(18) -0.0014(15) 0.0077(14) -0.0014(15) C28 0.0282(18) 0.0230(18) 0.0330(19) 0.0007(15) 0.0066(15) 0.0029(15) C29 0.049(2) 0.032(2) 0.045(2) -0.0062(19) 0.019(2) -0.0083(19) C30 0.035(2) 0.051(3) 0.040(2) -0.006(2) -0.0004(18) -0.010(2) C31 0.0288(18) 0.0260(19) 0.0340(19) -0.0003(16) 0.0057(15) 0.0021(15) C32 0.0285(18) 0.0258(18) 0.0274(17) -0.0013(15) 0.0056(14) 0.0000(15) C33 0.0323(19) 0.034(2) 0.033(2) -0.0017(17) 0.0052(16) 0.0019(17) C34 0.045(2) 0.030(2) 0.035(2) 0.0039(17) 0.0016(17) 0.0052(18) C35 0.041(2) 0.031(2) 0.036(2) 0.0035(17) 0.0087(17) -0.0045(18) C36 0.0348(19) 0.0253(19) 0.0295(18) -0.0033(15) 0.0063(15) -0.0044(16) C37 0.0332(19) 0.030(2) 0.035(2) -0.0038(16) 0.0092(16) -0.0088(16) C38 0.039(2) 0.054(3) 0.046(2) 0.004(2) 0.0156(19) -0.007(2) C39 0.077(4) 0.076(5) 0.064(4) 0.019(3) 0.001(3) 0.012(4) C40 0.101(5) 0.059(4) 0.062(4) -0.001(3) 0.019(4) 0.007(4) C41 0.087(5) 0.058(4) 0.065(4) 0.011(3) 0.021(3) 0.031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.957(3) . ? Ni1 N8 2.017(3) . ? Ni1 N1 2.053(3) . ? Ni1 O3 2.075(3) . ? Ni1 N4 2.094(3) . ? Ni1 Ni2 2.4053(6) . ? Ni2 N2 1.884(3) . ? Ni2 N5 1.886(3) . ? Ni2 N10 1.900(3) . ? Ni2 N9 1.908(3) . ? Ni2 Ni3 2.4018(6) . ? Ni3 O4 1.957(3) . ? Ni3 N11 2.022(3) . ? Ni3 N6 2.063(3) . ? Ni3 O2 2.070(3) . ? Ni3 N3 2.091(3) . ? N1 C1 1.355(5) . ? N1 C5 1.364(5) . ? N2 C5 1.381(5) . ? N2 C6 1.385(5) . ? N3 C10 1.354(5) . ? N3 C6 1.357(5) . ? N4 C11 1.349(5) . ? N4 C15 1.361(5) . ? N5 C15 1.375(5) . ? N5 C16 1.376(5) . ? N6 C20 1.353(5) . ? N6 C16 1.369(5) . ? N7 C21 1.316(6) . ? N7 C23 1.378(5) . ? N8 C23 1.354(5) . ? N8 C27 1.362(5) . ? N9 C28 1.348(5) . ? N9 C27 1.400(5) . ? N10 C31 1.343(5) . ? N10 C32 1.411(5) . ? N11 C36 1.358(5) . ? N11 C32 1.362(5) . ? N12 C37 1.305(5) . ? N12 C36 1.386(5) . ? O1 C21 1.285(5) . ? O2 C28 1.262(4) . ? O3 C31 1.252(5) . ? O4 C37 1.285(5) . ? C1 C2 1.383(7) . ? C1 H1A 0.9500 . ? C2 C3 1.385(7) . ? C2 H2A 0.9500 . ? C3 C4 1.376(6) . ? C3 H3A 0.9500 . ? C4 C5 1.399(6) . ? C4 H4A 0.9500 . ? C6 C7 1.408(6) . ? C7 C8 1.371(6) . ? C7 H7A 0.9500 . ? C8 C9 1.396(7) . ? C8 H8A 0.9500 . ? C9 C10 1.372(6) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.370(6) . ? C11 H11A 0.9500 . ? C12 C13 1.390(6) . ? C12 H12A 0.9500 . ? C13 C14 1.378(6) . ? C13 H13A 0.9500 . ? C14 C15 1.408(5) . ? C14 H14A 0.9500 . ? C16 C17 1.398(5) . ? C17 C18 1.381(5) . ? C17 H17A 0.9500 . ? C18 C19 1.403(6) . ? C18 H18A 0.9500 . ? C19 C20 1.361(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.510(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.414(6) . ? C24 C25 1.367(6) . ? C24 H24A 0.9500 . ? C25 C26 1.381(6) . ? C25 H25A 0.9500 . ? C26 C27 1.384(6) . ? C26 H26A 0.9500 . ? C28 C29 1.511(6) . ? C29 H29A 0.9601 . ? C29 H29B 0.9601 . ? C29 H29C 0.9599 . ? C30 C31 1.515(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C32 C33 1.382(5) . ? C33 C34 1.383(6) . ? C33 H33A 0.9500 . ? C34 C35 1.376(6) . ? C34 H34A 0.9500 . ? C35 C36 1.394(6) . ? C35 H35A 0.9500 . ? C37 C38 1.512(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C41 1.371(10) 3_776 ? C39 C40 1.386(9) . ? C39 H39A 0.9500 . ? C40 C41 1.356(9) . ? C40 H40A 0.9500 . ? C41 C39 1.371(10) 3_776 ? C41 H41A 0.9500 . ? C42 C47 1.237(17) . ? C42 C43 1.409(9) . ? C42 H42A 0.9500 . ? C43 C44 1.395(9) . ? C43 H43A 0.9500 . ? C44 C45 1.389(9) . ? C44 H44A 0.9500 . ? C45 C46 1.391(9) . ? C45 H45A 0.9500 . ? C46 C47 1.398(9) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 C49 1.449(14) . ? C48 H48A 0.9801 . ? C48 H48B 0.9800 . ? C48 H48C 0.9799 . ? C49 O5 1.426(8) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? O5 C50 1.445(8) . ? C50 C51 1.459(9) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 H51D 0.9599 . ? C51 H51A 0.9600 . ? C51 H51B 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 O1 Ni1 N8 92.29(13) . . ? O1 Ni1 N1 97.46(13) . . ? N8 Ni1 N1 169.77(13) . . ? O1 Ni1 O3 98.22(11) . . ? N8 Ni1 O3 88.53(12) . . ? N1 Ni1 O3 87.01(12) . . ? O1 Ni1 N4 97.01(12) . . ? N8 Ni1 N4 91.97(12) . . ? N1 Ni1 N4 89.92(13) . . ? O3 Ni1 N4 164.72(12) . . ? O1 Ni1 Ni2 179.38(10) . . ? N8 Ni1 Ni2 88.18(9) . . ? N1 Ni1 Ni2 82.09(9) . . ? O3 Ni1 Ni2 82.19(7) . . ? N4 Ni1 Ni2 82.57(9) . . ? N2 Ni2 N5 90.87(14) . . ? N2 Ni2 N10 88.39(13) . . ? N5 Ni2 N10 178.45(13) . . ? N2 Ni2 N9 178.54(13) . . ? N5 Ni2 N9 89.51(14) . . ? N10 Ni2 N9 91.26(13) . . ? N2 Ni2 Ni3 92.25(9) . . ? N5 Ni2 Ni3 90.77(10) . . ? N10 Ni2 Ni3 87.89(10) . . ? N9 Ni2 Ni3 89.16(9) . . ? N2 Ni2 Ni1 91.57(9) . . ? N5 Ni2 Ni1 91.40(10) . . ? N10 Ni2 Ni1 89.98(10) . . ? N9 Ni2 Ni1 87.01(9) . . ? Ni3 Ni2 Ni1 175.57(3) . . ? O4 Ni3 N11 92.35(12) . . ? O4 Ni3 N6 97.75(12) . . ? N11 Ni3 N6 169.82(13) . . ? O4 Ni3 O2 96.11(11) . . ? N11 Ni3 O2 88.88(12) . . ? N6 Ni3 O2 88.83(12) . . ? O4 Ni3 N3 99.08(12) . . ? N11 Ni3 N3 89.73(12) . . ? N6 Ni3 N3 89.87(13) . . ? O2 Ni3 N3 164.79(11) . . ? O4 Ni3 Ni2 178.90(9) . . ? N11 Ni3 Ni2 87.01(9) . . ? N6 Ni3 Ni2 82.87(8) . . ? O2 Ni3 Ni2 82.98(7) . . ? N3 Ni3 Ni2 81.81(9) . . ? C1 N1 C5 118.8(4) . . ? C1 N1 Ni1 117.6(3) . . ? C5 N1 Ni1 123.3(2) . . ? C5 N2 C6 123.0(3) . . ? C5 N2 Ni2 118.1(2) . . ? C6 N2 Ni2 118.7(2) . . ? C10 N3 C6 118.5(3) . . ? C10 N3 Ni3 119.3(3) . . ? C6 N3 Ni3 122.2(2) . . ? C11 N4 C15 118.3(3) . . ? C11 N4 Ni1 120.3(3) . . ? C15 N4 Ni1 121.1(2) . . ? C15 N5 C16 122.5(3) . . ? C15 N5 Ni2 118.3(2) . . ? C16 N5 Ni2 119.1(2) . . ? C20 N6 C16 118.1(3) . . ? C20 N6 Ni3 119.6(3) . . ? C16 N6 Ni3 122.1(2) . . ? C21 N7 C23 125.1(4) . . ? C23 N8 C27 119.8(3) . . ? C23 N8 Ni1 121.3(3) . . ? C27 N8 Ni1 118.4(3) . . ? C28 N9 C27 122.1(3) . . ? C28 N9 Ni2 118.3(3) . . ? C27 N9 Ni2 119.5(2) . . ? C31 N10 C32 123.5(3) . . ? C31 N10 Ni2 118.1(3) . . ? C32 N10 Ni2 118.0(2) . . ? C36 N11 C32 118.9(3) . . ? C36 N11 Ni3 120.8(3) . . ? C32 N11 Ni3 119.3(2) . . ? C37 N12 C36 125.6(3) . . ? C21 O1 Ni1 122.3(3) . . ? C28 O2 Ni3 119.7(2) . . ? C31 O3 Ni1 119.8(2) . . ? C37 O4 Ni3 122.0(3) . . ? N1 C1 C2 123.0(4) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 118.1(4) . . ? C1 C2 H2A 121.0 . . ? C3 C2 H2A 121.0 . . ? C4 C3 C2 119.8(4) . . ? C4 C3 H3A 120.1 . . ? C2 C3 H3A 120.1 . . ? C3 C4 C5 120.1(4) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? N1 C5 N2 114.4(3) . . ? N1 C5 C4 120.2(4) . . ? N2 C5 C4 125.2(4) . . ? N3 C6 N2 115.3(3) . . ? N3 C6 C7 120.3(4) . . ? N2 C6 C7 124.3(4) . . ? C8 C7 C6 120.0(4) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 119.5(4) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C10 C9 C8 117.9(4) . . ? C10 C9 H9A 121.1 . . ? C8 C9 H9A 121.1 . . ? N3 C10 C9 123.7(4) . . ? N3 C10 H10A 118.1 . . ? C9 C10 H10A 118.1 . . ? N4 C11 C12 123.3(4) . . ? N4 C11 H11A 118.3 . . ? C12 C11 H11A 118.3 . . ? C11 C12 C13 118.8(4) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C14 C13 C12 119.3(4) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C15 119.4(4) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? N4 C15 N5 115.8(3) . . ? N4 C15 C14 120.9(3) . . ? N5 C15 C14 123.2(3) . . ? N6 C16 N5 114.4(3) . . ? N6 C16 C17 121.1(3) . . ? N5 C16 C17 124.3(3) . . ? C18 C17 C16 119.4(4) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 119.3(4) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? C20 C19 C18 118.4(4) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? N6 C20 C19 123.8(4) . . ? N6 C20 H20A 118.1 . . ? C19 C20 H20A 118.1 . . ? O1 C21 N7 130.4(4) . . ? O1 C21 C22 114.8(4) . . ? N7 C21 C22 114.8(4) . . ? 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 . . ? N8 C23 N7 125.2(4) . . ? N8 C23 C24 119.3(4) . . ? N7 C23 C24 115.5(4) . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 119.8(4) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C25 C26 C27 118.6(4) . . ? C25 C26 H26A 120.7 . . ? C27 C26 H26A 120.7 . . ? N8 C27 C26 121.7(4) . . ? N8 C27 N9 115.8(3) . . ? C26 C27 N9 122.3(3) . . ? O2 C28 N9 120.2(3) . . ? O2 C28 C29 116.6(3) . . ? N9 C28 C29 123.0(3) . . ? C28 C29 H29A 109.6 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.4 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 C31 N10 120.9(3) . . ? O3 C31 C30 116.7(4) . . ? N10 C31 C30 122.3(4) . . ? N11 C32 C33 122.1(4) . . ? N11 C32 N10 114.9(3) . . ? C33 C32 N10 122.8(3) . . ? C32 C33 C34 118.6(4) . . ? C32 C33 H33A 120.7 . . ? C34 C33 H33A 120.7 . . ? C35 C34 C33 119.6(4) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 120.1(4) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? N11 C36 N12 124.2(3) . . ? N11 C36 C35 120.4(4) . . ? N12 C36 C35 115.4(3) . . ? O4 C37 N12 130.9(4) . . ? O4 C37 C38 113.3(4) . . ? N12 C37 C38 115.8(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 C39 C40 119.7(7) 3_776 . ? C41 C39 H39A 120.2 3_776 . ? C40 C39 H39A 120.2 . . ? C41 C40 C39 119.0(6) . . ? C41 C40 H40A 120.5 . . ? C39 C40 H40A 120.5 . . ? C40 C41 C39 121.3(6) . 