# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email yshxie@ecust.edu.cn _publ_contact_author_name 'Yongshu Xie' _publ_author_name 'Yongshu Xie' data_co _database_code_depnum_ccdc_archive 'CCDC 886465' #TrackingRef '- 3-Xie-CCDC 886465-886468.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H38 Cl Co N4 O11' _chemical_formula_weight 664.97 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' _cell_length_a 12.9687(12) _cell_length_b 7.9248(7) _cell_length_c 14.4847(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.2220(10) _cell_angle_gamma 90.00 _cell_volume 1429.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8040 _exptl_absorpt_correction_T_max 0.9630 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13170 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3291 _reflns_number_gt 2574 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0774P)^2^+2.0095P] 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 3291 _refine_ls_number_parameters 218 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1687 _refine_ls_wR_factor_gt 0.1545 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.089 _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 Co1 Co 0.5000 0.72986(8) 0.2500 0.0302(2) Uani 1 2 d S . . Cl1 Cl 1.0000 0.6545(2) 0.2500 0.0784(6) Uani 1 2 d SD . . O1 O 0.2180(2) 1.0685(4) 0.1996(2) 0.0557(8) Uani 1 1 d . . . O2 O 0.3929(2) 0.8989(3) 0.21654(17) 0.0383(6) Uani 1 1 d . . . O3 O 0.4570(5) 0.1992(7) 0.3200(4) 0.0505(14) Uani 0.50 1 d P A -1 H3A H 0.4390 0.1043 0.2992 0.061 Uiso 0.50 1 calc PR A -1 O4 O 0.9939(10) 0.7288(15) 0.3364(7) 0.117(4) Uani 0.50 1 d PDU B -2 O5 O 0.8949(6) 0.6175(13) 0.1963(7) 0.136(4) Uani 0.50 1 d PDU B -2 O6 O 1.0565(7) 0.5058(10) 0.2706(7) 0.124(4) Uani 0.50 1 d PDU B -2 O7 O 1.0473(9) 0.7640(16) 0.2013(10) 0.182(10) Uani 0.50 1 d PD B -2 O8 O 0.8194(4) 0.5874(8) 0.4078(4) 0.1121(17) Uani 1 1 d . . . H8 H 0.8709 0.5761 0.3860 0.168 Uiso 1 1 calc R . . N1 N 0.5237(3) 0.7328(4) 0.1264(2) 0.0402(7) Uani 1 1 d . . . N2 N 0.6138(2) 0.5591(4) 0.2806(2) 0.0419(7) Uani 1 1 d . . . H2 H 0.6681 0.6044 0.3282 0.050 Uiso 1 1 calc R . . C1 C 0.1216(4) 1.1595(7) 0.1930(5) 0.0735(15) Uani 1 1 d . . . H1A H 0.1138 1.1771 0.2563 0.110 Uiso 1 1 calc R . . H1B H 0.0614 1.0961 0.1553 0.110 Uiso 1 1 calc R . . H1C H 0.1245 1.2666 0.1629 0.110 Uiso 1 1 calc R . . C2 C 0.2400(3) 1.0282(5) 0.1166(3) 0.0447(9) Uani 1 1 d . . . C3 C 0.1785(4) 1.0721(6) 0.0261(4) 0.0602(12) Uani 1 1 d . . . H3 H 0.1154 1.1327 0.0191 0.072 Uiso 1 1 calc R . . C4 C 0.2093(4) 1.0271(7) -0.0548(4) 0.0702(14) Uani 1 1 d . . . H4 H 0.1664 1.0570 -0.1155 0.084 Uiso 1 1 calc R . . C5 C 0.3014(4) 0.9402(6) -0.0461(3) 0.0609(12) Uani 1 1 d . . . H5A H 0.3218 0.9118 -0.1007 0.073 Uiso 1 1 calc R . . C6 C 0.3664(3) 0.8924(5) 0.0454(3) 0.0414(8) Uani 1 1 d . . . C7 C 0.3366(3) 0.9352(4) 0.1288(3) 0.0353(7) Uani 1 1 d . . . C8 C 0.4642(3) 0.8041(5) 0.0509(3) 0.0452(9) Uani 1 1 d . . . H8A H 0.4862 0.7980 -0.0048 0.054 Uiso 1 1 calc R . . C9 C 0.6302(4) 0.6667(8) 0.1278(4) 0.0766(17) Uani 1 1 d . . . H9A H 0.6287 0.6246 0.0646 0.092 Uiso 1 1 calc R . . H9B H 0.6831 0.7563 0.1446 0.092 Uiso 1 1 calc R . . C10 C 0.6583(5) 0.5350(7) 0.1960(4) 0.0792(18) Uani 1 1 d . . . H10A H 0.7360 0.5278 0.2190 0.095 Uiso 1 1 calc R . . H10B H 0.6320 0.4290 0.1647 0.095 Uiso 1 1 calc R . . C11 C 0.5888(3) 0.3950(4) 0.3178(3) 0.0415(8) Uani 1 1 d . A . H11A H 0.5688 0.4151 0.3766 0.050 Uiso 1 1 calc R . . H11B H 0.6535 0.3271 0.3344 0.050 Uiso 1 1 calc R . . C12 C 0.5000 0.2939(6) 0.2500 0.0425(12) Uani 1 2 d S . . H12 H 0.5310 0.2148 0.2131 0.051 Uiso 0.50 1 calc PR A . C13 C 0.8522(8) 0.5778(12) 0.5027(5) 0.136(4) Uani 1 1 d . . . H13A H 0.8901 0.6792 0.5282 0.204 Uiso 1 1 calc R . . H13B H 0.8992 0.4826 0.5214 0.204 Uiso 1 1 calc R . . H13C H 0.7913 0.5646 0.5274 0.204 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 Co1 0.0326(4) 0.0226(3) 