3_776 ? C40 C41 H41A 119.3 . . ? C39 C41 H41A 119.3 3_776 . ? C47 C42 C43 116.7(12) . . ? C47 C42 H42A 121.7 . . ? C43 C42 H42A 121.7 . . ? C44 C43 C42 119.6(11) . . ? C44 C43 H43A 120.2 . . ? C42 C43 H43A 120.2 . . ? C45 C44 C43 120.2(11) . . ? C45 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? C44 C45 C46 118.4(11) . . ? C44 C45 H45A 120.8 . . ? C46 C45 H45A 120.8 . . ? C45 C46 C47 115.8(12) . . ? C45 C46 H46A 122.1 . . ? C47 C46 H46A 122.1 . . ? C42 C47 C46 128.5(14) . . ? C42 C47 H47A 115.8 . . ? C46 C47 H47A 115.8 . . ? C49 C48 H48A 94.9 . . ? C49 C48 H48B 119.4 . . ? H48A C48 H48B 109.5 . . ? C49 C48 H48C 113.0 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O5 C49 C48 100.8(7) . . ? O5 C49 H49A 111.6 . . ? C48 C49 H49A 111.6 . . ? O5 C49 H49B 111.6 . . ? C48 C49 H49B 111.6 . . ? H49A C49 H49B 109.4 . . ? C49 O5 C50 112.2(8) . . ? O5 C50 C51 129.6(11) . . ? O5 C50 H50A 104.9 . . ? C51 C50 H50A 104.9 . . ? O5 C50 H50B 104.9 . . ? C51 C50 H50B 104.9 . . ? H50A C50 H50B 105.8 . . ? C50 C51 H51D 109.9 . . ? C50 C51 H51A 108.7 . . ? H51D C51 H51A 109.5 . . ? C50 C51 H51B 109.8 . . ? H51D C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.656 _refine_diff_density_min -1.753 _refine_diff_density_rms 0.222 #===END data_ic11175(comp4) _database_code_depnum_ccdc_archive 'CCDC 618766' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72.61 H75.42 N18.20 Ni3 O11.20 S4' _chemical_formula_weight 1686.66 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.4817(3) _cell_length_b 14.3337(2) _cell_length_c 23.9519(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.0642(6) _cell_angle_gamma 90.00 _cell_volume 7784.68(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.641 _exptl_absorpt_correction_T_max 0.845 _exptl_absorpt_process_details ? _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41752 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8934 _reflns_number_gt 6809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1398P)^2^+26.2076P] 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 8934 _refine_ls_number_parameters 466 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2328 _refine_ls_wR_factor_gt 0.2147 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.20504(5) 0.2500 0.0348(2) Uani 1 2 d S . . Ni2 Ni 0.0000 0.36958(5) 0.2500 0.02764(19) Uani 1 2 d S . . Ni3 Ni 0.0000 0.53635(5) 0.2500 0.0283(2) Uani 1 2 d S . . S1 S -0.05964(6) 0.11179(8) 0.13998(5) 0.0472(3) Uani 1 1 d . . . S2 S 0.07198(5) 0.59024(8) 0.15368(5) 0.0422(3) Uani 1 1 d . . . O1 O -0.05730(18) 0.0514(2) 0.18847(17) 0.0592(10) Uani 1 1 d . . . O2 O -0.02757(17) 0.0829(3) 0.09915(17) 0.0649(11) Uani 1 1 d . . . O3 O 0.0493(2) 0.6245(3) 0.09520(16) 0.0630(11) Uani 1 1 d . . . O4 O 0.08918(15) 0.6603(2) 0.19766(15) 0.0458(8) Uani 1 1 d . . . N1 N 0.07511(16) 0.2138(2) 0.23294(15) 0.0385(8) Uani 1 1 d . . . N2 N 0.08257(15) 0.3677(2) 0.26473(15) 0.0329(7) Uani 1 1 d . . . N3 N 0.08527(14) 0.5201(2) 0.29702(14) 0.0318(7) Uani 1 1 d . . . N4 N 0.08364(16) 0.6753(3) 0.33090(16) 0.0388(8) Uani 1 1 d . . . H4B H 0.0945 0.7045 0.3643 0.047 Uiso 1 1 calc R . . N5 N 0.0000 0.6754(3) 0.2500 0.0310(10) Uani 1 2 d S . . N6 N -0.03818(16) 0.2121(2) 0.16937(15) 0.0388(8) Uani 1 1 d . . . N7 N -0.00830(15) 0.3667(2) 0.16698(14) 0.0317(7) Uani 1 1 d . . . N8 N 0.02833(15) 0.5183(3) 0.17410(14) 0.0350(7) Uani 1 1 d . . . C1 C 0.0958(2) 0.1393(3) 0.2092(2) 0.0486(12) Uani 1 1 d . . . H1A H 0.0717 0.0853 0.2003 0.058 Uiso 1 1 calc R . . C2 C 0.1496(3) 0.1384(4) 0.1977(2) 0.0598(15) Uani 1 1 d . . . H2A H 0.1634 0.0846 0.1821 0.072 Uiso 1 1 calc R . . C3 C 0.1838(3) 0.2189(4) 0.2095(3) 0.0583(14) Uani 1 1 d . . . H3A H 0.2215 0.2206 0.2019 0.070 Uiso 1 1 calc R . . C4 C 0.1632(2) 0.2953(4) 0.2319(2) 0.0476(11) Uani 1 1 d . . . H4A H 0.1864 0.3505 0.2392 0.057 Uiso 1 1 calc R . . C5 C 0.10777(19) 0.2932(3) 0.24431(18) 0.0363(9) Uani 1 1 d . . . C6 C 0.11500(17) 0.4380(3) 0.29774(17) 0.0337(8) Uani 1 1 d . . . C7 C 0.17250(19) 0.4270(3) 0.3330(2) 0.0427(10) Uani 1 1 d . . . H7A H 0.1922 0.3688 0.3348 0.051 Uiso 1 1 calc R . . C8 C 0.1999(2) 0.5021(4) 0.3649(2) 0.0503(12) Uani 1 1 d . . . H8A H 0.2393 0.4960 0.3881 0.060 Uiso 1 1 calc R . . C9 C 0.1708(2) 0.5858(3) 0.3634(2) 0.0479(11) Uani 1 1 d . . . H9A H 0.1896 0.6380 0.3849 0.057 Uiso 1 1 calc R . . C10 C 0.11267(18) 0.5919(3) 0.32935(18) 0.0361(9) Uani 1 1 d . . . C11 C -0.04035(19) 0.7219(3) 0.2106(2) 0.0378(9) Uani 1 1 d . . . C12 C -0.0412(2) 0.8188(3) 0.2086(2) 0.0524(12) Uani 1 1 d . . . H12A H -0.0695 0.8513 0.1795 0.063 Uiso 1 1 calc R . . C13 C 0.0000 0.8661(5) 0.2500 0.057(2) Uani 1 2 d S . . H13A H 0.0000 0.9324 0.2500 0.069 Uiso 1 2 calc SR . . C14 C -0.1343(2) 0.1240(3) 0.1015(2) 0.0454(11) Uani 1 1 d . . . C15 C -0.1754(2) 0.1545(4) 0.1295(2) 0.0557(13) Uani 1 1 d . . . H15A H -0.1635 0.1708 0.1693 0.067 Uiso 1 1 calc R . . C16 C -0.2344(2) 0.1612(4) 0.0987(3) 0.0602(14) Uani 1 1 d . . . H16A H -0.2629 0.1828 0.1174 0.072 Uiso 1 1 calc R . . C17 C -0.2518(3) 0.1364(4) 0.0405(3) 0.0628(16) Uani 1 1 d . . . C18 C -0.3172(3) 0.1427(6) 0.0082(3) 0.084(2) Uani 1 1 d . . . H18A H -0.3210 0.1618 -0.0319 0.126 Uiso 1 1 calc R . . H18B H -0.3367 0.1888 0.0272 0.126 Uiso 1 1 calc R . . H18C H -0.3358 0.0816 0.0087 0.126 Uiso 1 1 calc R . . C19 C -0.2106(3) 0.1054(6) 0.0145(3) 0.085(2) Uani 1 1 d . . . H19A H -0.2228 0.0868 -0.0249 0.102 Uiso 1 1 calc R . . C20 C -0.1515(3) 0.0998(5) 0.0433(3) 0.0741(19) Uani 1 1 d . . . H20A H -0.1232 0.0799 0.0238 0.089 Uiso 1 1 calc R . . C21 C -0.03049(19) 0.2886(3) 0.13632(18) 0.0362(9) Uani 1 1 d . . . C22 C -0.0443(2) 0.2889(4) 0.07520(19) 0.0440(11) Uani 1 1 d . . . H22A H -0.0591 0.2343 0.0539 0.053 Uiso 1 1 calc R . . C23 C -0.0362(2) 0.3689(4) 0.04729(19) 0.0490(12) Uani 1 1 d . . . H23A H -0.0471 0.3705 0.0062 0.059 Uiso 1 1 calc R . . C24 C -0.0123(2) 0.4473(4) 0.07769(19) 0.0436(10) Uani 1 1 d . . . H24A H -0.0065 0.5024 0.0578 0.052 Uiso 1 1 calc R . . C25 C 0.00330(18) 0.4449(3) 0.13838(17) 0.0347(9) Uani 1 1 d . . . C26 C 0.1382(2) 0.5289(4) 0.1551(3) 0.0554(14) Uani 1 1 d . . . C27 C 0.1431(3) 0.4756(5) 0.1078(3) 0.079(2) Uani 1 1 d . . . H27A H 0.1107 0.4688 0.0746 0.095 Uiso 1 1 calc R . . C28 C 0.1974(4) 0.4323(5) 0.1108(4) 0.095(3) Uani 1 1 d . . . H28A H 0.2014 0.3936 0.0799 0.114 Uiso 1 1 calc R . . C29 C 0.2447(4) 0.4447(5) 0.1575(5) 0.102(3) Uani 1 1 d . . . C30 C 0.3038(4) 0.3956(7) 0.1595(6) 0.144(5) Uani 1 1 d . . . H30A H 0.3362 0.4309 0.1846 0.216 Uiso 1 1 calc R . . H30B H 0.3093 0.3923 0.1204 0.216 Uiso 1 1 calc R . . H30C H 0.3032 0.3323 0.1749 0.216 Uiso 1 1 calc R . . C31 C 0.2387(3) 0.4951(5) 0.2029(4) 0.080(2) Uani 1 1 d . . . H31A H 0.2712 0.5007 0.2360 0.096 Uiso 1 1 calc R . . C32 C 0.1855(2) 0.5394(4) 0.2025(3) 0.0614(15) Uani 1 1 d . . . H32A H 0.1821 0.5761 0.2345 0.074 Uiso 1 1 calc R . . O5 O 0.1458(2) 0.2237(4) -0.0685(2) 0.0721(16) Uiso 0.879(9) 1 d PD . . N9 N 0.1238(4) 0.2273(7) 0.0151(4) 0.113(3) Uiso 0.879(9) 1 d PD . . C33 C 0.1095(6) 0.2406(12) -0.0452(5) 0.167(6) Uiso 0.879(9) 1 d PD . . H33A H 0.0717 0.2624 -0.0659 0.201 Uiso 0.879(9) 1 calc PR . . C34 C 0.1740(8) 0.1604(13) 0.0397(9) 0.224(9) Uiso 0.879(9) 1 d PD . . H34A H 0.2047 0.1922 0.0691 0.336 Uiso 0.879(9) 1 d PR . . H34B H 0.1906 0.1384 0.0085 0.336 Uiso 0.879(9) 1 d PR . . H34C H 0.1591 0.1070 0.0572 0.336 Uiso 0.879(9) 1 d PR . . C35 C 0.0910(5) 0.2267(9) 0.0589(5) 0.122(4) Uiso 0.879(9) 1 d PD . . H35A H 0.0591 0.2727 0.0486 0.183 Uiso 0.879(9) 1 d PR . . H35B H 0.1175 0.2427 0.0965 0.183 Uiso 0.879(9) 1 d PR . . H35C H 0.0742 0.1646 0.0609 0.183 Uiso 0.879(9) 1 d PR . . O6 O 0.3466(5) 0.4947(8) 0.4200(5) 0.129(4) Uiso 0.722(11) 1 d PD . . N10 N 0.3972(6) 0.3937(8) 0.3856(5) 0.116(4) Uiso 0.722(11) 1 d PD . . C36 C 0.3957(6) 0.4754(10) 0.4187(7) 0.130(5) Uiso 0.722(11) 1 d PD . . H36A H 0.4296 0.5104 0.4376 0.157 Uiso 0.722(11) 1 calc PR . . C37 C 0.3366(7) 0.3592(18) 0.3693(12) 0.225(12) Uiso 0.722(11) 1 d PD . . H37A H 0.3076 0.4095 0.3577 0.337 Uiso 0.722(11) 1 d PR . . H37B H 0.3287 0.3250 0.4019 0.337 Uiso 0.722(11) 1 d PR . . H37C H 0.3335 0.3165 0.3367 0.337 Uiso 0.722(11) 1 d PR . . C38 C 0.4607(7) 0.3656(19) 0.4042(13) 0.244(13) Uiso 0.722(11) 1 d PD . . H38A H 0.4825 0.4052 0.4360 0.366 Uiso 0.722(11) 1 d PR . . H38B H 0.4770 0.3732 0.3708 0.366 Uiso 0.722(11) 1 d PR . . H38C H 0.4642 0.3002 0.4166 0.366 Uiso 0.722(11) 1 d 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 0.0359(4) 0.0303(4) 0.0290(4) 0.000 -0.0080(3) 0.000 Ni2 0.0266(3) 0.0296(4) 0.0225(3) 0.000 -0.0011(3) 0.000 Ni3 0.0267(3) 0.0290(4) 0.0263(4) 0.000 0.0019(3) 0.000 S1 0.0508(7) 0.0338(6) 0.0419(6) -0.0095(5) -0.0152(5) 0.0090(5) S2 0.0474(6) 0.0426(6) 0.0396(6) 0.0080(5) 0.0166(5) -0.0003(5) O1 0.069(2) 0.0333(17) 0.056(2) -0.0015(15) -0.0202(18) -0.0008(16) O2 0.061(2) 0.061(2) 0.058(2) -0.0244(19) -0.0114(18) 0.0213(19) O3 0.082(3) 0.064(2) 0.0407(19) 0.0175(17) 0.0129(19) -0.012(2) O4 0.0494(18) 0.0408(17) 0.0505(19) 0.0019(14) 0.0188(15) -0.0064(14) N1 0.0400(19) 0.0364(19) 0.0308(18) -0.0024(14) -0.0057(15) 0.0088(15) N2 0.0299(16) 0.0342(18) 0.0311(17) 0.0008(13) 0.0017(13) 0.0024(13) N3 0.0281(16) 0.0336(17) 0.0305(17) 0.0033(13) 0.0021(13) 0.0005(13) N4 0.0395(18) 0.0373(19) 0.0344(18) -0.0052(15) 0.0002(15) -0.0051(16) N5 0.029(2) 0.029(2) 0.033(2) 0.000 0.0042(19) 0.000 N6 0.0403(19) 0.0382(19) 0.0276(17) -0.0042(14) -0.0095(14) 0.0018(15) N7 0.0316(16) 0.0355(18) 0.0238(15) 0.0009(13) -0.0002(13) 0.0077(14) N8 0.0350(17) 0.0404(19) 0.0292(17) 0.0036(14) 0.0076(14) 0.0000(15) C1 0.049(3) 0.044(3) 0.044(3) -0.006(2) -0.005(2) 0.017(2) C2 0.064(3) 0.055(3) 0.054(3) -0.007(2) 0.005(3) 0.027(3) C3 0.053(3) 0.061(3) 0.062(3) 0.001(3) 0.017(3) 0.023(3) C4 0.042(2) 0.049(3) 0.051(3) 0.004(2) 0.011(2) 0.010(2) C5 0.035(2) 0.037(2) 0.031(2) 0.0028(16) -0.0016(16) 0.0063(17) C6 0.0291(19) 0.038(2) 0.031(2) 0.0041(16) 0.0028(15) -0.0020(16) C7 0.030(2) 0.041(2) 0.049(3) 0.005(2) -0.0033(18) 0.0023(18) C8 0.035(2) 0.051(3) 0.053(3) 0.007(2) -0.010(2) -0.003(2) C9 0.042(2) 0.044(3) 0.047(3) 0.000(2) -0.009(2) -0.006(2) C10 0.0314(19) 0.038(2) 0.033(2) 0.0024(17) -0.0019(16) -0.0075(17) C11 0.034(2) 0.035(2) 0.041(2) 0.0017(18) 0.0042(18) 0.0041(17) C12 0.047(3) 0.038(2) 0.060(3) 0.005(2) -0.008(2) 0.007(2) C13 0.055(4) 0.026(3) 0.077(5) 0.000 -0.010(4) 0.000 C14 0.046(3) 0.034(2) 0.042(2) -0.0063(18) -0.014(2) 0.0019(18) C15 0.052(3) 0.057(3) 0.047(3) -0.011(2) -0.007(2) -0.006(2) C16 0.046(3) 0.063(3) 0.061(3) -0.007(3) -0.005(2) -0.004(3) C17 0.049(3) 0.061(3) 0.061(3) 0.002(3) -0.019(3) -0.002(3) C18 0.056(3) 0.096(5) 0.075(4) 0.000(4) -0.027(3) -0.004(3) C19 0.065(4) 0.120(6) 0.051(3) -0.033(4) -0.022(3) 0.006(4) C20 0.058(3) 0.096(5) 0.050(3) -0.033(3) -0.017(3) 0.007(3) C21 0.036(2) 0.038(2) 0.028(2) -0.0043(16) -0.0031(16) 0.0063(17) C22 0.041(2) 0.054(3) 0.029(2) -0.0082(19) -0.0041(18) 0.001(2) C23 0.046(3) 0.074(3) 0.023(2) 0.004(2) 0.0024(18) 0.004(2) C24 0.045(2) 0.054(3) 0.029(2) 0.0050(19) 0.0049(18) 0.001(2) C25 0.034(2) 0.042(2) 0.0279(19) 0.0020(16) 0.0063(16) 0.0045(17) C26 0.057(3) 0.048(3) 0.076(4) 0.003(3) 0.043(3) -0.005(2) C27 0.081(4) 0.083(4) 0.093(5) -0.023(4) 0.058(4) -0.021(4) C28 0.100(6) 0.074(5) 0.143(8) -0.029(5) 0.087(6) -0.015(4) C29 0.065(4) 0.065(4) 0.199(11) -0.001(5) 0.078(6) -0.007(4) C30 0.075(5) 0.103(7) 0.287(17) -0.019(8) 0.106(8) 0.004(5) C31 0.049(3) 0.059(4) 0.140(7) 0.000(4) 0.038(4) -0.004(3) C32 0.046(3) 0.053(3) 0.088(4) 0.003(3) 0.022(3) -0.004(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 N6 1.909(3) 2 ? Ni1 N6 1.909(3) . ? Ni1 N1 1.915(4) 2 ? Ni1 N1 1.915(4) . ? Ni1 Ni2 2.3585(10) . ? Ni2 N2 1.878(3) . ? Ni2 N2 1.878(3) 2 ? Ni2 N7 1.947(3) 2 ? Ni2 N7 1.947(3) . ? Ni2 Ni3 2.3904(9) . ? Ni3 N5 1.994(5) . ? Ni3 N3 2.039(3) 2 ? Ni3 N3 2.039(3) . ? Ni3 N8 2.108(3) 2 ? Ni3 N8 2.108(3) . ? S1 O1 1.438(4) . ? S1 O2 1.442(4) . ? S1 N6 1.622(4) . ? S1 C14 1.764(5) . ? S2 O4 1.435(4) . ? S2 O3 1.449(4) . ? S2 N8 1.617(4) . ? S2 C26 1.778(5) . ? N1 C1 1.358(6) . ? N1 C5 1.359(6) . ? N2 C5 1.371(5) . ? N2 C6 1.382(5) . ? N3 C10 1.348(5) . ? N3 C6 1.365(5) . ? N4 C10 1.381(6) . ? N4 C11 1.393(6) 2 ? N4 H4B 0.8800 . ? N5 C11 1.329(5) 2 ? N5 C11 1.329(5) . ? N6 C21 1.392(6) . ? N7 C21 1.366(5) . ? N7 C25 1.377(5) . ? N8 C25 1.388(5) . ? C1 C2 1.361(8) . ? C1 H1A 0.9500 . ? C2 C3 1.391(9) . ? C2 H2A 0.9500 . ? C3 C4 1.362(7) . ? C3 H3A 0.9500 . ? C4 C5 1.409(7) . ? C4 H4A 0.9500 . ? C6 C7 1.403(6) . ? C7 C8 1.379(7) . ? C7 H7A 0.9500 . ? C8 C9 1.378(7) . ? C8 H8A 0.9500 . ? C9 C10 1.398(6) . ? C9 H9A 0.9500 . ? C11 C12 1.390(7) . ? C11 N4 1.393(6) 2 ? C12 C13 1.372(6) . ? C12 H12A 0.9500 . ? C13 C12 1.372(6) 2 ? C13 H13A 0.9500 . ? C14 C15 1.381(8) . ? C14 C20 1.392(7) . ? C15 C16 1.395(7) . ? C15 H15A 0.9500 . ? C16 C17 1.392(8) . ? C16 H16A 0.9500 . ? C17 C19 1.354(10) . ? C17 C18 1.533(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.384(8) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.415(6) . ? C22 C23 1.366(7) . ? C22 H22A 0.9500 . ? C23 C24 1.376(7) . ? C23 H23A 0.9500 . ? C24 C25 1.404(6) . ? C24 H24A 0.9500 . ? C26 C32 1.375(9) . ? C26 C27 1.397(9) . ? C27 C28 1.403(11) . ? C27 H27A 0.9500 . ? C28 C29 1.367(14) . ? C28 H28A 0.9500 . ? C29 C31 1.343(12) . ? C29 C30 1.546(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.400(8) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? O5 C33 1.161(9) . ? N9 C33 1.407(9) . ? N9 C35 1.454(8) . ? N9 C34 1.514(9) . ? C33 H33A 0.9500 . ? C34 H34A 0.9799 . ? C34 H34B 0.9799 . ? C34 H34C 0.9802 . ? C35 H35A 0.9799 . ? C35 H35B 0.9801 . ? C35 H35C 0.9800 . ? O6 C36 1.193(9) . ? N10 C36 1.421(9) . ? N10 C37 1.462(10) . ? N10 C38 1.495(10) . ? C36 H36A 0.9500 . ? C37 H37A 0.9798 . ? C37 H37B 0.9798 . ? C37 H37C 0.9801 . ? C38 H38A 0.9801 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ni1 N6 174.0(2) 2 . ? N6 Ni1 N1 89.83(16) 2 2 ? N6 Ni1 N1 89.77(16) . 2 ? N6 Ni1 N1 89.77(16) 2 . ? N6 Ni1 N1 89.83(16) . . ? N1 Ni1 N1 172.5(2) 2 . ? N6 Ni1 Ni2 86.98(11) 2 . ? N6 Ni1 Ni2 86.98(11) . . ? N1 Ni1 Ni2 86.24(11) 2 . ? N1 Ni1 Ni2 86.24(11) . . ? N2 Ni2 N2 178.3(2) . 2 ? N2 Ni2 N7 89.05(15) . 2 ? N2 Ni2 N7 90.91(15) 2 2 ? N2 Ni2 N7 90.91(15) . . ? N2 Ni2 N7 89.05(15) 2 . ? N7 Ni2 N7 177.6(2) 2 . ? N2 Ni2 Ni1 89.16(10) . . ? N2 Ni2 Ni1 89.16(10) 2 . ? N7 Ni2 Ni1 88.79(10) 2 . ? N7 Ni2 Ni1 88.79(10) . . ? N2 Ni2 Ni3 90.84(10) . . ? N2 Ni2 Ni3 90.84(10) 2 . ? N7 Ni2 Ni3 91.21(10) 2 . ? N7 Ni2 Ni3 91.21(10) . . ? Ni1 Ni2 Ni3 180.0 . . ? N5 Ni3 N3 96.57(10) . 2 ? N5 Ni3 N3 96.57(10) . . ? N3 Ni3 N3 166.9(2) 2 . ? N5 Ni3 N8 97.04(10) . 2 ? N3 Ni3 N8 88.72(13) 2 2 ? N3 Ni3 N8 89.67(13) . 2 ? N5 Ni3 N8 97.04(10) . . ? N3 Ni3 N8 89.67(13) 2 . ? N3 Ni3 N8 88.72(13) . . ? N8 Ni3 N8 165.9(2) 2 . ? N5 Ni3 Ni2 180.000(1) . . ? N3 Ni3 Ni2 83.43(10) 2 . ? N3 Ni3 Ni2 83.43(10) . . ? N8 Ni3 Ni2 82.96(10) 2 . ? N8 Ni3 Ni2 82.96(10) . . ? O1 S1 O2 117.2(2) . . ? O1 S1 N6 103.9(2) . . ? O2 S1 N6 113.0(2) . . ? O1 S1 C14 107.8(3) . . ? O2 S1 C14 107.3(2) . . ? N6 S1 C14 107.0(2) . . ? O4 S2 O3 115.8(2) . . ? O4 S2 N8 107.66(19) . . ? O3 S2 N8 113.9(2) . . ? O4 S2 C26 104.7(3) . . ? O3 S2 C26 106.6(3) . . ? N8 S2 C26 107.4(2) . . ? C1 N1 C5 119.8(4) . . ? C1 N1 Ni1 119.2(3) . . ? C5 N1 Ni1 121.0(3) . . ? C5 N2 C6 123.2(3) . . ? C5 N2 Ni2 117.7(3) . . ? C6 N2 Ni2 119.0(3) . . ? C10 N3 C6 119.0(3) . . ? C10 N3 Ni3 118.9(3) . . ? C6 N3 Ni3 122.1(3) . . ? C10 N4 C11 132.0(4) . 2 ? C10 N4 H4B 114.0 . . ? C11 N4 H4B 114.0 2 . ? C11 N5 C11 119.9(5) 2 . ? C11 N5 Ni3 120.1(3) 2 . ? C11 N5 Ni3 120.1(3) . . ? C21 N6 S1 121.6(3) . . ? C21 N6 Ni1 121.4(3) . . ? S1 N6 Ni1 113.8(2) . . ? C21 N7 C25 119.8(3) . . ? C21 N7 Ni2 119.3(3) . . ? C25 N7 Ni2 120.7(3) . . ? C25 N8 S2 119.8(3) . . ? C25 N8 Ni3 116.5(3) . . ? S2 N8 Ni3 123.4(2) . . ? N1 C1 C2 123.0(5) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 117.9(5) . . ? C1 C2 H2A 121.1 . . ? C3 C2 H2A 121.1 . . ? C4 C3 C2 120.1(5) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 120.5(5) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? N1 C5 N2 116.7(4) . . ? N1 C5 C4 118.7(4) . . ? N2 C5 C4 124.5(4) . . ? N3 C6 N2 114.7(3) . . ? N3 C6 C7 120.9(4) . . ? N2 C6 C7 124.3(4) . . ? C8 C7 C6 119.0(4) . . ? C8 C7 H7A 120.5 . . ? C6 C7 H7A 120.5 . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 118.2(4) . . ? C8 C9 H9A 120.9 . . ? C10 C9 H9A 120.9 . . ? N3 C10 N4 120.8(4) . . ? N3 C10 C9 122.3(4) . . ? N4 C10 C9 116.9(4) . . ? N5 C11 C12 121.8(4) . . ? N5 C11 N4 121.3(4) . 2 ? C12 C11 N4 116.9(4) . 2 ? C13 C12 C11 117.9(5) . . ? C13 C12 H12A 121.1 . . ? C11 C12 H12A 121.1 . . ? C12 C13 C12 120.8(6) 2 . ? C12 C13 H13A 119.6 2 . ? C12 C13 H13A 119.6 . . ? C15 C14 C20 120.6(5) . . ? C15 C14 S1 120.2(4) . . ? C20 C14 S1 119.2(4) . . ? C14 C15 C16 119.2(5) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C17 C16 C15 120.3(6) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C19 C17 C16 119.2(5) . . ? C19 C17 C18 121.9(6) . . ? C16 C17 C18 118.9(6) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 C20 122.2(6) . . ? C17 C19 H19A 118.9 . . ? C20 C19 H19A 118.9 . . ? C19 C20 C14 118.5(6) . . ? C19 C20 H20A 120.7 . . ? C14 C20 H20A 120.7 . . ? N7 C21 N6 115.3(3) . . ? N7 C21 C22 120.5(4) . . ? N6 C21 C22 124.2(4) . . ? C23 C22 C21 119.0(4) . . ? C23 C22 H22A 120.5 . . ? C21 C22 H22A 120.5 . . ? C22 C23 C24 121.1(4) . . ? C22 C23 H23A 119.5 . . ? C24 C23 H23A 119.5 . . ? C23 C24 C25 119.3(4) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? N7 C25 N8 114.7(3) . . ? N7 C25 C24 120.2(4) . . ? N8 C25 C24 125.1(4) . . ? C32 C26 C27 120.8(6) . . ? C32 C26 S2 118.4(4) . . ? C27 C26 S2 120.7(5) . . ? C26 C27 C28 117.7(8) . . ? C26 C27 H27A 121.2 . . ? C28 C27 H27A 121.2 . . ? C29 C28 C27 121.3(7) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C31 C29 C28 120.0(7) . . ? C31 C29 C30 120.1(10) . . ? C28 C29 C30 119.8(9) . . ? 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 . . ? C29 C31 C32 121.3(8) . . ? C29 C31 H31A 119.4 . . ? C32 C31 H31A 119.4 . . ? C26 C32 C31 118.9(7) . . ? C26 C32 H32A 120.5 . . ? C31 C32 H32A 120.5 . . ? C33 N9 C35 135.3(10) . . ? C33 N9 C34 116.1(12) . . ? C35 N9 C34 102.7(12) . . ? O5 C33 N9 117.2(12) . . ? O5 C33 H33A 121.4 . . ? N9 C33 H33A 121.4 . . ? N9 C34 H34A 109.7 . . ? N9 C34 H34B 109.2 . . ? H34A C34 H34B 109.5 . . ? N9 C34 H34C 109.4 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N9 C35 H35A 109.1 . . ? N9 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N9 C35 H35C 109.7 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C36 N10 C37 105.3(15) . . ? C36 N10 C38 102.9(15) . . ? C37 N10 C38 144.6(18) . . ? O6 C36 N10 111.7(13) . . ? O6 C36 H36A 124.1 . . ? N10 C36 H36A 124.1 . . ? N10 C37 H37A 112.5 . . ? N10 C37 H37B 109.1 . . ? H37A C37 H37B 109.5 . . ? N10 C37 H37C 106.7 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N10 C38 H38A 110.9 . . ? N10 C38 H38B 107.3 . . ? H38A C38 H38B 109.5 . . ? N10 C38 H38C 110.2 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.020 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.288 #===END data_ic10979(comp5) _database_code_depnum_ccdc_archive 'CCDC 618767' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H54 B Cl4 F4 N12 Ni3 O8 S4' _chemical_formula_weight 1604.