0.0346(3) 0.000 0.0083(3) 0.000 Cl1 0.0488(10) 0.0609(11) 0.1267(18) 0.000 0.0262(10) 0.000 O1 0.0450(16) 0.0521(17) 0.071(2) 0.0028(15) 0.0183(15) 0.0141(13) O2 0.0457(14) 0.0306(12) 0.0378(13) 0.0005(10) 0.0104(11) 0.0101(11) O3 0.073(4) 0.033(3) 0.049(3) -0.001(2) 0.024(3) -0.014(3) O4 0.105(7) 0.097(7) 0.149(8) -0.058(6) 0.038(6) 0.004(6) O5 0.116(6) 0.142(7) 0.141(7) 0.015(6) 0.023(5) -0.024(6) O6 0.134(7) 0.096(6) 0.146(8) 0.013(6) 0.047(6) 0.052(5) O7 0.133(13) 0.097(9) 0.36(3) 0.008(13) 0.135(16) -0.051(9) O8 0.073(3) 0.126(4) 0.123(4) -0.019(3) 0.003(3) -0.002(3) N1 0.0403(17) 0.0407(17) 0.0397(16) -0.0062(13) 0.0114(13) 0.0044(13) N2 0.0348(16) 0.0319(16) 0.058(2) 0.0072(14) 0.0109(15) 0.0004(12) C1 0.053(3) 0.071(3) 0.103(4) 0.008(3) 0.031(3) 0.021(3) C2 0.039(2) 0.0323(18) 0.058(2) 0.0019(17) 0.0069(18) -0.0010(15) C3 0.046(2) 0.055(3) 0.067(3) 0.005(2) -0.006(2) 0.011(2) C4 0.069(3) 0.073(3) 0.053(3) 0.014(2) -0.009(2) 0.016(3) C5 0.069(3) 0.066(3) 0.041(2) 0.006(2) 0.005(2) 0.007(2) C6 0.045(2) 0.0359(19) 0.0408(19) 0.0037(15) 0.0071(16) -0.0015(16) C7 0.0356(18) 0.0258(16) 0.0419(19) 0.0022(14) 0.0067(15) -0.0031(13) C8 0.056(2) 0.044(2) 0.0363(19) -0.0023(16) 0.0140(17) -0.0004(18) C9 0.069(3) 0.113(5) 0.055(3) 0.008(3) 0.028(2) 0.040(3) C10 0.073(3) 0.080(4) 0.106(4) 0.044(3) 0.060(3) 0.034(3) C11 0.045(2) 0.0285(17) 0.050(2) 0.0080(15) 0.0125(17) 0.0060(15) C12 0.059(3) 0.022(2) 0.052(3) 0.000 0.023(3) 0.000 C13 0.170(8) 0.135(7) 0.082(5) -0.005(5) 0.000(5) 0.084(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.892(2) 4_656 ? Co1 O2 1.892(2) . ? Co1 N1 1.900(3) . ? Co1 N1 1.900(3) 4_656 ? Co1 N2 1.960(3) 4_656 ? Co1 N2 1.960(3) . ? Cl1 O7 1.367(7) . ? Cl1 O7 1.367(7) 4_756 ? Cl1 O6 1.376(7) . ? Cl1 O6 1.376(7) 4_756 ? Cl1 O5 1.399(7) . ? Cl1 O5 1.399(7) 4_756 ? Cl1 O4 1.405(7) 4_756 ? Cl1 O4 1.405(7) . ? O1 C2 1.349(5) . ? O1 C1 1.424(5) . ? O2 C7 1.309(4) . ? O3 C12 1.490(6) . ? O8 C13 1.323(8) . ? N1 C8 1.280(5) . ? N1 C9 1.471(6) . ? N2 C11 1.478(5) . ? N2 C10 1.506(6) . ? C2 C3 1.375(6) . ? C2 C7 1.421(5) . ? C3 C4 1.386(7) . ? C4 C5 1.353(7) . ? C5 C6 1.409(6) . ? C6 C7 1.408(5) . ? C6 C8 1.431(6) . ? C9 C10 1.413(7) . ? C11 C12 1.517(5) . ? C12 O3 1.490(6) 4_656 ? C12 C11 1.517(5) 4_656 ? 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 O2 Co1 O2 89.87(16) 4_656 . ? O2 Co1 N1 86.11(12) 4_656 . ? O2 Co1 N1 92.89(12) . . ? O2 Co1 N1 92.89(12) 4_656 4_656 ? O2 Co1 N1 86.11(12) . 4_656 ? N1 Co1 N1 178.60(19) . 4_656 ? O2 Co1 N2 177.50(12) 4_656 4_656 ? O2 Co1 N2 88.76(12) . 4_656 ? N1 Co1 N2 96.04(14) . 4_656 ? N1 Co1 N2 84.94(14) 4_656 4_656 ? O2 Co1 N2 88.76(12) 4_656 . ? O2 Co1 N2 177.50(12) . . ? N1 Co1 N2 84.94(14) . . ? N1 Co1 N2 96.04(14) 4_656 . ? N2 Co1 N2 92.68(18) 4_656 . ? O7 Cl1 O7 101.2(13) . 4_756 ? O7 Cl1 O6 111.6(5) . . ? O7 Cl1 O6 136.1(8) 4_756 . ? O7 Cl1 O6 136.1(8) . 4_756 ? O7 Cl1 O6 111.6(5) 4_756 4_756 ? O6 Cl1 O6 62.1(8) . 4_756 ? O7 Cl1 O5 110.7(5) . . ? O7 Cl1 O5 85.0(7) 4_756 . ? O6 Cl1 O5 108.5(5) . . ? O6 Cl1 O5 47.4(6) 4_756 . ? O7 Cl1 O5 85.0(7) . 4_756 ? O7 Cl1 O5 110.7(5) 4_756 4_756 ? O6 Cl1 O5 47.4(6) . 4_756 ? O6 Cl1 O5 108.5(5) 4_756 4_756 ? O5 Cl1 O5 155.8(8) . 4_756 ? O7 Cl1 O4 29.5(8) . 4_756 ? O7 Cl1 O4 109.8(5) 4_756 4_756 ? O6 Cl1 O4 113.1(8) . 4_756 ? O6 Cl1 O4 108.9(5) 4_756 4_756 ? O5 Cl1 O4 83.2(5) . 4_756 ? O5 Cl1 O4 107.1(5) 4_756 4_756 ? O7 Cl1 O4 109.8(5) . . ? O7 Cl1 O4 29.5(8) 4_756 . ? O6 Cl1 O4 108.9(5) . . ? O6 Cl1 O4 113.1(8) 4_756 . ? O5 Cl1 O4 107.1(5) . . ? O5 Cl1 O4 83.2(5) 4_756 . ? O4 Cl1 O4 130.5(11) 4_756 . ? C2 O1 C1 117.4(4) . . ? C7 O2 Co1 125.1(2) . . ? C8 N1 C9 120.6(4) . . ? C8 N1 Co1 126.3(3) . . ? C9 N1 Co1 112.4(3) . . ? C11 N2 C10 111.0(3) . . ? C11 N2 Co1 117.5(2) . . ? C10 N2 Co1 109.8(3) . . ? O1 C2 C3 125.4(4) . . ? O1 C2 C7 114.3(3) . . ? C3 C2 C7 120.4(4) . . ? C2 C3 C4 120.9(4) . . ? C5 C4 C3 120.4(4) . . ? C4 C5 C6 120.4(5) . . ? C7 C6 C5 120.4(4) . . ? C7 C6 C8 121.4(3) . . ? C5 C6 C8 118.2(4) . . ? O2 C7 C6 124.5(3) . . ? O2 C7 C2 117.9(3) . . ? C6 C7 C2 117.5(3) . . ? N1 C8 C6 125.3(4) . . ? C10 C9 N1 109.4(4) . . ? C9 C10 N2 113.1(4) . . ? N2 C11 C12 115.7(3) . . ? O3 C12 O3 119.5(6) 4_656 . ? O3 C12 C11 110.3(3) 4_656 . ? O3 C12 C11 100.7(3) . . ? O3 C12 C11 100.7(3) 4_656 4_656 ? O3 C12 C11 110.3(3) . 4_656 ? C11 C12 C11 116.2(4) . 4_656 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.788 _refine_diff_density_min -0.650 _refine_diff_density_rms 0.081 #END data_ni _database_code_depnum_ccdc_archive 'CCDC 886466' #TrackingRef '- 3-Xie-CCDC 886465-886468.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15.50 H28 Cl2 N4 Ni O11.50' _chemical_formula_weight 584.03 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.6242(12) _cell_length_b 11.8799(8) _cell_length_c 11.8432(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.9330(10) _cell_angle_gamma 90.00 _cell_volume 2345.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6950 _exptl_absorpt_correction_T_max 0.8961 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22074 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5392 _reflns_number_gt 4094 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0669P)^2^+1.7279P] 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 5392 _refine_ls_number_parameters 359 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.70283(2) 0.48286(3) 0.37767(3) 0.03605(13) Uani 1 1 d . . . Cl1 Cl 0.68904(5) 0.66038(7) 0.84542(8) 0.0506(2) Uani 1 1 d . . . Cl2 Cl 0.9558(5) 0.2880(8) 0.6768(7) 0.106(3) Uani 0.50 1 d PDU A 1 Cl2' Cl 0.9479(4) 0.2823(6) 0.6908(6) 0.0745(14) Uani 0.50 1 d PDU . . O1 O 0.73959(15) 0.3617(2) 0.7437(2) 0.0601(6) Uani 1 1 d . . . O2 O 0.70569(12) 0.43280(19) 0.52607(17) 0.0434(5) Uani 1 1 d . . . O3 O 0.84867(17) 0.6237(3) 0.2534(3) 0.0769(8) Uani 1 1 d . . . H3O H 0.8970 0.6434 0.2791 0.115 Uiso 1 1 calc R . . O4 O 0.77151(15) 0.6306(3) 0.8982(2) 0.0697(7) Uani 1 1 d . . . O5 O 0.6742(2) 0.6857(5) 0.7261(3) 0.139(2) Uani 1 1 d . . . O6 O 0.6725(2) 0.7571(4) 0.9017(5) 0.1371(18) Uani 1 1 d . . . O7 O 0.63849(18) 0.5733(3) 0.8568(3) 0.0930(10) Uani 1 1 d . . . O8 O 0.9711(7) 0.4071(7) 0.7041(11) 0.124(4) Uani 0.50 1 d PDU A 1 O9 O 0.8726(4) 0.2773(9) 0.6252(10) 0.103(3) Uani 0.50 1 d PDU A 1 O10 O 0.9833(6) 0.2284(8) 0.7834(8) 0.121(3) Uani 0.50 1 d PDU A 1 O11 O 0.9975(7) 0.2586(12) 0.6005(11) 0.205(6) Uani 0.50 1 d PDU A 1 O8' O 0.9683(7) 0.3868(8) 0.6543(10) 0.121(4) Uani 0.50 1 d PDU A 2 O9' O 0.8813(6) 0.2367(10) 0.6016(10) 0.143(6) Uani 0.50 1 d PDU A 2 O10' O 0.9278(8) 0.2950(10) 0.7977(8) 0.172(4) Uani 0.50 1 d PDU A 2 O11' O 1.0120(5) 0.2082(9) 0.7143(12) 0.155(4) Uani 0.50 1 d PDU A 2 N1 N 0.59185(15) 0.4802(2) 0.3159(2) 0.0407(5) Uani 1 1 d . . . N2 N 0.70065(16) 0.5312(3) 0.2221(2) 0.0484(6) Uani 1 1 d D . . H2 H 0.7106 0.6039 0.2264 0.058 Uiso 1 1 calc RD . . N3 N 0.81962(14) 0.4890(2) 0.4473(2) 0.0390(5) Uani 1 1 d D . . H3 H 0.8307 0.4390 0.5052 0.047 Uiso 1 1 calc RD . . N4 N 0.83303(19) 0.5527(3) 0.7059(3) 0.0648(8) Uani 1 1 d D . . H41 H 0.8795 0.5199 0.7158 0.078 Uiso 1 1 calc RD . . H42 H 0.7952 0.5012 0.6917 0.078 Uiso 1 1 calc RD . . H43 H 0.8352 0.5901 0.7710 0.078 Uiso 1 1 calc RD . . C1 C 0.7587(3) 0.3345(4) 0.8678(3) 0.0704(11) Uani 1 1 d . . . H1A H 0.8140 0.3574 0.9107 0.106 Uiso 1 1 calc R . . H1B H 0.7532 0.2532 0.8766 0.106 Uiso 1 1 calc R . . H1C H 0.7219 0.3744 0.9007 0.106 Uiso 1 1 calc R . . C2 C 0.6622(2) 0.3458(3) 0.6719(3) 0.0463(7) Uani 1 1 d . . . C3 C 0.6031(2) 0.2940(3) 0.7061(3) 0.0551(8) Uani 1 1 d . . . H3A H 0.6154 0.2658 0.7851 0.066 Uiso 1 1 calc R . . C4 C 0.5263(2) 0.2827(3) 0.6267(4) 0.0589(9) Uani 1 1 d . . . H4 H 0.4867 0.2437 0.6501 0.071 Uiso 1 1 calc R . . C5 C 0.5071(2) 0.3273(3) 0.5149(3) 0.0524(8) Uani 1 1 d . . . H5 H 0.4537 0.3221 0.4617 0.063 Uiso 1 1 calc R . . C6 C 