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 12.9703(2) _cell_length_b 15.1127(2) _cell_length_c 19.0513(3) _cell_angle_alpha 82.2079(7) _cell_angle_beta 81.4266(8) _cell_angle_gamma 64.9834(7) _cell_volume 3335.23(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1638 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_process_details ? _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47468 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15158 _reflns_number_gt 10490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1390P)^2^+6.3153P] 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 15158 _refine_ls_number_parameters 856 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2374 _refine_ls_wR_factor_gt 0.2120 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.009 _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 0.75588(6) 0.29321(5) 0.37094(3) 0.02821(17) Uani 1 1 d . . . Ni2 Ni 0.81546(5) 0.29024(4) 0.25052(3) 0.02178(16) Uani 1 1 d . . . Ni3 Ni 0.87485(5) 0.28890(4) 0.13033(3) 0.02187(16) Uani 1 1 d . . . S1 S 0.52724(12) 0.30482(12) 0.41731(7) 0.0419(4) Uani 1 1 d . . . S2 S 0.71984(10) 0.44315(8) 0.03469(6) 0.0250(3) Uani 1 1 d . . . S3 S 1.09999(11) 0.13310(9) 0.08540(6) 0.0285(3) Uani 1 1 d . . . S4 S 0.92154(13) 0.30717(11) 0.46056(7) 0.0396(3) Uani 1 1 d . . . O1 O 0.6039(3) 0.2747(3) 0.47217(19) 0.0458(10) Uani 1 1 d . . . O2 O 0.4252(4) 0.3934(4) 0.4257(2) 0.0540(12) Uani 1 1 d . . . O3 O 0.6364(3) 0.4313(3) -0.00083(17) 0.0306(8) Uani 1 1 d . . . O4 O 0.8368(3) 0.4026(2) 0.00392(17) 0.0289(7) Uani 1 1 d . . . O5 O 1.0278(3) 0.1737(3) 0.02854(18) 0.0339(8) Uani 1 1 d . . . O6 O 1.2073(3) 0.1420(3) 0.07678(19) 0.0373(9) Uani 1 1 d . . . O7 O 0.8074(4) 0.3477(3) 0.49532(19) 0.0431(9) Uani 1 1 d . . . O8 O 1.0065(4) 0.2278(4) 0.4990(2) 0.0554(12) Uani 1 1 d . . . N1 N 0.7057(4) 0.4329(3) 0.3576(2) 0.0333(10) Uani 1 1 d . . . N2 N 0.8204(4) 0.4122(3) 0.2501(2) 0.0268(9) Uani 1 1 d . . . N3 N 0.9345(3) 0.3811(3) 0.1432(2) 0.0254(8) Uani 1 1 d . . . N4 N 0.6113(4) 0.3087(3) 0.3456(2) 0.0330(10) Uani 1 1 d . . . N5 N 0.6580(3) 0.3554(3) 0.2293(2) 0.0234(8) Uani 1 1 d . . . N6 N 0.7287(3) 0.3911(3) 0.1157(2) 0.0242(8) Uani 1 1 d . . . N7 N 0.8108(4) 0.1538(3) 0.3736(2) 0.0306(9) Uani 1 1 d . . . N8 N 0.8115(4) 0.1675(3) 0.2515(2) 0.0263(8) Uani 1 1 d . . . N9 N 0.8109(3) 0.1959(3) 0.1288(2) 0.0239(8) Uani 1 1 d . . . N10 N 0.9060(4) 0.2735(3) 0.3862(2) 0.0325(9) Uani 1 1 d . . . N11 N 0.9725(3) 0.2246(3) 0.2716(2) 0.0246(8) Uani 1 1 d . . . N12 N 1.0162(3) 0.1866(3) 0.1542(2) 0.0253(8) Uani 1 1 d . . . C1 C 0.6272(5) 0.4905(4) 0.4061(3) 0.0422(13) Uani 1 1 d . . . H1A H 0.6003 0.4601 0.4472 0.051 Uiso 1 1 calc R . . C2 C 0.5854(6) 0.5894(5) 0.3984(4) 0.0601(19) Uani 1 1 d . . . H2A H 0.5324 0.6274 0.4344 0.072 Uiso 1 1 calc R . . C3 C 0.6210(7) 0.6346(5) 0.3376(4) 0.0608(19) Uani 1 1 d . . . H3A H 0.5920 0.7041 0.3311 0.073 Uiso 1 1 calc R . . C4 C 0.6992(6) 0.5778(4) 0.2863(3) 0.0450(14) Uani 1 1 d . . . H4A H 0.7226 0.6078 0.2436 0.054 Uiso 1 1 calc R . . C5 C 0.7435(5) 0.4756(4) 0.2982(3) 0.0326(11) Uani 1 1 d . . . C6 C 0.8956(4) 0.4347(3) 0.2011(2) 0.0265(10) Uani 1 1 d . . . C7 C 0.9386(5) 0.5032(4) 0.2083(3) 0.0390(13) Uani 1 1 d . . . H7A H 0.9151 0.5386 0.2496 0.047 Uiso 1 1 calc R . . C8 C 1.0147(5) 0.5194(5) 0.1558(3) 0.0454(14) Uani 1 1 d . . . H8A H 1.0407 0.5685 0.1595 0.054 Uiso 1 1 calc R . . C9 C 1.0540(5) 0.4637(4) 0.0972(3) 0.0392(13) Uani 1 1 d . . . H9A H 1.1076 0.4735 0.0608 0.047 Uiso 1 1 calc R . . C10 C 1.0136(4) 0.3952(4) 0.0934(3) 0.0299(11) Uani 1 1 d . . . H10A H 1.0419 0.3555 0.0543 0.036 Uiso 1 1 calc R . . C11 C 0.4849(5) 0.2102(5) 0.4118(3) 0.0471(16) Uani 1 1 d . . . C12 C 0.3898(7) 0.2083(8) 0.4572(4) 0.075(3) Uani 1 1 d . . . H12A H 0.3434 0.2619 0.4847 0.090 Uiso 1 1 calc R . . C13 C 0.3650(9) 0.1283(11) 0.4610(5) 0.102(4) Uani 1 1 d . . . H13A H 0.3021 0.1261 0.4927 0.123 Uiso 1 1 calc R . . C14 C 0.4302(9) 0.0489(9) 0.4192(5) 0.084(3) Uani 1 1 d . . . C15 C 0.4017(10) -0.0393(9) 0.4265(6) 0.126(5) Uani 1 1 d . . . H15A H 0.4627 -0.0918 0.4005 0.188 Uiso 1 1 d R . . H15B H 0.3292 -0.0213 0.4067 0.188 Uiso 1 1 d R . . H15C H 0.3947 -0.0619 0.4769 0.188 Uiso 1 1 d R . . C16 C 0.5188(7) 0.0546(6) 0.3733(5) 0.073(2) Uani 1 1 d . . . H16A H 0.5625 0.0029 0.3436 0.087 Uiso 1 1 calc R . . C17 C 0.5466(6) 0.1348(6) 0.3692(4) 0.0594(19) Uani 1 1 d . . . H17A H 0.6086 0.1374 0.3368 0.071 Uiso 1 1 calc R . . C18 C 0.5729(4) 0.3563(4) 0.2809(3) 0.0301(11) Uani 1 1 d . . . C19 C 0.4587(5) 0.4029(4) 0.2669(3) 0.0356(12) Uani 1 1 d . . . H19A H 0.3991 0.4029 0.3026 0.043 Uiso 1 1 calc R . . C20 C 0.4346(5) 0.4489(4) 0.2002(3) 0.0361(12) Uani 1 1 d . . . H20A H 0.3571 0.4816 0.1902 0.043 Uiso 1 1 calc R . . C21 C 0.5192(4) 0.4487(4) 0.1478(3) 0.0301(11) Uani 1 1 d . . . H21A H 0.5010 0.4813 0.1021 0.036 Uiso 1 1 calc R . . C22 C 0.6326(4) 0.4000(3) 0.1629(2) 0.0238(9) Uani 1 1 d . . . C23 C 0.6749(4) 0.5694(3) 0.0407(3) 0.0291(10) Uani 1 1 d . . . C24 C 0.5688(5) 0.6356(4) 0.0209(3) 0.0395(13) Uani 1 1 d . . . H24A H 0.5190 0.6134 0.0043 0.047 Uiso 1 1 calc R . . C25 C 0.5371(5) 0.7339(4) 0.0256(4) 0.0520(16) Uani 1 1 d . . . H25A H 0.4644 0.7792 0.0121 0.062 Uiso 1 1 calc R . . C26 C 0.6085(5) 0.7691(4) 0.0495(4) 0.0475(15) Uani 1 1 d . . . C27 C 0.5721(7) 0.8769(5) 0.0539(6) 0.079(3) Uani 1 1 d . . . H27A H 0.6333 0.8876 0.0708 0.119 Uiso 1 1 d R . . H27B H 0.5027 0.9021 0.0870 0.119 Uiso 1 1 d R . . H27C H 0.5566 0.9112 0.0066 0.119 Uiso 1 1 d R . . C28 C 0.7131(5) 0.7024(4) 0.0690(3) 0.0450(14) Uani 1 1 d . . . H28A H 0.7626 0.7249 0.0855 0.054 Uiso 1 1 calc R . . C29 C 0.7481(5) 0.6024(4) 0.0651(3) 0.0361(12) Uani 1 1 d . . . H29A H 0.8207 0.5571 0.0788 0.043 Uiso 1 1 calc R . . C30 C 0.8352(5) 0.0999(4) 0.4371(3) 0.0395(13) Uani 1 1 d . . . H30A H 0.8229 0.1331 0.4786 0.047 Uiso 1 1 calc R . . C31 C 0.8761(6) 0.0014(5) 0.4435(3) 0.0484(15) Uani 1 1 d . . . H31A H 0.8891 -0.0339 0.4889 0.058 Uiso 1 1 calc R . . C32 C 0.8987(6) -0.0477(4) 0.3830(3) 0.0479(15) Uani 1 1 d . . . H32A H 0.9272 -0.1171 0.3865 0.057 Uiso 1 1 calc R . . C33 C 0.8797(5) 0.0051(4) 0.3170(3) 0.0381(12) Uani 1 1 d . . . H33A H 0.8990 -0.0283 0.2749 0.046 Uiso 1 1 calc R . . C34 C 0.8323(4) 0.1069(4) 0.3128(3) 0.0287(10) Uani 1 1 d . . . C35 C 0.7910(4) 0.1429(3) 0.1889(2) 0.0242(9) Uani 1 1 d . . . C36 C 0.7480(4) 0.0733(4) 0.1851(3) 0.0300(11) Uani 1 1 d . . . H36A H 0.7331 0.0369 0.2271 0.036 Uiso 1 1 calc R . . C37 C 0.7275(5) 0.0580(4) 0.1200(3) 0.0351(12) Uani 1 1 d . . . H37A H 0.7011 0.0091 0.1165 0.042 Uiso 1 1 calc R . . C38 C 0.7452(4) 0.1141(4) 0.0594(3) 0.0323(11) Uani 1 1 d . . . H38A H 0.7297 0.1049 0.0144 0.039 Uiso 1 1 calc R . . C39 C 0.7854(4) 0.1829(3) 0.0655(3) 0.0271(10) Uani 1 1 d . . . H39A H 0.7957 0.2225 0.0243 0.033 Uiso 1 1 calc R . . C40 C 0.9710(6) 0.4008(5) 0.4340(3) 0.0494(16) Uani 1 1 d . . . C41 C 1.0882(7) 0.3751(8) 0.4222(4) 0.076(3) Uani 1 1 d . . . H41A H 1.1416 0.3097 0.4321 0.091 Uiso 1 1 calc R . . C42 C 1.1242(10) 0.4481(11) 0.3955(5) 0.105(4) Uani 1 1 d . . . H42A H 1.2040 0.4316 0.3872 0.126 Uiso 1 1 calc R . . C43 C 1.0489(11) 0.5445(10) 0.3802(4) 0.090(4) Uani 1 1 d . . . C44 C 1.0914(13) 0.6199(11) 0.3484(5) 0.140(6) Uani 1 1 d . . . H44A H 1.0263 0.6831 0.3415 0.211 Uiso 1 1 d R . . H44B H 1.1355 0.6006 0.3024 0.211 Uiso 1 1 d R . . H44C H 1.1403 0.6256 0.3805 0.211 Uiso 1 1 d R . . C45 C 0.9333(9) 0.5665(7) 0.3959(4) 0.078(3) Uani 1 1 d . . . H45A H 0.8797 0.6324 0.3883 0.093 Uiso 1 1 calc R . . C46 C 0.8932(7) 0.4953(6) 0.4225(4) 0.0595(19) Uani 1 1 d . . . H46A H 0.8135 0.5119 0.4325 0.071 Uiso 1 1 calc R . . C47 C 0.9990(4) 0.2225(4) 0.3391(2) 0.0310(11) Uani 1 1 d . . . C48 C 1.1106(5) 0.1694(5) 0.3557(3) 0.0406(13) Uani 1 1 d . . . H48A H 1.1291 0.1646 0.4029 0.049 Uiso 1 1 calc R . . C49 C 1.1942(5) 0.1239(5) 0.3028(3) 0.0422(13) Uani 1 1 d . . . H49A H 1.2711 0.0893 0.3136 0.051 Uiso 1 1 calc R . . C50 C 1.1688(5) 0.1274(4) 0.2346(3) 0.0364(12) Uani 1 1 d . . . H50A H 1.2274 0.0957 0.1986 0.044 Uiso 1 1 calc R . . C51 C 1.0555(4) 0.1785(4) 0.2192(3) 0.0270(10) Uani 1 1 d . . . C52 C 1.1283(5) 0.0080(4) 0.1030(3) 0.0318(11) Uani 1 1 d . . . C53 C 1.2332(5) -0.0584(4) 0.1260(3) 0.0415(13) Uani 1 1 d . . . H53A H 1.2905 -0.0371 0.1315 0.050 Uiso 1 1 calc R . . C54 C 1.2517(6) -0.1565(4) 0.1404(3) 0.0471(15) Uani 1 1 d . . . H54A H 1.3231 -0.2028 0.1551 0.056 Uiso 1 1 calc R . . C55 C 1.1674(6) -0.1879(4) 0.1338(3) 0.0482(15) Uani 1 1 d . . . C56 C 1.1893(8) -0.2941(5) 0.1490(4) 0.068(2) Uani 1 1 d . . . H56A H 1.1212 -0.3030 0.1417 0.102 Uiso 1 1 d R . . H56B H 1.2066 -0.3152 0.1985 0.102 Uiso 1 1 d R . . H56C H 1.2543 -0.3333 0.1169 0.102 Uiso 1 1 d R . . C57 C 1.0650(6) -0.1209(4) 0.1108(3) 0.0435(14) Uani 1 1 d . . . H57A H 1.0076 -0.1421 0.1056 0.052 Uiso 1 1 calc R . . C58 C 1.0444(5) -0.0228(4) 0.0950(3) 0.0379(12) Uani 1 1 d . . . H58A H 0.9736 0.0227 0.0790 0.046 Uiso 1 1 calc R . . B1 B 0.7789(11) 0.8174(9) 0.2603(7) 0.153(7) Uiso 1 1 d D . . F1 F 0.6891(8) 0.8869(8) 0.2299(6) 0.192(4) Uiso 1 1 d D . . F2 F 0.7508(10) 0.8030(9) 0.3310(6) 0.207(4) Uiso 1 1 d D . . F3 F 0.8053(8) 0.7276(7) 0.2364(5) 0.166(3) Uiso 1 1 d D . . F4 F 0.8745(10) 0.8320(8) 0.2465(6) 0.192(4) Uiso 1 1 d D . . C59 C 0.3138(5) 1.2751(6) 0.1577(4) 0.057(2) Uani 0.80 1 d PD . . H59A H 0.3316 1.3282 0.1246 0.068 Uiso 0.80 1 d P . . H59B H 0.2641 1.2591 0.1337 0.068 Uiso 0.80 1 d P . . Cl1 Cl 0.23946(18) 1.33055(17) 0.23682(11) 0.0551(5) Uani 0.80 1 d P A . Cl2 Cl 0.4473(4) 1.1982(6) 0.1727(3) 0.085(2) Uani 0.40 1 d PD A 1 Cl2' Cl 0.4337(6) 1.1556(5) 0.1733(4) 0.080(2) Uiso 0.40 1 d PD A 2 C60 C 0.447(5) 0.8946(18) 0.252(2) 0.13(2) Uiso 0.20 1 d PD A 1 H60A H 0.3649 0.9060 0.2573 0.160 Uiso 0.20 1 calc PR A 1 H60B H 0.4722 0.8809 0.3002 0.160 Uiso 0.20 1 calc PR A 1 Cl3 Cl 0.4590(11) 0.9982(10) 0.2132(9) 0.119(5) Uani 0.20 1 d PD . . Cl4 Cl 0.5231(19) 0.7943(16) 0.2055(11) 0.147(6) Uiso 0.20 1 d PD . . C61 C 0.2914(16) 0.7587(8) 0.3720(7) 0.201(8) Uiso 1 1 d D . . H61A H 0.3562 0.7601 0.3928 0.241 Uiso 1 1 calc R . . H61B H 0.2495 0.7311 0.4097 0.241 Uiso 1 1 calc R . . Cl5 Cl 0.3449(3) 0.6824(3) 0.30522(19) 0.1441(15) Uani 1 1 d D . . Cl6 Cl 0.1990(4) 0.8800(5) 0.3466(2) 0.173(2) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0323(4) 0.0315(4) 0.0201(3) -0.0032(2) -0.0038(3) -0.0117(3) Ni2 0.0278(3) 0.0200(3) 0.0191(3) -0.0033(2) -0.0042(2) -0.0103(2) Ni3 0.0275(3) 0.0195(3) 0.0204(3) -0.0027(2) -0.0047(2) -0.0104(2) S1 0.0330(7) 0.0635(10) 0.0238(6) 0.0020(6) 0.0000(5) -0.0171(7) S2 0.0328(6) 0.0228(6) 0.0216(5) -0.0010(4) -0.0064(5) -0.0128(5) S3 0.0310(6) 0.0289(6) 0.0241(6) -0.0054(5) -0.0025(5) -0.0099(5) S4 0.0450(8) 0.0511(9) 0.0229(6) -0.0085(6) -0.0088(6) -0.0165(7) O1 0.042(2) 0.067(3) 0.0236(18) -0.0036(18) -0.0058(16) -0.017(2) O2 0.036(2) 0.074(3) 0.035(2) -0.003(2) 0.0006(18) -0.008(2) O3 0.038(2) 0.0342(19) 0.0246(16) -0.0035(14) -0.0105(15) -0.0174(16) O4 0.040(2) 0.0275(17) 0.0240(16) -0.0029(14) -0.0040(14) -0.0174(15) O5 0.038(2) 0.038(2) 0.0236(17) -0.0058(15) -0.0055(15) -0.0118(17) O6 0.033(2) 0.043(2) 0.034(2) -0.0039(16) 0.0015(16) -0.0155(17) O7 0.051(2) 0.054(2) 0.0228(18) -0.0084(17) -0.0050(17) -0.018(2) O8 0.054(3) 0.072(3) 0.026(2) -0.005(2) -0.0163(19) -0.009(2) N1 0.038(2) 0.036(2) 0.024(2) -0.0124(18) -0.0022(18) -0.012(2) N2 0.034(2) 0.0214(19) 0.028(2) -0.0083(16) -0.0049(17) -0.0116(17) N3 0.030(2) 0.0234(19) 0.027(2) -0.0027(16) -0.0050(16) -0.0134(17) N4 0.030(2) 0.043(3) 0.025(2) -0.0003(18) -0.0046(18) -0.015(2) N5 0.030(2) 0.0212(19) 0.0223(19) -0.0031(15) -0.0046(16) -0.0122(16) N6 0.030(2) 0.0209(19) 0.0237(19) 0.0022(15) -0.0076(16) -0.0116(17) N7 0.039(2) 0.033(2) 0.023(2) 0.0014(17) -0.0065(18) -0.018(2) N8 0.034(2) 0.025(2) 0.0226(19) -0.0007(16) -0.0058(17) -0.0145(18) N9 0.029(2) 0.0202(19) 0.0234(19) -0.0050(15) -0.0061(16) -0.0087(16) N10 0.037(2) 0.037(2) 0.023(2) -0.0041(18) -0.0083(18) -0.013(2) N11 0.029(2) 0.026(2) 0.0204(19) -0.0040(15) -0.0060(16) -0.0109(17) N12 0.028(2) 0.0228(19) 0.0233(19) -0.0069(16) -0.0055(16) -0.0065(16) C1 0.046(3) 0.043(3) 0.031(3) -0.016(2) 0.001(2) -0.009(3) C2 0.068(5) 0.052(4) 0.041(4) -0.025(3) 0.008(3) -0.004(3) C3 0.079(5) 0.034(3) 0.061(4) -0.023(3) -0.009(4) -0.009(3) C4 0.060(4) 0.030(3) 0.044(3) -0.013(2) 0.000(3) -0.017(3) C5 0.040(3) 0.030(3) 0.030(3) -0.012(2) -0.007(2) -0.012(2) C6 0.034(3) 0.022(2) 0.025(2) -0.0010(18) -0.009(2) -0.011(2) C7 0.053(3) 0.038(3) 0.040(3) -0.010(2) -0.008(3) -0.029(3) C8 0.057(4) 0.046(3) 0.050(3) 0.001(3) -0.014(3) -0.036(3) C9 0.041(3) 0.047(3) 0.038(3) 0.003(2) -0.007(2) -0.027(3) C10 0.034(3) 0.034(3) 0.027(2) 0.001(2) -0.008(2) -0.019(2) C11 0.037(3) 0.073(4) 0.033(3) 0.021(3) -0.011(2) -0.029(3) C12 0.054(4) 0.141(8) 0.046(4) 0.018(4) -0.011(3) -0.062(5) C13 0.082(7) 0.198(13) 0.070(6) 0.063(7) -0.039(5) -0.111(8) C14 0.082(6) 0.122(8) 0.080(6) 0.065(6) -0.058(5) -0.078(6) C15 0.144(9) 0.165(10) 0.137(9) 0.105(8) -0.102(8) -0.136(9) C16 0.073(5) 0.073(5) 0.092(6) 0.024(4) -0.035(5) -0.050(5) C17 0.053(4) 0.068(5) 0.063(4) 0.015(4) -0.007(3) -0.037(4) C18 0.033(3) 0.030(3) 0.026(2) -0.004(2) -0.002(2) -0.012(2) C19 0.032(3) 0.047(3) 0.028(3) -0.003(2) -0.001(2) -0.017(2) C20 0.030(3) 0.039(3) 0.036(3) 0.002(2) -0.007(2) -0.012(2) C21 0.034(3) 0.026(2) 0.030(2) -0.001(2) -0.007(2) -0.012(2) C22 0.031(2) 0.019(2) 0.025(2) -0.0036(18) -0.0065(19) -0.0118(19) C23 0.041(3) 0.023(2) 0.026(2) 0.0009(19) -0.005(2) -0.016(2) C24 0.037(3) 0.032(3) 0.049(3) 0.008(2) -0.012(3) -0.015(2) C25 0.041(3) 0.028(3) 0.078(5) 0.010(3) -0.011(3) -0.008(3) C26 0.049(4) 0.024(3) 0.067(4) -0.005(3) 0.005(3) -0.016(3) C27 0.063(5) 0.025(3) 0.141(8) -0.010(4) 0.008(5) -0.014(3) C28 0.052(4) 0.033(3) 0.059(4) -0.007(3) -0.011(3) -0.023(3) C29 0.043(3) 0.025(3) 0.043(3) -0.003(2) -0.011(2) -0.015(2) C30 0.046(3) 0.047(3) 0.026(3) 0.009(2) -0.011(2) -0.021(3) C31 0.063(4) 0.048(4) 0.038(3) 0.016(3) -0.019(3) -0.028(3) C32 0.066(4) 0.036(3) 0.047(3) 0.013(3) -0.024(3) -0.025(3) C33 0.051(3) 0.029(3) 0.039(3) 0.002(2) -0.016(3) -0.018(3) C34 0.033(3) 0.028(2) 0.027(2) 0.000(2) -0.007(2) -0.014(2) C35 0.028(2) 0.019(2) 0.026(2) -0.0043(18) -0.0079(19) -0.0073(19) C36 0.036(3) 0.023(2) 0.035(3) -0.001(2) -0.008(2) -0.014(2) C37 0.040(3) 0.024(2) 0.049(3) -0.008(2) -0.016(2) -0.016(2) C38 0.036(3) 0.030(3) 0.034(3) -0.010(2) -0.011(2) -0.012(2) C39 0.031(3) 0.024(2) 0.025(2) -0.0052(19) -0.0056(19) -0.008(2) C40 0.057(4) 0.074(5) 0.031(3) -0.025(3) -0.006(3) -0.033(4) C41 0.068(5) 0.115(7) 0.067(5) -0.049(5) 0.004(4) -0.051(5) C42 0.105(8) 0.186(13) 0.084(7) -0.078(8) 0.030(6) -0.111(9) C43 0.146(10) 0.138(9) 0.046(4) -0.046(5) 0.017(5) -0.114(9) C44 0.243(15) 0.216(14) 0.071(6) -0.064(8) 0.042(8) -0.202(14) C45 0.133(8) 0.094(6) 0.044(4) -0.013(4) -0.019(5) -0.077(6) C46 0.079(5) 0.072(5) 0.047(4) -0.017(3) -0.013(4) -0.044(4) C47 0.036(3) 0.040(3) 0.021(2) -0.002(2) -0.007(2) -0.017(2) C48 0.038(3) 0.052(3) 0.029(3) -0.004(2) -0.012(2) -0.012(3) C49 0.030(3) 0.056(4) 0.035(3) -0.006(3) -0.009(2) -0.010(3) C50 0.031(3) 0.046(3) 0.030(3) -0.008(2) -0.005(2) -0.011(2) C51 0.030(3) 0.027(2) 0.025(2) -0.0041(19) -0.0059(19) -0.011(2) C52 0.038(3) 0.026(2) 0.029(2) -0.010(2) -0.003(2) -0.008(2) C53 0.047(3) 0.035(3) 0.036(3) -0.013(2) -0.010(3) -0.006(3) C54 0.061(4) 0.032(3) 0.037(3) -0.009(2) -0.015(3) -0.003(3) C55 0.077(5) 0.031(3) 0.036(3) -0.010(2) -0.007(3) -0.018(3) C56 0.112(7) 0.036(4) 0.058(4) 0.000(3) -0.027(4) -0.028(4) C57 0.059(4) 0.035(3) 0.042(3) -0.019(3) -0.001(3) -0.022(3) C58 0.038(3) 0.034(3) 0.039(3) -0.014(2) -0.001(2) -0.010(2) C59 0.049(5) 0.088(7) 0.040(4) 0.004(4) -0.008(4) -0.036(5) Cl1 0.0540(12) 0.0767(14) 0.0498(11) -0.0043(10) -0.0066(9) -0.0413(11) Cl2 0.033(2) 0.108(5) 0.080(4) -0.040(4) -0.022(2) 0.017(3) Cl3 0.148(14) 0.074(8) 0.116(11) -0.006(8) -0.018(10) -0.025(9) Cl5 0.154(3) 0.204(4) 0.118(2) 0.066(2) -0.084(2) -0.116(3) Cl6 0.123(3) 0.300(6) 0.107(2) -0.018(3) -0.030(2) -0.091(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 N10 1.902(4) . ? Ni1 N7 1.914(4) . ? Ni1 N4 1.917(4) . ? Ni1 N1 1.920(5) . ? Ni1 Ni2 2.3091(8) . ? Ni2 N2 1.870(4) . ? Ni2 N8 1.876(4) . ? Ni2 N11 1.929(4) . ? Ni2 N5 1.935(4) . ? Ni2 Ni3 2.3045(8) . ? Ni3 N12 1.903(4) . ? Ni3 N6 1.903(4) . ? Ni3 N3 1.913(4) . ? Ni3 N9 1.915(4) . ? S1 O2 1.437(5) . ? S1 O1 1.444(4) . ? S1 N4 1.627(4) . ? S1 C11 1.755(7) . ? S2 O4 1.437(4) . ? S2 O3 1.441(3) . ? S2 N6 1.631(4) . ? S2 C23 1.758(5) . ? S3 O5 1.437(4) . ? S3 O6 1.438(4) . ? S3 N12 1.635(4) . ? S3 C52 1.760(5) . ? S4 O7 1.434(4) . ? S4 O8 1.439(5) . ? S4 N10 1.636(4) . ? S4 C40 1.775(7) . ? N1 C1 1.355(7) . ? N1 C5 1.356(7) . ? N2 C6 1.363(6) . ? N2 C5 1.382(6) . ? N3 C10 1.356(6) . ? N3 C6 1.364(6) . ? N4 C18 1.387(7) . ? N5 C18 1.360(6) . ? N5 C22 1.368(6) . ? N6 C22 1.392(6) . ? N7 C30 1.364(6) . ? N7 C34 1.371(6) . ? N8 C34 1.367(6) . ? N8 C35 1.388(6) . ? N9 C39 1.356(6) . ? N9 C35 1.363(6) . ? N10 C47 1.390(7) . ? N11 C51 1.369(6) . ? N11 C47 1.372(6) . ? N12 C51 1.379(6) . ? C1 C2 1.353(9) . ? C1 H1A 0.9500 . ? C2 C3 1.385(10) . ? C2 H2A 0.9500 . ? C3 C4 1.384(9) . ? C3 H3A 0.9500 . ? C4 C5 1.401(8) . ? C4 H4A 0.9500 . ? C6 C7 1.398(7) . ? C7 C8 1.370(8) . ? C7 H7A 0.9500 . ? C8 C9 1.392(9) . ? C8 H8A 0.9500 . ? C9 C10 1.358(7) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C17 1.372(10) . ? C11 C12 1.405(9) . ? C12 C13 1.367(14) . ? C12 H12A 0.9500 . ? C13 C14 1.411(16) . ? C13 H13A 0.9500 . ? C14 C16 1.362(12) . ? C14 C15 1.511(12) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.394(10) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.394(8) . ? C19 C20 1.376(7) . ? C19 H19A 0.9500 . ? C20 C21 1.367(7) . ? C20 H20A 0.9500 . ? C21 C22 1.393(7) . ? C21 H21A 0.9500 . ? C23 C24 1.387(8) . ? C23 C29 1.400(7) . ? C24 C25 1.376(8) . ? C24 H24A 0.9500 . ? C25 C26 1.400(9) . ? C25 H25A 0.9500 . ? C26 C28 1.374(9) . ? C26 C27 1.502(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.391(7) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C31 1.348(9) . ? C30 H30A 0.9500 . ? C31 C32 1.382(9) . ? C31 H31A 0.9500 . ? C32 C33 1.389(8) . ? C32 H32A 0.9500 . ? C33 C34 1.391(7) . ? C33 H33A 0.9500 . ? C35 C36 1.398(6) . ? C36 C37 1.376(7) . ? C36 H36A 0.9500 . ? C37 C38 1.386(8) . ? C37 H37A 0.9500 . ? C38 C39 1.370(7) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C46 1.366(10) . ? C40 C41 1.391(10) . ? C41 C42 1.380(14) . ? C41 H41A 0.9500 . ? C42 C43 1.389(17) . ? C42 H42A 0.9500 . ? C43 C45 1.385(14) . ? C43 C44 1.488(13) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.391(11) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C48 1.388(8) . ? C48 C49 1.377(8) . ? C48 H48A 0.9500 . ? C49 C50 1.375(7) . ? C49 H49A 0.9500 . ? C50 C51 1.397(7) . ? C50 H50A 0.9500 . ? C52 C58 1.386(8) . ? C52 C53 1.397(8) . ? C53 C54 1.394(8) . ? C53 H53A 0.9500 . ? C54 C55 1.389(9) . ? C54 H54A 0.9500 . ? C55 C57 1.377(9) . ? C55 C56 1.502(8) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.387(8) . ? C57 H57A 0.9500 . ? C58 H58A 0.9500 . ? B1 F4 1.331(9) . ? B1 F1 1.340(9) . ? B1 F2 1.355(9) . ? B1 F3 1.377(9) . ? C59 Cl2 1.670(7) . ? C59 Cl1 1.769(8) . ? C59 Cl2' 1.840(8) . ? C59 H59A 1.0348 . ? C59 H59B 0.9662 . ? Cl2' Cl3 2.295(16) . ? C60 Cl3 1.699(10) . ? C60 Cl4 1.700(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 Cl5 1.698(9) . ? C61 Cl6 1.762(9) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? 