0.56653(17) 0.3815(3) 0.4775(3) 0.0415(6) Uani 1 1 d . . . C7 C 0.64590(17) 0.3878(2) 0.5543(3) 0.0394(6) Uani 1 1 d . . . C8 C 0.54318(18) 0.4347(3) 0.3632(3) 0.0444(7) Uani 1 1 d . . . H8 H 0.4876 0.4368 0.3189 0.053 Uiso 1 1 calc R . . C9 C 0.5600(2) 0.5384(4) 0.2002(3) 0.0566(9) Uani 1 1 d . . . H9A H 0.5558 0.6203 0.2122 0.068 Uiso 1 1 calc R . . H9B H 0.5061 0.5091 0.1546 0.068 Uiso 1 1 calc R . . C10 C 0.6183(2) 0.5149(4) 0.1354(3) 0.0608(10) Uani 1 1 d . . . H10A H 0.6117 0.4368 0.1047 0.073 Uiso 1 1 calc R . . H10B H 0.6091 0.5671 0.0671 0.073 Uiso 1 1 calc R . . C11 C 0.7604(3) 0.4761(4) 0.1741(3) 0.0648(10) Uani 1 1 d . . . H11A H 0.7525 0.3935 0.1718 0.078 Uiso 1 1 calc R . . H11B H 0.7514 0.5023 0.0914 0.078 Uiso 1 1 calc R . . C12 C 0.8438(2) 0.5029(3) 0.2489(3) 0.0622(10) Uani 1 1 d . . . H12A H 0.8810 0.4744 0.2071 0.075 Uiso 1 1 calc R . . C13 C 0.8684(2) 0.4521(3) 0.3720(3) 0.0500(8) Uani 1 1 d . . . H13A H 0.8648 0.3691 0.3641 0.060 Uiso 1 1 calc R . . H13B H 0.9252 0.4715 0.4138 0.060 Uiso 1 1 calc R . . C14 C 0.8512(2) 0.5974(3) 0.5101(3) 0.0512(8) Uani 1 1 d . . . H14A H 0.8417 0.6581 0.4498 0.061 Uiso 1 1 calc R . . H14B H 0.9100 0.5902 0.5485 0.061 Uiso 1 1 calc R . . C15 C 0.8148(2) 0.6318(3) 0.6032(3) 0.0586(9) Uani 1 1 d . . . H15A H 0.8349 0.7076 0.6332 0.070 Uiso 1 1 calc R . . H15B H 0.7559 0.6371 0.5657 0.070 Uiso 1 1 calc R . . O12 O 1.0311(12) 0.0274(17) 0.5059(18) 0.223(6) Uani 0.50 1 d PU B -1 H12 H 1.0410 0.0967 0.5089 0.334 Uiso 0.50 1 calc PR B -1 C16 C 0.9759(17) 0.000(2) 0.390(2) 0.223(6) Uani 0.50 1 d P B -1 H16A H 0.9218 -0.0089 0.3959 0.334 Uiso 0.50 1 calc PR B -1 H16B H 0.9923 -0.0713 0.3628 0.334 Uiso 0.50 1 calc PR B -1 H16C H 0.9757 0.0598 0.3339 0.334 Uiso 0.50 1 calc PR B -1 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 0.0330(2) 0.0430(2) 0.0331(2) -0.00122(14) 0.01195(15) -0.00253(15) Cl1 0.0408(4) 0.0559(5) 0.0536(5) 0.0007(3) 0.0132(3) -0.0011(3) Cl2 0.073(3) 0.131(5) 0.104(4) 0.043(3) 0.016(2) -0.018(3) Cl2' 0.0400(15) 0.092(3) 0.081(2) 0.039(2) 0.0055(16) -0.0029(15) O1 0.0546(14) 0.0857(18) 0.0385(12) 0.0106(12) 0.0132(11) -0.0024(12) O2 0.0347(10) 0.0602(13) 0.0359(10) 0.0010(9) 0.0121(8) -0.0071(9) O3 0.0606(16) 0.0781(19) 0.095(2) 0.0333(16) 0.0292(16) -0.0037(14) O4 0.0439(13) 0.092(2) 0.0678(17) -0.0021(14) 0.0101(12) 0.0091(13) O5 0.083(3) 0.256(6) 0.073(2) 0.062(3) 0.0168(19) 0.013(3) O6 0.073(2) 0.105(3) 0.214(5) -0.075(3) 0.020(3) 0.009(2) O7 0.0693(19) 0.090(2) 0.116(3) 0.023(2) 0.0244(18) -0.0193(17) O8 0.100(6) 0.112(7) 0.157(9) -0.006(6) 0.038(6) -0.011(5) O9 0.062(4) 0.103(6) 0.125(7) 0.013(5) 0.004(4) -0.007(4) O10 0.112(6) 0.122(6) 0.097(5) 0.053(5) -0.010(5) -0.006(5) O11 0.199(9) 0.242(10) 0.214(9) -0.004(8) 0.124(8) -0.002(8) O8' 0.117(7) 0.121(7) 0.109(7) 0.065(5) 0.016(5) -0.035(6) O9' 0.106(7) 0.150(9) 0.131(8) -0.017(6) -0.021(5) -0.020(6) O10' 0.202(9) 0.188(9) 0.150(7) 0.021(7) 0.088(7) -0.033(7) O11' 0.101(6) 0.154(7) 0.179(8) 0.012(7) 0.003(6) 0.059(6) N1 0.0360(12) 0.0473(14) 0.0356(13) -0.0024(10) 0.0071(10) -0.0022(10) N2 0.0458(15) 0.0607(17) 0.0403(14) 0.0060(12) 0.0160(12) -0.0017(12) N3 0.0353(12) 0.0438(13) 0.0407(13) 0.0043(10) 0.0161(10) 0.0006(10) N4 0.0539(18) 0.088(2) 0.0535(18) -0.0170(17) 0.0187(14) -0.0063(16) C1 0.090(3) 0.073(3) 0.043(2) 0.0150(17) 0.0142(19) 0.004(2) C2 0.0494(18) 0.0483(18) 0.0451(17) 0.0023(13) 0.0205(14) 0.0032(14) C3 0.070(2) 0.0509(19) 0.056(2) 0.0100(15) 0.0363(18) 0.0016(17) C4 0.059(2) 0.054(2) 0.078(3) 0.0028(18) 0.041(2) -0.0066(16) C5 0.0415(17) 0.055(2) 0.066(2) -0.0044(16) 0.0245(16) -0.0064(14) C6 0.0387(15) 0.0428(16) 0.0453(16) -0.0041(13) 0.0166(13) -0.0035(12) C7 0.0403(15) 0.0407(15) 0.0415(15) -0.0040(12) 0.0193(12) -0.0020(12) C8 0.0332(14) 0.0484(17) 0.0495(17) -0.0075(14) 0.0104(13) -0.0048(12) C9 0.0439(18) 0.075(2) 0.0432(18) 0.0089(16) 0.0042(14) -0.0012(16) C10 0.056(2) 0.085(3) 0.0366(17) 