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 N10 Ni1 N7 87.40(19) . . ? N10 Ni1 N4 173.90(18) . . ? N7 Ni1 N4 90.57(19) . . ? N10 Ni1 N1 92.49(19) . . ? N7 Ni1 N1 173.87(17) . . ? N4 Ni1 N1 88.91(19) . . ? N10 Ni1 Ni2 87.71(13) . . ? N7 Ni1 Ni2 86.82(12) . . ? N4 Ni1 Ni2 86.43(12) . . ? N1 Ni1 Ni2 87.06(12) . . ? N2 Ni2 N8 179.52(19) . . ? N2 Ni2 N11 90.59(17) . . ? N8 Ni2 N11 88.98(17) . . ? N2 Ni2 N5 89.70(17) . . ? N8 Ni2 N5 90.73(17) . . ? N11 Ni2 N5 179.71(16) . . ? N2 Ni2 Ni3 89.53(12) . . ? N8 Ni2 Ni3 90.68(12) . . ? N11 Ni2 Ni3 90.19(11) . . ? N5 Ni2 Ni3 89.81(11) . . ? N2 Ni2 Ni1 89.87(12) . . ? N8 Ni2 Ni1 89.91(12) . . ? N11 Ni2 Ni1 89.86(11) . . ? N5 Ni2 Ni1 90.15(11) . . ? Ni3 Ni2 Ni1 179.40(3) . . ? N12 Ni3 N6 174.63(16) . . ? N12 Ni3 N3 88.34(17) . . ? N6 Ni3 N3 91.54(17) . . ? N12 Ni3 N9 90.87(17) . . ? N6 Ni3 N9 88.65(16) . . ? N3 Ni3 N9 173.59(16) . . ? N12 Ni3 Ni2 87.21(12) . . ? N6 Ni3 Ni2 87.42(12) . . ? N3 Ni3 Ni2 87.20(12) . . ? N9 Ni3 Ni2 86.41(11) . . ? O2 S1 O1 117.0(3) . . ? O2 S1 N4 114.0(3) . . ? O1 S1 N4 102.2(2) . . ? O2 S1 C11 107.5(3) . . ? O1 S1 C11 108.3(3) . . ? N4 S1 C11 107.4(3) . . ? O4 S2 O3 117.5(2) . . ? O4 S2 N6 102.5(2) . . ? O3 S2 N6 112.6(2) . . ? O4 S2 C23 109.2(2) . . ? O3 S2 C23 107.3(2) . . ? N6 S2 C23 107.2(2) . . ? O5 S3 O6 118.1(2) . . ? O5 S3 N12 102.9(2) . . ? O6 S3 N12 112.5(2) . . ? O5 S3 C52 109.0(2) . . ? O6 S3 C52 108.0(2) . . ? N12 S3 C52 105.6(2) . . ? O7 S4 O8 117.2(3) . . ? O7 S4 N10 103.7(2) . . ? O8 S4 N10 111.4(3) . . ? O7 S4 C40 110.2(3) . . ? O8 S4 C40 108.7(3) . . ? N10 S4 C40 105.0(2) . . ? C1 N1 C5 119.1(5) . . ? C1 N1 Ni1 119.9(4) . . ? C5 N1 Ni1 120.9(3) . . ? C6 N2 C5 124.2(4) . . ? C6 N2 Ni2 118.6(3) . . ? C5 N2 Ni2 117.2(3) . . ? C10 N3 C6 119.8(4) . . ? C10 N3 Ni3 119.8(3) . . ? C6 N3 Ni3 120.4(3) . . ? C18 N4 S1 124.0(4) . . ? C18 N4 Ni1 121.0(3) . . ? S1 N4 Ni1 109.8(2) . . ? C18 N5 C22 120.3(4) . . ? C18 N5 Ni2 119.5(3) . . ? C22 N5 Ni2 120.1(3) . . ? C22 N6 S2 122.5(3) . . ? C22 N6 Ni3 121.4(3) . . ? S2 N6 Ni3 113.6(2) . . ? C30 N7 C34 119.5(5) . . ? C30 N7 Ni1 118.7(4) . . ? C34 N7 Ni1 121.6(3) . . ? C34 N8 C35 124.3(4) . . ? C34 N8 Ni2 118.1(3) . . ? C35 N8 Ni2 117.5(3) . . ? C39 N9 C35 119.7(4) . . ? C39 N9 Ni3 118.4(3) . . ? C35 N9 Ni3 122.0(3) . . ? C47 N10 S4 122.1(4) . . ? C47 N10 Ni1 120.2(3) . . ? S4 N10 Ni1 117.4(2) . . ? C51 N11 C47 121.1(4) . . ? C51 N11 Ni2 119.2(3) . . ? C47 N11 Ni2 119.7(3) . . ? C51 N12 S3 122.6(3) . . ? C51 N12 Ni3 121.4(3) . . ? S3 N12 Ni3 113.7(2) . . ? C2 C1 N1 122.8(6) . . ? C2 C1 H1A 118.6 . . ? N1 C1 H1A 118.6 . . ? C1 C2 C3 119.1(6) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C4 C3 C2 119.4(6) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 119.2(6) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? N1 C5 N2 115.7(4) . . ? N1 C5 C4 120.3(5) . . ? N2 C5 C4 123.8(5) . . ? N2 C6 N3 115.7(4) . . ? N2 C6 C7 125.0(4) . . ? N3 C6 C7 119.2(4) . . ? C8 C7 C6 120.0(5) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 120.0(5) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C10 C9 C8 118.3(5) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? N3 C10 C9 122.6(5) . . ? N3 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? C17 C11 C12 119.5(7) . . ? C17 C11 S1 122.2(5) . . ? C12 C11 S1 118.1(6) . . ? C13 C12 C11 119.0(10) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? C12 C13 C14 121.9(8) . . ? C12 C13 H13A 119.1 . . ? C14 C13 H13A 119.1 . . ? C16 C14 C13 117.9(8) . . ? C16 C14 C15 122.0(12) . . ? C13 C14 C15 120.1(10) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 C17 121.2(10) . . ? C14 C16 H16A 119.4 . . ? C17 C16 H16A 119.4 . . ? C11 C17 C16 120.4(7) . . ? C11 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? N5 C18 N4 114.0(4) . . ? N5 C18 C19 120.6(4) . . ? N4 C18 C19 125.4(5) . . ? C20 C19 C18 118.3(5) . . ? C20 C19 H19A 120.9 . . ? C18 C19 H19A 120.9 . . ? C21 C20 C19 121.8(5) . . ? C21 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? C20 C21 C22 118.6(5) . . ? C20 C21 H21A 120.7 . . ? C22 C21 H21A 120.7 . . ? N5 C22 N6 113.5(4) . . ? N5 C22 C21 120.3(4) . . ? N6 C22 C21 126.1(4) . . ? C24 C23 C29 120.4(5) . . ? C24 C23 S2 120.5(4) . . ? C29 C23 S2 119.1(4) . . ? C25 C24 C23 118.9(5) . . ? C25 C24 H24A 120.6 . . ? C23 C24 H24A 120.6 . . ? C24 C25 C26 122.1(6) . . ? C24 C25 H25A 119.0 . . ? C26 C25 H25A 119.0 . . ? C28 C26 C25 118.1(5) . . ? C28 C26 C27 120.8(6) . . ? C25 C26 C27 121.1(6) . . ? 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 C29 121.4(5) . . ? C26 C28 H28A 119.3 . . ? C29 C28 H28A 119.3 . . ? C28 C29 C23 119.2(5) . . ? C28 C29 H29A 120.4 . . ? C23 C29 H29A 120.4 . . ? C31 C30 N7 122.6(5) . . ? C31 C30 H30A 118.7 . . ? N7 C30 H30A 118.7 . . ? C30 C31 C32 119.0(5) . . ? C30 C31 H31A 120.5 . . ? C32 C31 H31A 120.5 . . ? C31 C32 C33 119.7(6) . . ? C31 C32 H32A 120.2 . . ? C33 C32 H32A 120.2 . . ? C32 C33 C34 119.8(5) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? N8 C34 N7 114.8(4) . . ? N8 C34 C33 125.7(5) . . ? N7 C34 C33 119.3(5) . . ? N9 C35 N8 115.0(4) . . ? N9 C35 C36 120.2(4) . . ? N8 C35 C36 124.7(4) . . ? C37 C36 C35 119.2(5) . . ? C37 C36 H36A 120.4 . . ? C35 C36 H36A 120.4 . . ? C36 C37 C38 120.0(4) . . ? C36 C37 H37A 120.0 . . ? C38 C37 H37A 120.0 . . ? C39 C38 C37 119.0(5) . . ? C39 C38 H38A 120.5 . . ? C37 C38 H38A 120.5 . . ? N9 C39 C38 121.8(4) . . ? N9 C39 H39A 119.1 . . ? C38 C39 H39A 119.1 . . ? C46 C40 C41 121.9(8) . . ? C46 C40 S4 119.2(5) . . ? C41 C40 S4 118.8(7) . . ? C42 C41 C40 117.6(10) . . ? C42 C41 H41A 121.2 . . ? C40 C41 H41A 121.2 . . ? C41 C42 C43 122.9(10) . . ? C41 C42 H42A 118.6 . . ? C43 C42 H42A 118.6 . . ? C45 C43 C42 116.9(9) . . ? C45 C43 C44 122.1(13) . . ? C42 C43 C44 121.1(12) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 C46 122.2(10) . . ? C43 C45 H45A 118.9 . . ? C46 C45 H45A 118.9 . . ? C40 C46 C45 118.5(8) . . ? C40 C46 H46A 120.8 . . ? C45 C46 H46A 120.8 . . ? N11 C47 C48 119.8(5) . . ? N11 C47 N10 114.4(4) . . ? C48 C47 N10 125.8(5) . . ? C49 C48 C47 119.0(5) . . ? C49 C48 H48A 120.5 . . ? C47 C48 H48A 120.5 . . ? C50 C49 C48 121.5(5) . . ? C50 C49 H49A 119.3 . . ? C48 C49 H49A 119.3 . . ? C49 C50 C51 118.8(5) . . ? C49 C50 H50A 120.6 . . ? C51 C50 H50A 120.6 . . ? N11 C51 N12 114.6(4) . . ? N11 C51 C50 119.7(4) . . ? N12 C51 C50 125.7(4) . . ? C58 C52 C53 120.9(5) . . ? C58 C52 S3 119.0(4) . . ? C53 C52 S3 120.1(4) . . ? C54 C53 C52 118.4(6) . . ? C54 C53 H53A 120.8 . . ? C52 C53 H53A 120.8 . . ? C55 C54 C53 121.1(6) . . ? C55 C54 H54A 119.4 . . ? C53 C54 H54A 119.4 . . ? C57 C55 C54 119.2(5) . . ? C57 C55 C56 120.5(6) . . ? C54 C55 C56 120.3(7) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 C57 C58 121.2(6) . . ? C55 C57 H57A 119.4 . . ? C58 C57 H57A 119.4 . . ? C52 C58 C57 119.2(6) . . ? C52 C58 H58A 120.4 . . ? C57 C58 H58A 120.4 . . ? F4 B1 F1 114.3(12) . . ? F4 B1 F2 112.5(12) . . ? F1 B1 F2 110.4(12) . . ? F4 B1 F3 105.8(11) . . ? F1 B1 F3 110.5(11) . . ? F2 B1 F3 102.6(11) . . ? Cl2 C59 Cl1 109.4(5) . . ? Cl2 C59 Cl2' 23.5(3) . . ? Cl1 C59 Cl2' 113.6(5) . . ? Cl2 C59 H59A 98.7 . . ? Cl1 C59 H59A 106.2 . . ? Cl2' C59 H59A 117.3 . . ? Cl2 C59 H59B 124.3 . . ? Cl1 C59 H59B 109.9 . . ? Cl2' C59 H59B 102.9 . . ? H59A C59 H59B 106.4 . . ? C59 Cl2' Cl3 137.8(6) . . ? Cl3 C60 Cl4 114.0(18) . . ? Cl3 C60 H60A 108.7 . . ? Cl4 C60 H60A 108.8 . . ? Cl3 C60 H60B 108.8 . . ? Cl4 C60 H60B 108.8 . . ? H60A C60 H60B 107.6 . . ? C60 Cl3 Cl2' 166.8(17) . . ? Cl5 C61 Cl6 115.2(8) . . ? Cl5 C61 H61A 108.5 . . ? Cl6 C61 H61A 108.5 . . ? Cl5 C61 H61B 108.5 . . ? Cl6 C61 H61B 108.5 . . ? H61A C61 H61B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.198 _refine_diff_density_min -1.432 _refine_diff_density_rms 0.191 #===END data_ic11673(comp6) _database_code_depnum_ccdc_archive 'CCDC 618768' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H44 N12 Ni3 O9 S4' _chemical_formula_weight 1117.22 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.9738(4) _cell_length_b 13.6219(3) _cell_length_c 17.4912(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4520.76(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour deep-brown _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 1.