0.0073(16) 0.0076(15) -0.0070(18) C11 0.071(3) 0.087(3) 0.047(2) 0.0028(18) 0.0324(19) 0.004(2) C12 0.060(2) 0.080(3) 0.060(2) 0.0183(18) 0.0385(19) 0.0132(18) C13 0.0446(17) 0.0554(19) 0.0573(19) 0.0080(15) 0.0265(15) 0.0079(14) C14 0.0423(17) 0.0508(18) 0.059(2) -0.0033(15) 0.0142(15) -0.0093(14) C15 0.0514(19) 0.055(2) 0.063(2) -0.0178(17) 0.0098(17) -0.0046(16) O12 0.216(10) 0.241(10) 0.201(10) -0.018(9) 0.055(8) -0.028(8) C16 0.216(10) 0.241(10) 0.201(10) -0.018(9) 0.055(8) -0.028(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 1.841(2) . ? Ni1 N1 1.853(3) . ? Ni1 N2 1.918(3) . ? Ni1 N3 1.955(2) . ? Cl1 O5 1.384(4) . ? Cl1 O7 1.400(3) . ? Cl1 O6 1.406(4) . ? Cl1 O4 1.428(3) . ? Cl2 O11 1.382(8) . ? Cl2 O10 1.391(7) . ? Cl2 O9 1.400(7) . ? Cl2 O8 1.456(8) . ? Cl2' O10 1.248(10) . ? Cl2' O9 1.304(11) . ? Cl2' O11' 1.386(7) . ? Cl2' O8' 1.399(7) . ? Cl2' O9' 1.407(7) . ? Cl2' O10' 1.429(8) . ? Cl2' O8 1.533(14) . ? Cl2' O11 1.610(12) . ? O1 C2 1.366(4) . ? O1 C1 1.433(4) . ? O2 C7 1.318(3) . ? O3 C12 1.438(5) . ? O3 H3O 0.8400 . ? N1 C8 1.286(4) . ? N1 C9 1.474(4) . ? N2 C10 1.494(4) . ? N2 C11 1.500(5) . ? N2 H2 0.8800 . ? N3 C13 1.491(4) . ? N3 C14 1.500(4) . ? N3 H3 0.8800 . ? N4 C15 1.488(5) . ? N4 H41 0.8800 . ? N4 H42 0.8800 . ? N4 H43 0.8800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.378(5) . ? C2 C7 1.419(4) . ? C3 C4 1.382(5) . ? C3 H3A 0.9500 . ? C4 C5 1.364(5) . ? C4 H4 0.9500 . ? C5 C6 1.416(4) . ? C5 H5 0.9500 . ? C6 C7 1.401(4) . ? C6 C8 1.428(4) . ? C8 H8 0.9500 . ? C9 C10 1.494(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.483(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.506(5) . ? C12 H12A 1.0000 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.502(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O12 C16 1.44(3) . ? O12 H12 0.8400 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 O2 Ni1 N1 94.00(10) . . ? O2 Ni1 N2 178.51(11) . . ? N1 Ni1 N2 86.35(11) . . ? O2 Ni1 N3 84.85(9) . . ? N1 Ni1 N3 178.01(11) . . ? N2 Ni1 N3 94.84(11) . . ? O5 Cl1 O7 110.1(3) . . ? O5 Cl1 O6 107.9(3) . . ? O7 Cl1 O6 108.8(3) . . ? O5 Cl1 O4 109.2(2) . . ? O7 Cl1 O4 111.3(2) . . ? O6 Cl1 O4 109.5(2) . . ? O11 Cl2 O10 111.3(7) . . ? O11 Cl2 O9 113.3(8) . . ? O10 Cl2 O9 110.9(7) . . ? O11 Cl2 O8 107.0(7) . . ? O10 Cl2 O8 107.9(7) . . ? O9 Cl2 O8 106.2(7) . . ? O11' Cl2' O8' 110.6(7) . . ? O11' Cl2' O9' 109.5(7) . . ? O8' Cl2' O9' 110.2(6) . . ? O11' Cl2' O10' 108.0(6) . . ? O8' Cl2' O10' 110.0(7) . . ? O9' Cl2' O10' 108.6(7) . . ? O10 Cl2' O8 111.4(8) . . ? O9 Cl2' O8 107.0(7) . . ? O11' Cl2' O8 114.9(9) . . ? O10 Cl2' O11 105.7(7) . . ? O9 Cl2' O11 105.2(8) . . ? C2 O1 C1 117.5(3) . . ? C7 O2 Ni1 126.64(19) . . ? C12 O3 H3O 109.5 . . ? Cl2 O8 Cl2' 9.5(6) . . ? Cl2' O9 Cl2 10.2(6) . . ? Cl2' O10 Cl2 9.4(6) . . ? Cl2 O11 Cl2' 4.6(6) . . ? C8 N1 C9 119.7(3) . . ? C8 N1 Ni1 127.1(2) . . ? C9 N1 Ni1 113.2(2) . . ? C10 N2 C11 109.1(3) . . ? C10 N2 Ni1 109.5(2) . . ? C11 N2 Ni1 115.9(2) . . ? C10 N2 H2 107.3 . . ? C11 N2 H2 107.3 . . ? Ni1 N2 H2 107.3 . . ? C13 N3 C14 110.8(2) . . ? C13 N3 Ni1 117.9(2) . . ? C14 N3 Ni1 114.34(19) . . ? C13 N3 H3 103.9 . . ? C14 N3 H3 103.9 . . ? Ni1 N3 H3 103.9 . . ? C15 N4 H41 109.5 . . ? C15 N4 H42 109.5 . . ? H41 N4 H42 109.5 . . ? C15 N4 H43 109.5 . . ? H41 N4 H43 109.5 . . ? H42 N4 H43 109.5 . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.2(3) . . ? O1 C2 C7 113.9(3) . . ? C3 C2 C7 120.9(3) . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 120.3(3) . . ? C7 C6 C8 120.7(3) . . ? C5 C6 C8 118.8(3) . . ? O2 C7 C6 124.7(3) . . ? O2 C7 C2 117.9(3) . . ? C6 C7 C2 117.4(3) . . ? N1 C8 C6 124.8(3) . . ? N1 C8 H8 117.6 . . ? C6 C8 H8 117.6 . . ? N1 C9 C10 105.8(3) . . ? N1 C9 H9A 110.6 . . ? C10 C9 H9A 110.6 . . ? N1 C9 H9B 110.6 . . ? C10 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? N2 C10 C9 107.5(3) . . ? N2 C10 H10A 110.2 . . ? C9 C10 H10A 110.2 . . ? N2 C10 H10B 110.2 . . ? C9 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? C12 C11 N2 111.1(3) . . ? C12 C11 H11A 109.4 . . ? N2 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? N2 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? O3 C12 C11 105.8(3) . . ? O3 C12 C13 111.6(3) . . ? C11 C12 C13 114.2(3) . . ? O3 C12 H12A 108.3 . . ? C11 C12 H12A 108.3 . . ? C13 C12 H12A 108.3 . . ? N3 C13 C12 114.9(3) . . ? N3 C13 H13A 108.5 . . ? C12 C13 H13A 108.5 . . ? N3 C13 H13B 108.5 . . ? C12 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? N3 C14 C15 114.8(3) . . ? N3 C14 H14A 108.6 . . ? C15 C14 H14A 108.6 . . ? N3 C14 H14B 108.6 . . ? C15 C14 H14B 108.6 . . ? H14A C14 H14B 107.5 . . ? N4 C15 C14 113.4(3) . . ? N4 C15 H15A 108.9 . . ? C14 C15 H15A 108.9 . . ? N4 C15 H15B 108.9 . . ? C14 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.691 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.064 #END data_090802c _database_code_depnum_ccdc_archive 'CCDC 886467' #TrackingRef '- 3-Xie-CCDC 886465-886468.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38.50 H58 Cl N11 Ni4 O7.50 S3' _chemical_formula_weight 1161.43 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.1068(16) _cell_length_b 17.4396(18) _cell_length_c 20.834(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.0550(10) _cell_angle_gamma 90.00 _cell_volume 5485.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3396 _cell_measurement_theta_min 2.336 _cell_measurement_theta_max 22.026 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2412 _exptl_absorpt_coefficient_mu 1.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5522 _exptl_absorpt_correction_T_max 0.7446 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27130 _diffrn_reflns_av_R_equivalents 0.0890 _diffrn_reflns_av_sigmaI/netI 0.1546 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9611 _reflns_number_gt 4041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0756P)^2^+19.5459P] 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 9611 _refine_ls_number_parameters 624 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1957 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.2640 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 0.22389(9) 0.34177(7) 0.17116(6) 0.0419(4) Uani 1 1 d . . . Ni2 Ni 0.19139(9) 0.34278(7) 0.39584(6) 0.0425(4) Uani 1 1 d . . . Ni3 Ni 0.40273(9) 0.41570(8) 0.16956(7) 0.0460(4) Uani 1 1 d . . . Ni4 Ni 0.00444(9) 0.39606(8) 0.39658(7) 0.0446(4) Uani 1 1 d . . . Cl1 Cl 0.7771(3) 0.3826(4) 0.2420(3) 0.151(2) Uani 1 1 d . . . N1 N 0.4933(5) 0.4305(5) 0.1143(5) 0.046(2) Uani 1 1 d . . . N2 N 0.4668(5) 0.4736(5) 0.2313(4) 0.049(2) Uani 1 1 d . . . H2 H 0.5017 0.4415 0.2556 0.059 Uiso 1 1 calc R . . N3 N 0.3092(5) 0.3237(5) 0.3477(4) 0.046(2) Uani 1 1 d . . . H3 H 0.2937 0.3021 0.3092 0.056 Uiso 1 1 calc R . . N4 N 0.2572(6) 0.2941(5) 0.4711(5) 0.050(2) Uani 1 1 d . . . N5 N -0.0825(6) 0.4101(5) 0.4537(4) 0.048(2) Uani 1 1 d . . . N6 N -0.0646(5) 0.4511(4) 0.3363(4) 0.045(2) Uani 1 1 d . . . H6 H -0.0994 0.4178 0.3131 0.053 Uiso 1 1 calc R . . N7 N 0.1075(5) 0.3111(5) 0.2192(4) 0.047(2) Uani 1 1 d . . . H7A H 0.1246 0.2922 0.2584 0.056 Uiso 1 1 calc R . . N8 N 0.1645(6) 0.2907(5) 0.0949(5) 0.051(2) Uani 1 1 d . . . N9 N 0.2793(6) 0.2436(6) 0.2070(4) 0.053(3) Uani 1 1 d . . . N10 N 0.1507(6) 0.2295(6) 0.3626(5) 0.055(3) Uani 1 1 d . . . N11 N 0.2299(6) 0.4505(6) 0.4256(5) 0.055(2) Uani 1 1 d . A . O1 O 0.3300(4) 0.3610(4) 0.1138(3) 0.0448(18) Uani 1 1 d . . . O2 O 0.3110(4) 0.4090(4) 0.2253(3) 0.0472(18) Uani 1 1 d . . . O3 O 0.0811(4) 0.3450(4) 0.4525(3) 0.0475(18) Uani 1 1 d . . . O4 O 0.0923(4) 0.3887(4) 0.3375(3) 0.0444(18) Uani 1 1 d . . . O5 O 0.1739(5) 0.4505(4) 0.1411(4) 0.058(2) Uani 1 1 d . . . H5 H 0.2088 0.4837 0.1536 0.087 Uiso 1 1 d R . . O6 O 0.6077(8) 0.4044(8) 0.3145(6) 0.124(4) Uani 1 1 d . . . H6A H 0.6520 0.4011 0.2930 0.185 Uiso 