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details ? _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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30178 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9158 _reflns_number_gt 7368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1045P)^2^+3.2541P] 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 0.017(16) _refine_ls_number_reflns 9158 _refine_ls_number_parameters 576 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1647 _refine_ls_wR_factor_gt 0.1503 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.035 _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 0.52020(4) 0.64179(5) 0.73196(4) 0.04087(18) Uani 1 1 d . . . Ni2 Ni 0.43379(4) 0.72675(6) 0.80147(4) 0.04117(18) Uani 1 1 d . . . Ni3 Ni 0.34731(5) 0.81261(8) 0.87182(5) 0.0613(3) Uani 1 1 d . . . N1 N 0.4776(3) 0.6996(4) 0.6423(3) 0.0465(12) Uani 1 1 d . . . N2 N 0.4194(3) 0.8116(4) 0.7178(3) 0.0531(13) Uani 1 1 d . . . N3 N 0.3622(4) 0.9196(6) 0.7997(4) 0.087(2) Uani 1 1 d . . . N4 N 0.4562(3) 0.5344(4) 0.7239(3) 0.0449(11) Uani 1 1 d . . . N5 N 0.3632(2) 0.6364(4) 0.7623(3) 0.0435(11) Uani 1 1 d . . . N6 N 0.2806(3) 0.7487(5) 0.8035(4) 0.0606(16) Uani 1 1 d . . . N7 N 0.5532(2) 0.5955(4) 0.8297(3) 0.0423(11) Uani 1 1 d . . . N8 N 0.4487(3) 0.6424(4) 0.8855(3) 0.0399(10) Uani 1 1 d . . . N9 N 0.3425(3) 0.6986(4) 0.9370(3) 0.0531(13) Uani 1 1 d . . . N10 N 0.5785(3) 0.7547(4) 0.7449(3) 0.0548(14) Uani 1 1 d . . . N11 N 0.5048(3) 0.8175(4) 0.8383(3) 0.0533(13) Uani 1 1 d . . . N12 N 0.4221(4) 0.8665(5) 0.9322(4) 0.0714(18) Uani 1 1 d . . . O1 O 0.5652(2) 0.4539(4) 0.6889(3) 0.0611(12) Uani 1 1 d . . . O2 O 0.4540(3) 0.3768(4) 0.6453(3) 0.0660(13) Uani 1 1 d . . . O3 O 0.2126(4) 0.8716(7) 0.8663(5) 0.132(3) Uani 1 1 d . . . O4 O 0.1459(3) 0.7324(8) 0.8176(4) 0.125(3) Uani 1 1 d . . . O5 O 0.6409(3) 0.6671(4) 0.6467(3) 0.0716(16) Uani 1 1 d . . . O6 O 0.7102(3) 0.7759(5) 0.7234(5) 0.110(3) Uani 1 1 d . . . O7 O 0.4483(5) 0.9751(5) 1.0468(4) 0.126(3) Uani 1 1 d . . . O8 O 0.3367(5) 0.8851(8) 1.0343(5) 0.133(3) Uani 1 1 d . . . S1 S 0.49229(9) 0.43101(12) 0.70378(9) 0.0494(4) Uani 1 1 d . . . S2 S 0.20358(12) 0.7960(3) 0.80730(19) 0.1029(10) Uani 1 1 d . . . S3 S 0.64571(9) 0.75732(16) 0.68789(15) 0.0712(6) Uani 1 1 d . . . S4 S 0.41268(18) 0.8901(2) 1.02161(13) 0.0990(9) Uani 1 1 d . . . C1 C 0.4905(4) 0.6589(5) 0.5731(4) 0.0520(15) Uani 1 1 d . . . H1A H 0.5205 0.6032 0.5710 0.062 Uiso 1 1 calc R . . C2 C 0.4632(4) 0.6928(5) 0.5070(4) 0.0590(17) Uani 1 1 d . . . H2A H 0.4761 0.6638 0.4596 0.071 Uiso 1 1 calc R . . C3 C 0.4160(4) 0.7705(5) 0.5092(4) 0.0572(16) Uani 1 1 d . . . H3A H 0.3948 0.7942 0.4635 0.069 Uiso 1 1 calc R . . C4 C 0.4003(4) 0.8132(5) 0.5791(4) 0.0612(18) Uani 1 1 d . . . H4A H 0.3675 0.8657 0.5822 0.073 Uiso 1 1 calc R . . C5 C 0.4338(3) 0.7775(5) 0.6456(4) 0.0498(15) Uani 1 1 d . . . C6 C 0.3980(4) 0.9060(5) 0.7319(4) 0.067(2) Uani 1 1 d . . . C7 C 0.4153(7) 0.9872(7) 0.6854(5) 0.097(3) Uani 1 1 d . . . H7A H 0.4426 0.9792 0.6403 0.117 Uiso 1 1 calc R . . C8 C 0.3909(11) 1.0796(8) 0.7075(7) 0.159(8) Uani 1 1 d . . . H8A H 0.4022 1.1356 0.6775 0.191 Uiso 1 1 calc R . . C9 C 0.3506(11) 1.0904(9) 0.7726(9) 0.160(8) Uani 1 1 d . . . H9A H 0.3294 1.1518 0.7843 0.192 Uiso 1 1 calc R . . C10 C 0.3416(7) 1.0125(9) 0.8194(7) 0.124(5) Uani 1 1 d . . . H10A H 0.3201 1.0226 0.8678 0.149 Uiso 1 1 calc R . . C11 C 0.3832(3) 0.5490(4) 0.7305(3) 0.0401(11) Uani 1 1 d . . . C12 C 0.3328(3) 0.4827(5) 0.7047(3) 0.0530(15) Uani 1 1 d . . . H12A H 0.3471 0.4212 0.6844 0.064 Uiso 1 1 calc R . . C13 C 0.2626(3) 0.5059(6) 0.7087(4) 0.0622(18) Uani 1 1 d . . . H13A H 0.2281 0.4612 0.6903 0.075 Uiso 1 1 calc R . . C14 C 0.2422(3) 0.5966(6) 0.7404(4) 0.0626(18) Uani 1 1 d . . . H14A H 0.1937 0.6137 0.7434 0.075 Uiso 1 1 calc R . . C15 C 0.2936(3) 0.6614(6) 0.7672(4) 0.0518(16) Uani 1 1 d . . . C16 C 0.4882(4) 0.3606(5) 0.7883(4) 0.0645(19) Uani 1 1 d . . . H16A H 0.5152 0.2999 0.7815 0.097 Uiso 1 1 calc R . . H16B H 0.4389 0.3444 0.7996 0.097 Uiso 1 1 calc R . . H16C H 0.5081 0.3984 0.8308 0.097 Uiso 1 1 calc R . . C17 C 0.1973(6) 0.8439(9) 0.7309(10) 0.134(6) Uani 1 1 d . . . H17A H 0.1514 0.8764 0.7269 0.202 Uiso 1 1 calc R . . H17B H 0.2015 0.7941 0.6907 0.202 Uiso 1 1 calc R . . H17C H 0.2349 0.8926 0.7250 0.202 Uiso 1 1 calc R . . C18 C 0.6200(3) 0.5625(6) 0.8343(4) 0.0606(18) Uani 1 1 d . . . H18A H 0.6482 0.5638 0.7894 0.073 Uiso 1 1 calc R . . C19 C 0.6497(4) 0.5267(7) 0.9011(5) 0.074(2) Uani 1 1 d . . . H19A H 0.6947 0.4959 0.9012 0.089 Uiso 1 1 calc R . . C20 C 0.6106(3) 0.5378(6) 0.9681(4) 0.0618(18) Uani 1 1 d . . . H20A H 0.6302 0.5193 1.0160 0.074 Uiso 1 1 calc R . . C21 C 0.5441(3) 0.5754(5) 0.9646(4) 0.0499(14) Uani 1 1 d . . . H21A H 0.5178 0.5840 1.0103 0.060 Uiso 1 1 calc R . . C22 C 0.5137(3) 0.6017(4) 0.8935(3) 0.0412(12) Uani 1 1 d . . . C23 C 0.3937(3) 0.6268(5) 0.9343(3) 0.0438(13) Uani 1 1 d . . . C24 C 0.3858(3) 0.5409(5) 0.9788(3) 0.0488(14) Uani 1 1 d . . . H24A H 0.4203 0.4904 0.9760 0.059 Uiso 1 1 calc R . . C25 C 0.3270(4) 0.5297(7) 1.0274(4) 0.070(2) Uani 1 1 d . . . H25A H 0.3214 0.4732 1.0586 0.084 Uiso 1 1 calc R . . C26 C 0.2774(4) 0.6055(7) 1.0275(4) 0.069(2) Uani 1 1 d . . . H26A H 0.2372 0.6008 1.0597 0.083 Uiso 1 1 calc R . . C27 C 0.2856(4) 0.6858(7) 0.9823(4) 0.065(2) Uani 1 1 d . . . H27A H 0.2500 0.7348 0.9826 0.078 Uiso 1 1 calc R . . C28 C 0.5675(4) 0.8269(6) 0.8003(5) 0.0644(18) Uani 1 1 d . . . C29 C 0.6136(7) 0.8997(9) 0.8165(8) 0.114(4) Uani 1 1 d . . . H29A H 0.6588 0.9019 0.7931 0.137 Uiso 1 1 calc R . . C30 C 0.5934(10) 0.9689(11) 0.8670(11) 0.160(7) Uani 1 1 d . . . H30A H 0.6223 1.0252 0.8738 0.192 Uiso 1 1 calc R . . C31 C 0.5347(9) 0.9612(8) 0.9075(8) 0.126(5) Uani 1 1 d . . . H31A H 0.5243 1.0094 0.9452 0.151 Uiso 1 1 calc R . . C32 C 0.4866(6) 0.8819(6) 0.8957(6) 0.084(3) Uani 1 1 d . . . C33 C 0.6292(6) 0.8549(7) 0.6236(7) 0.101(4) Uani 1 1 d . . . H33A H 0.6701 0.8639 0.5901 0.152 Uiso 1 1 calc R . . H33B H 0.6207 0.9154 0.6525 0.152 Uiso 1 1 calc R . . H33C H 0.5876 0.8395 0.5926 0.152 Uiso 1 1 calc R . . C34 C 0.4539(7) 0.7924(7) 1.0709(5) 0.095(3) Uani 1 1 d . . . H34A H 0.4546 0.8069 1.1258 0.142 Uiso 1 1 calc R . . H34B H 0.5023 0.7847 1.0523 0.142 Uiso 1 1 calc R . . H34C H 0.4275 0.7316 1.0620 0.142 Uiso 1 1 calc R . . O9 O 0.7428(5) 0.8210(7) 0.4715(5) 0.126(3) Uiso 1 1 d . . . C36 C 0.6664(9) 0.7252(12) 0.4323(11) 0.146(5) Uiso 1 1 d . . . H36A H 0.6539 0.6736 0.3957 0.220 Uiso 1 1 calc R . . H36B H 0.6520 0.7892 0.4120 0.220 Uiso 1 1 calc R . . H36C H 0.6423 0.7131 0.4810 0.220 Uiso 1 1 calc R . . C37 C 0.7414(11) 0.7248(14) 0.4444(13) 0.172(7) Uiso 1 1 d . . . H37A H 0.7565 0.6762 0.4831 0.207 Uiso 1 1 calc R . . H37B H 0.7685 0.7161 0.3965 0.207 Uiso 1 1 calc R . . C38 C 0.8113(9) 0.8260(12) 0.5065(11) 0.151(6) Uiso 1 1 d . . . H38A H 0.8501 0.8118 0.4702 0.181 Uiso 1 1 calc R . . H38B H 0.8154 0.7839 0.5524 0.181 Uiso 1 1 calc R . . C39 C 0.8048(13) 0.9404(15) 0.5268(14) 0.212(9) Uiso 1 1 d . . . H39A H 0.8210 0.9514 0.5793 0.319 Uiso 1 1 calc R . . H39B H 0.7556 0.9610 0.5221 0.319 Uiso 1 1 calc R . . H39C H 0.8340 0.9786 0.4915 0.319 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 0.0331(3) 0.0498(4) 0.0396(3) 0.0091(3) -0.0002(3) -0.0016(3) Ni2 0.0363(3) 0.0501(4) 0.0371(3) -0.0043(3) -0.0088(3) -0.0003(3) Ni3 0.0542(5) 0.0843(7) 0.0453(4) -0.0216(4) -0.0145(4) 0.0169(4) N1 0.043(3) 0.054(3) 0.043(3) 0.004(2) -0.002(2) -0.003(2) N2 0.057(3) 0.055(3) 0.047(3) -0.005(2) -0.019(3) 0.012(2) N3 0.106(5) 0.093(5) 0.061(4) -0.033(4) -0.043(4) 0.049(4) N4 0.039(2) 0.051(3) 0.045(3) 0.003(2) 0.002(2) -0.002(2) N5 0.033(2) 0.063(3) 0.035(2) -0.007(2) 0.001(2) -0.004(2) N6 0.037(3) 0.094(4) 0.051(3) -0.033(3) -0.006(3) 0.011(2) N7 0.035(2) 0.055(3) 0.037(2) 0.013(2) 0.000(2) -0.004(2) N8 0.036(2) 0.051(3) 0.033(2) -0.004(2) -0.004(2) -0.004(2) N9 0.048(3) 0.078(4) 0.033(2) -0.019(2) 0.002(2) 0.003(3) N10 0.038(2) 0.070(4) 0.055(3) 0.025(3) -0.010(2) -0.014(2) N11 0.055(3) 0.048(3) 0.057(3) 0.000(3) -0.019(3) -0.005(2) N12 0.080(5) 0.077(4) 0.057(4) -0.027(3) -0.024(3) 0.009(3) O1 0.055(3) 0.061(3) 0.067(3) 0.009(2) 0.019(2) 0.013(2) O2 0.069(3) 0.073(3) 0.056(3) -0.020(2) 0.004(2) 0.010(3) O3 0.094(5) 0.180(8) 0.122(6) -0.075(6) -0.025(5) 0.063(5) O4 0.041(3) 0.230(10) 0.104(6) -0.068(6) 0.001(3) 0.017(4) O5 0.049(3) 0.089(4) 0.077(4) 0.042(3) 0.015(2) -0.003(2) O6 0.042(3) 0.125(5) 0.163(7) 0.043(5) -0.017(4) -0.031(3) O7 0.184(8) 0.095(5) 0.098(5) -0.059(4) -0.058(5) 0.046(5) O8 0.124(6) 0.169(8) 0.108(6) -0.050(6) 0.000(5) 0.074(6) S1 0.0549(8) 0.0516(8) 0.0416(7) 0.0028(6) 0.0076(7) 0.0025(7) S2 0.0561(12) 0.153(3) 0.0998(18) -0.0583(19) -0.0181(14) 0.0419(14) S3 0.0445(9) 0.0704(13) 0.0987(15) 0.0432(11) 0.0047(10) -0.0107(8) S4 0.146(2) 0.0898(16) 0.0614(12) -0.0355(11) -0.0309(14) 0.0497(16) C1 0.058(4) 0.057(4) 0.042(3) 0.002(3) 0.006(3) 0.011(3) C2 0.074(4) 0.060(4) 0.043(3) 0.003(3) -0.002(3) 0.006(3) C3 0.066(4) 0.059(4) 0.047(3) 0.008(3) -0.015(3) -0.003(3) C4 0.080(5) 0.059(4) 0.044(3) -0.004(3) -0.021(3) 0.004(4) C5 0.046(3) 0.048(3) 0.055(4) -0.001(3) -0.020(3) 0.006(3) C6 0.084(5) 0.060(4) 0.057(4) -0.006(4) -0.032(4) 0.021(4) C7 0.159(9) 0.066(5) 0.067(5) -0.006(4) -0.032(6) 0.036(6) C8 0.31(2) 0.060(6) 0.104(9) -0.021(6) -0.102(12) 0.064(9) C9 0.27(2) 0.076(7) 0.131(12) -0.047(8) -0.065(12) 0.091(10) C10 0.149(10) 0.118(9) 0.105(8) -0.053(7) -0.051(8) 0.091(8) C11 0.033(2) 0.052(3) 