1 1 calc R . . O7 O 0.865(2) 0.379(2) 0.1025(16) 0.188(15) Uani 0.50 1 d P . . H7 H 0.8490 0.3741 0.1396 0.282 Uiso 0.50 1 calc PR . . O8 O 0.645(3) 0.610(3) 0.348(2) 0.224(18) Uani 0.50 1 d P . . H8 H 0.6703 0.5800 0.3246 0.335 Uiso 0.50 1 calc PR . . O9 O 0.737(2) 0.559(2) 0.2327(16) 0.167(12) Uani 0.50 1 d P . . H9 H 0.7509 0.5143 0.2367 0.250 Uiso 0.50 1 calc PR . . S1 S 0.3334(3) 0.10455(19) 0.2587(2) 0.0881(13) Uani 1 1 d . . . S2 S 0.1672(2) 0.08091(18) 0.41116(19) 0.0754(11) Uani 1 1 d . . . S3 S 0.3163(15) 0.5908(11) 0.4347(11) 0.104(5) Uani 0.68(4) 1 d P A 1 S3' S 0.346(3) 0.5691(18) 0.454(2) 0.104(5) Uani 0.32(4) 1 d P A 2 C1 C 0.3455(7) 0.3415(6) 0.0541(5) 0.046(3) Uani 1 1 d . . . C2 C 0.4263(7) 0.3610(6) 0.0236(6) 0.048(3) Uani 1 1 d . . . C3 C 0.4417(8) 0.3375(6) -0.0381(5) 0.050(3) Uani 1 1 d . . . H3A H 0.4954 0.3497 -0.0562 0.060 Uiso 1 1 calc R . . C4 C 0.3787(8) 0.2961(6) -0.0740(6) 0.052(3) Uani 1 1 d . . . C5 C 0.3012(8) 0.2779(6) -0.0452(5) 0.052(3) Uani 1 1 d . . . H5A H 0.2593 0.2494 -0.0686 0.062 Uiso 1 1 calc R . . C6 C 0.2817(7) 0.2997(6) 0.0170(5) 0.049(3) Uani 1 1 d . . . C7 C 0.4948(7) 0.4066(6) 0.0567(6) 0.051(3) Uani 1 1 d . . . H7B H 0.5441 0.4193 0.0335 0.061 Uiso 1 1 calc R . . C8 C 0.3954(8) 0.2738(7) -0.1427(6) 0.070(4) Uani 1 1 d . . . H8A H 0.3748 0.3139 -0.1711 0.104 Uiso 1 1 calc R . . H8B H 0.3642 0.2272 -0.1531 0.104 Uiso 1 1 calc R . . H8C H 0.4577 0.2662 -0.1476 0.104 Uiso 1 1 calc R . . C9 C 0.1948(7) 0.2753(6) 0.0397(6) 0.052(3) Uani 1 1 d . . . H9A H 0.1590 0.2463 0.0116 0.062 Uiso 1 1 calc R . . C10 C 0.0680(7) 0.3256(6) 0.5134(5) 0.045(3) Uani 1 1 d . . . C11 C 0.1369(7) 0.2880(6) 0.5479(5) 0.049(3) Uani 1 1 d . . . C12 C 0.1214(7) 0.2640(6) 0.6110(5) 0.052(3) Uani 1 1 d . . . H12 H 0.1659 0.2383 0.6342 0.062 Uiso 1 1 calc R . . C13 C 0.0400(8) 0.2782(6) 0.6397(5) 0.051(3) Uani 1 1 d . . . C14 C -0.0234(8) 0.3164(6) 0.6050(6) 0.054(3) Uani 1 1 d . . . H14 H -0.0770 0.3265 0.6240 0.065 Uiso 1 1 calc R . . C15 C -0.0123(7) 0.3417(6) 0.5415(5) 0.047(3) Uani 1 1 d . . . C16 C 0.2266(7) 0.2737(6) 0.5246(6) 0.054(3) Uani 1 1 d . . . H16 H 0.2651 0.2467 0.5522 0.064 Uiso 1 1 calc R . . C17 C 0.0289(8) 0.2525(7) 0.7089(5) 0.070(4) Uani 1 1 d . . . H17A H 0.0490 0.2924 0.7376 0.105 Uiso 1 1 calc R . . H17B H 0.0631 0.2069 0.7171 0.105 Uiso 1 1 calc R . . H17C H -0.0325 0.2420 0.7156 0.105 Uiso 1 1 calc R . . C18 C -0.0839(7) 0.3853(6) 0.5110(6) 0.050(3) Uani 1 1 d . . . H18 H -0.1335 0.3958 0.5347 0.060 Uiso 1 1 calc R . . C19 C 0.5668(8) 0.4761(7) 0.1444(6) 0.066(4) Uani 1 1 d . . . H19A H 0.5945 0.5079 0.1126 0.079 Uiso 1 1 calc R . . H19B H 0.6113 0.4426 0.1640 0.079 Uiso 1 1 calc R . . C20 C 0.5236(8) 0.5268(7) 0.1964(6) 0.060(3) Uani 1 1 d . . . H20A H 0.5685 0.5492 0.2251 0.072 Uiso 1 1 calc R . . H20B H 0.4887 0.5677 0.1766 0.072 Uiso 1 1 calc R . . C21 C 0.3997(7) 0.5083(6) 0.2723(6) 0.053(3) Uani 1 1 d . . . H21A H 0.3705 0.5508 0.2503 0.064 Uiso 1 1 calc R . . H21B H 0.4272 0.5269 0.3121 0.064 Uiso 1 1 calc R . . C22 C 0.3329(7) 0.4441(6) 0.2857(5) 0.051(3) Uani 1 1 d . . . H22 H 0.2794 0.4671 0.3027 0.061 Uiso 1 1 calc R . . C23 C 0.3713(7) 0.3878(6) 0.3344(5) 0.051(3) Uani 1 1 d . . . H23A H 0.4258 0.3668 0.3185 0.061 Uiso 1 1 calc R . . H23B H 0.3857 0.4147 0.3741 0.061 Uiso 1 1 calc R . . C24 C 0.3563(7) 0.2630(6) 0.3869(5) 0.051(3) Uani 1 1 d . . . H24A H 0.3299 0.2134 0.3775 0.061 Uiso 1 1 calc R . . H24B H 0.4181 0.2611 0.3758 0.061 Uiso 1 1 calc R . . C25 C 0.3500(7) 0.2801(7) 0.4565(6) 0.055(3) Uani 1 1 d . . . H25A H 0.3727 0.2372 0.4817 0.066 Uiso 1 1 calc R . . H25B H 0.3853 0.3250 0.4676 0.066 Uiso 1 1 calc R . . C26 C -0.1585(7) 0.4556(7) 0.4260(6) 0.059(3) Uani 1 1 d . . . H26A H -0.1827 0.4886 0.4585 0.070 Uiso 1 1 calc R . . H26B H -0.2050 0.4219 0.4095 0.070 Uiso 1 1 calc R . . C27 C -0.1213(7) 0.5033(6) 0.3720(5) 0.055(3) Uani 1 1 d . . . H27A H -0.1689 0.5231 0.3442 