0.035(2) 0.003(2) -0.005(2) -0.006(2) C12 0.051(3) 0.066(4) 0.041(3) -0.006(3) 0.006(3) -0.019(3) C13 0.046(3) 0.095(5) 0.046(3) -0.017(3) -0.003(3) -0.016(3) C14 0.032(3) 0.108(6) 0.048(3) -0.016(4) -0.002(3) -0.008(3) C15 0.034(3) 0.085(5) 0.036(3) -0.016(3) -0.005(2) 0.006(3) C16 0.079(5) 0.052(4) 0.063(4) 0.011(3) 0.015(4) 0.004(3) C17 0.085(7) 0.107(8) 0.211(17) -0.077(10) 0.058(9) -0.005(6) C18 0.036(3) 0.093(5) 0.053(4) 0.026(4) -0.004(3) 0.001(3) C19 0.039(3) 0.114(7) 0.071(5) 0.032(5) -0.013(3) 0.008(4) C20 0.045(3) 0.084(5) 0.056(4) 0.012(3) -0.008(3) -0.002(3) C21 0.041(3) 0.068(4) 0.041(3) 0.001(3) -0.008(3) -0.010(3) C22 0.038(3) 0.045(3) 0.041(3) 0.003(2) -0.012(2) -0.011(2) C23 0.041(3) 0.065(4) 0.025(2) -0.008(2) -0.005(2) -0.009(3) C24 0.042(3) 0.070(4) 0.034(3) -0.011(3) 0.003(3) -0.009(3) C25 0.059(4) 0.110(6) 0.040(3) -0.011(4) 0.001(3) -0.010(4) C26 0.041(3) 0.116(6) 0.051(4) -0.031(4) 0.001(3) 0.000(4) C27 0.048(4) 0.110(6) 0.036(3) -0.022(4) 0.001(3) 0.002(4) C28 0.062(4) 0.069(4) 0.062(4) 0.006(4) -0.017(4) -0.020(3) C29 0.107(8) 0.096(8) 0.140(10) 0.000(7) -0.021(8) -0.056(7) C30 0.173(14) 0.115(11) 0.192(16) -0.008(11) -0.039(13) -0.106(11) C31 0.177(13) 0.073(7) 0.128(10) -0.029(7) -0.054(10) -0.036(8) C32 0.113(8) 0.054(4) 0.085(6) -0.004(4) -0.053(6) 0.003(5) C33 0.095(7) 0.090(7) 0.119(8) 0.068(6) 0.040(6) 0.018(5) C34 0.153(9) 0.079(6) 0.052(5) -0.023(4) -0.030(6) 0.027(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 N4 1.906(5) . ? Ni1 N10 1.909(6) . ? Ni1 N7 1.928(5) . ? Ni1 N1 1.932(5) . ? Ni1 Ni2 2.3464(11) . ? Ni2 N2 1.885(5) . ? Ni2 N8 1.887(5) . ? Ni2 N11 1.938(5) . ? Ni2 N5 1.944(5) . ? Ni2 Ni3 2.3611(11) . ? Ni3 N12 1.915(7) . ? Ni3 N9 1.928(6) . ? Ni3 N6 1.945(5) . ? Ni3 N3 1.948(9) . ? N1 C5 1.348(8) . ? N1 C1 1.353(8) . ? N2 C6 1.371(9) . ? N2 C5 1.374(9) . ? N3 C10 1.369(12) . ? N3 C6 1.378(11) . ? N4 C11 1.404(7) . ? N4 S1 1.605(5) . ? N5 C15 1.366(8) . ? N5 C11 1.369(8) . ? N6 C15 1.371(9) . ? N6 S2 1.599(5) . ? N7 C18 1.347(8) . ? N7 C22 1.348(8) . ? N8 C22 1.359(8) . ? N8 C23 1.364(8) . ? N9 C27 1.351(9) . ? N9 C23 1.379(8) . ? N10 C28 1.395(11) . ? N10 S3 1.619(6) . ? N11 C28 1.369(10) . ? N11 C32 1.378(11) . ? N12 C32 1.396(13) . ? N12 S4 1.607(7) . ? O1 S1 1.441(5) . ? O2 S1 1.455(5) . ? O3 S2 1.468(8) . ? O4 S2 1.407(9) . ? O5 S3 1.428(7) . ? O6 S3 1.396(6) . ? O7 S4 1.412(8) . ? O8 S4 1.460(10) . ? S1 C16 1.764(7) . ? S2 C17 1.492(19) . ? S3 C33 1.769(8) . ? S4 C34 1.767(9) . ? C1 C2 1.349(10) . ? C1 H1A 0.9500 . ? C2 C3 1.387(11) . ? C2 H2A 0.9500 . ? C3 C4 1.386(10) . ? C3 H3A 0.9500 . ? C4 C5 1.412(9) . ? C4 H4A 0.9500 . ? C6 C7 1.412(13) . ? C7 C8 1.395(15) . ? C7 H7A 0.9500 . ? C8 C9 1.38(2) . ? C8 H8A 0.9500 . ? C9 C10 1.35(2) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.390(8) . ? C12 C13 1.370(10) . ? C12 H12A 0.9500 . ? C13 C14 1.409(11) . ? C13 H13A 0.9500 . ? C14 C15 1.398(9) . ? C14 H14A 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.385(10) . ? C18 H18A 0.9500 . ? C19 C20 1.396(11) . ? C19 H19A 0.9500 . ? C20 C21 1.364(9) . ? C20 H20A 0.9500 . ? C21 C22 1.416(8) . ? C21 H21A 0.9500 . ? C23 C24 1.413(9) . ? C24 C25 1.411(10) . ? C24 H24A 0.9500 . ? C25 C26 1.397(12) . ? C25 H25A 0.9500 . ? C26 C27 1.358(12) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C29 1.353(12) . ? C29 C30 1.35(2) . ? C29 H29A 0.9500 . ? C30 C31 1.33(2) . ? C30 H30A 0.9500 . ? C31 C32 1.429(15) . ? C31 H31A 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O9 C37 1.394(19) . ? O9 C38 1.438(19) . ? C36 C37 1.44(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.60(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ni1 N10 175.3(2) . . ? N4 Ni1 N7 91.2(2) . . ? N10 Ni1 N7 88.2(2) . . ? N4 Ni1 N1 89.2(2) . . ? N10 Ni1 N1 90.6(2) . . ? N7 Ni1 N1 171.7(2) . . ? N4 Ni1 Ni2 88.38(15) . . ? N10 Ni1 Ni2 86.91(19) . . ? N7 Ni1 Ni2 85.92(15) . . ? N1 Ni1 Ni2 85.81(16) . . ? N2 Ni2 N8 179.6(3) . . ? N2 Ni2 N11 88.2(2) . . ? N8 Ni2 N11 91.5(2) . . ? N2 Ni2 N5 90.8(2) . . ? N8 Ni2 N5 89.6(2) . . ? N11 Ni2 N5 178.8(3) . . ? N2 Ni2 Ni1 90.09(18) . . ? N8 Ni2 Ni1 89.92(15) . . ? N11 Ni2 Ni1 90.04(19) . . ? N5 Ni2 Ni1 89.24(15) . . ? N2 Ni2 Ni3 90.00(18) . . ? N8 Ni2 Ni3 89.98(15) . . ? N11 Ni2 Ni3 89.68(19) . . ? N5 Ni2 Ni3 91.04(15) . . ? Ni1 Ni2 Ni3 179.70(5) . . ? N12 Ni3 N9 91.0(3) . . ? N12 Ni3 N6 172.7(3) . . ? N9 Ni3 N6 88.4(3) . . ? N12 Ni3 N3 87.9(3) . . ? N9 Ni3 N3 172.7(3) . . ? N6 Ni3 N3 91.8(3) . . ? N12 Ni3 Ni2 87.8(2) . . ? N9 Ni3 Ni2 86.66(15) . . ? N6 Ni3 Ni2 84.86(15) . . ? N3 Ni3 Ni2 86.1(2) . . ? C5 N1 C1 118.1(5) . . ? C5 N1 Ni1 123.0(4) . . ? C1 N1 Ni1 118.9(4) . . ? C6 N2 C5 122.8(6) . . ? C6 N2 Ni2 118.6(5) . . ? C5 N2 Ni2 118.6(4) . . ? C10 N3 C6 118.8(10) . . ? C10 N3 Ni3 119.1(8) . . ? C6 N3 Ni3 121.9(5) . . ? C11 N4 S1 124.2(4) . . ? C11 N4 Ni1 120.9(4) . . ? S1 N4 Ni1 114.7(3) . . ? C15 N5 C11 120.7(5) . . ? C15 N5 Ni2 119.1(4) . . ? C11 N5 Ni2 120.2(4) . . ? C15 N6 S2 122.2(4) . . ? C15 N6 Ni3 123.8(4) . . ? S2 N6 Ni3 112.9(3) . . ? C18 N7 C22 119.7(5) . . ? C18 N7 Ni1 117.9(4) . . ? C22 N7 Ni1 122.2(4) . . ? C22 N8 C23 124.4(5) . . ? C22 N8 Ni2 117.7(4) . . ? C23 N8 Ni2 117.9(4) . . ? C27 N9 C23 119.4(7) . . ? C27 N9 Ni3 119.2(5) . . ? C23 N9 Ni3 121.2(4) . . ? C28 N10 S3 122.0(5) . . ? C28 N10 Ni1 124.3(5) . . ? S3 N10 Ni1 113.6(4) . . ? C28 N11 C32 120.8(7) . . ? C28 N11 Ni2 120.2(5) . . ? C32 N11 Ni2 118.3(6) . . ? C32 N12 S4 120.8(6) . . ? C32 N12 Ni3 117.1(5) . . ? S4 N12 Ni3 122.1(5) . . ? O1 S1 O2 117.5(3) . . ? O1 S1 N4 105.0(3) . . ? O2 S1 N4 112.7(3) . . ? O1 S1 C16 108.1(4) . . ? O2 S1 C16 106.9(4) . . ? N4 S1 C16 105.9(3) . . ? O4 S2 O3 115.6(5) . . ? O4 S2 C17 108.8(6) . . ? O3 S2 C17 109.3(6) . . ? O4 S2 N6 117.9(5) . . ? O3 S2 N6 101.8(4) . . ? C17 S2 N6 102.3(5) . . ? O6 S3 O5 115.9(4) . . ? O6 S3 N10 114.8(5) . . ? O5 S3 N10 104.0(3) . . ? O6 S3 C33 107.6(5) . . ? O5 S3 C33 108.3(5) . . ? N10 S3 C33 105.6(4) . . ? O7 S4 O8 117.6(5) . . ? O7 S4 N12 114.5(5) . . ? O8 S4 N12 104.4(5) . . ? O7 S4 C34 104.7(5) . . ? O8 S4 C34 109.1(6) . . ? N12 S4 C34 106.0(4) . . ? C2 C1 N1 123.9(6) . . ? C2 C1 H1A 118.0 . . ? N1 C1 H1A 118.0 . . ? C1 C2 C3 119.0(7) . . ? C1 C2 H2A 120.5 . . ? C3 C2 H2A 120.5 . . ? C4 C3 C2 118.9(6) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C3 C4 C5 119.1(7) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? N1 C5 N2 115.3(5) . . ? N1 C5 C4 120.9(6) . . ? N2 C5 C4 123.5(6) . . ? N2 C6 N3 115.2(7) . . ? N2 C6 C7 124.3(8) . . ? N3 C6 C7 120.3(7) . . ? C8 C7 C6 118.1(12) . . ? C8 C7 H7A 121.0 . . ? C6 C7 H7A 121.0 . . ? C9 C8 C7 120.6(14) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C10 C9 C8 119.1(10) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? C9 C10 N3 122.5(12) . . ? C9 C10 H10A 118.7 . . ? N3 C10 H10A 118.7 . . ? N5 C11 C12 120.4(5) . . ? N5 C11 N4 115.5(5) . . ? C12 C11 N4 124.1(6) . . ? C13 C12 C11 120.1(7) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 119.3(6) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.3 . . ? C15 C14 C13 119.6(6) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? N5 C15 N6 114.8(5) . . ? N5 C15 C14 119.8(6) . . ? N6 C15 C14 125.3(6) . . ? S1 C16 H16A 109.5 . . ? S1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S2 C17 H17A 109.5 . . ? S2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 C19 123.4(6) . . ? N7 C18 H18A 118.3 . . ? C19 C18 H18A 118.3 . . ? C18 C19 C20 117.0(6) . . ? C18 C19 H19A 121.5 . . ? C20 C19 H19A 121.5 . . ? C21 C20 C19 119.6(6) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C20 C21 C22 120.8(6) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? N7 C22 N8 116.5(5) . . ? N7 C22 C21 118.9(5) . . ? N8 C22 C21 124.3(6) . . ? N8 C23 N9 116.7(5) . . ? N8 C23 C24 123.7(6) . . ? N9 C23 C24 119.6(5) . . ? C25 C24 C23 120.3(7) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C26 C25 C24 117.0(8) . . ? C26 C25 H25A 121.5 . . ? C24 C25 H25A 121.5 . . ? C27 C26 C25 121.1(7) . . ? C27 C26 H26A 119.4 . . ? C25 C26 H26A 119.4 . . ? N9 C27 C26 122.5(7) . . ? N9 C27 H27A 118.8 . . ? C26 C27 H27A 118.8 . . ? C29 C28 N11 121.9(10) . . ? C29 C28 N10 124.5(9) . . ? N11 C28 N10 113.6(6) . . ? C30 C29 C28 117.8(12) . . ? C30 C29 H29A 121.1 . . ? C28 C29 H29A 121.1 . . ? C31 C30 C29 122.4(10) . . ? C31 C30 H30A 118.8 . . ? C29 C30 H30A 118.8 . . ? C30 C31 C32 121.2(13) . . ? C30 C31 H31A 119.4 . . ? C32 C31 H31A 119.4 . . ? N11 C32 N12 117.1(7) . . ? N11 C32 C31 115.3(11) . . ? N12 C32 C31 127.4(10) . . ? S3 C33 H33A 109.5 . . ? S3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? S3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? S4 C34 H34A 109.5 . . ? S4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? S4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 O9 C38 102.0(13) . . ? C37 C36 H36A 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C37 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O9 C37 C36 93.8(15) . . ? O9 C37 H37A 113.0 . . ? C36 C37 H37A 113.0 . . ? O9 C37 H37B 113.0 . . ? C36 C37 H37B 113.0 . . ? H37A C37 H37B 110.4 . . ? O9 C38 C39 94.1(13) . . ? O9 C38 H38A 112.9 . . ? C39 C38 H38A 112.9 . . ? O9 C38 H38B 112.9 . . ? C39 C38 H38B 112.9 . . ? H38A C38 H38B 110.3 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.896 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.108 #===END