0.066 Uiso 1 1 calc R . . H27B H -0.0871 0.5461 0.3893 0.066 Uiso 1 1 calc R . . C28 C -0.0005(7) 0.4873(6) 0.2930(5) 0.049(3) Uani 1 1 d . . . H28A H 0.0266 0.5319 0.3134 0.058 Uiso 1 1 calc R . . H28B H -0.0303 0.5033 0.2532 0.058 Uiso 1 1 calc R . . C29 C 0.0708(7) 0.4255(6) 0.2797(5) 0.046(3) Uani 1 1 d . . . H29 H 0.1238 0.4511 0.2645 0.055 Uiso 1 1 calc R . . C30 C 0.0376(7) 0.3702(6) 0.2292(5) 0.049(3) Uani 1 1 d . . . H30A H -0.0162 0.3457 0.2428 0.059 Uiso 1 1 calc R . . H30B H 0.0243 0.3973 0.1894 0.059 Uiso 1 1 calc R . . C31 C 0.0722(7) 0.2463(6) 0.1799(5) 0.056(3) Uani 1 1 d . . . H31A H 0.0117 0.2359 0.1912 0.067 Uiso 1 1 calc R . . H31B H 0.1072 0.2007 0.1891 0.067 Uiso 1 1 calc R . . C32 C 0.0748(8) 0.2650(7) 0.1080(6) 0.058(3) Uani 1 1 d . . . H32A H 0.0600 0.2198 0.0826 0.070 Uiso 1 1 calc R . . H32B H 0.0324 0.3050 0.0969 0.070 Uiso 1 1 calc R . . C33 C 0.3011(7) 0.1858(7) 0.2283(6) 0.053(3) Uani 1 1 d . . . C34 C 0.1582(7) 0.1671(7) 0.3820(6) 0.050(3) Uani 1 1 d . . . C35 C 0.2712(8) 0.5057(7) 0.4310(6) 0.062(3) Uani 1 1 d . . . C36 C 0.1334(12) 0.4732(11) 0.0817(9) 0.134(7) Uani 1 1 d . . . H36A H 0.1318 0.5281 0.0793 0.201 Uiso 1 1 calc R . . H36B H 0.0742 0.4533 0.0784 0.201 Uiso 1 1 calc R . . H36C H 0.1670 0.4534 0.0470 0.201 Uiso 1 1 calc R . . C37 C 0.6135(16) 0.3508(15) 0.3657(14) 0.191(11) Uani 1 1 d . . . H37A H 0.6735 0.3483 0.3824 0.286 Uiso 1 1 calc R . . H37B H 0.5955 0.3011 0.3502 0.286 Uiso 1 1 calc R . . H37C H 0.5754 0.3666 0.3991 0.286 Uiso 1 1 calc R . . C38 C 0.809(3) 0.433(3) 0.070(2) 0.169(19) Uani 0.50 1 d P . . H38A H 0.7484 0.4163 0.0707 0.254 Uiso 0.50 1 calc PR . . H38B H 0.8260 0.4374 0.0259 0.254 Uiso 0.50 1 calc PR . . H38C H 0.8146 0.4821 0.0904 0.254 Uiso 0.50 1 calc PR . . C39 C 0.610(4) 0.570(3) 0.401(3) 0.18(2) Uani 0.50 1 d P . . H39A H 0.6024 0.6051 0.4359 0.270 Uiso 0.50 1 calc PR . . H39B H 0.6508 0.5303 0.4146 0.270 Uiso 0.50 1 calc PR . . H39C H 0.5543 0.5477 0.3885 0.270 Uiso 0.50 1 calc PR . . C40 C 0.800(3) 0.599(3) 0.196(3) 0.18(2) Uani 0.50 1 d P . . H40A H 0.8101 0.6489 0.2140 0.273 Uiso 0.50 1 calc PR . . H40B H 0.7791 0.6029 0.1526 0.273 Uiso 0.50 1 calc PR . . H40C H 0.8550 0.5704 0.1981 0.273 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0425(8) 0.0372(8) 0.0468(9) -0.0041(6) 0.0116(6) -0.0028(6) Ni2 0.0425(8) 0.0412(8) 0.0444(9) 0.0004(7) 0.0117(6) 0.0037(6) Ni3 0.0434(9) 0.0468(9) 0.0486(9) -0.0009(7) 0.0117(7) -0.0076(7) Ni4 0.0419(9) 0.0472(8) 0.0457(9) -0.0006(7) 0.0133(7) 0.0070(6) Cl1 0.088(3) 0.214(6) 0.150(5) 0.011(4) -0.018(3) -0.011(3) N1 0.044(6) 0.044(5) 0.050(6) 0.007(5) 0.005(5) -0.006(4) N2 0.042(6) 0.051(6) 0.054(6) 0.005(5) 0.006(5) -0.003(4) N3 0.045(5) 0.042(5) 0.053(6) -0.004(4) 0.014(4) -0.002(4) N4 0.044(6) 0.049(6) 0.060(7) 0.003(5) 0.014(5) 0.004(4) N5 0.046(6) 0.052(6) 0.046(6) 0.003(5) 0.005(5) 0.007(4) N6 0.042(5) 0.036(5) 0.056(6) -0.003(4) 0.013(4) 0.008(4) N7 0.047(6) 0.039(5) 0.055(6) -0.003(4) 0.016(5) 0.001(4) N8 0.047(6) 0.046(6) 0.061(7) -0.006(5) 0.017(5) -0.005(4) N9 0.052(6) 0.046(6) 0.063(7) -0.002(5) 0.020(5) 0.003(5) N10 0.054(6) 0.051(6) 0.062(7) -0.001(5) 0.014(5) 0.004(5) N11 0.054(6) 0.050(6) 0.061(7) -0.004(5) 0.010(5) 0.004(5) O1 0.044(4) 0.047(4) 0.044(5) -0.006(4) 0.014(3) -0.006(3) O2 0.047(5) 0.047(4) 0.048(5) -0.006(4) 0.012(4) -0.007(3) O3 0.046(4) 0.053(5) 0.045(5) 0.005(4) 0.015(3) 0.006(4) O4 0.045(4) 0.051(4) 0.038(4) 0.005(4) 0.009(3) 0.011(3) O5 0.059(5) 0.054(5) 0.061(5) 0.001(4) 0.003(4) -0.005(4) O6 0.111(9) 0.149(12) 0.111(10) 0.006(8) -0.001(8) 0.001(8) O7 0.12(2) 0.31(5) 0.14(3) -0.07(3) -0.02(2) -0.01(3) O8 0.19(4) 0.28(5) 0.20(4) -0.01(4) -0.03(3) 0.03(3) O9 0.14(3) 0.19(3) 0.17(3) 0.02(2) -0.02(2) 0.00(2) S1 0.107(3) 0.0428(19) 0.116(3) 0.015(2) 0.038(3) 0.0162(19) S2 0.083(3) 0.0489(19) 0.096(3) 0.0099(19) 0.029(2) 0.0055(17) S3 0.112(11) 0.059(8) 0.145(11) -0.026(7) 0.055(9) -0.025(6) S3' 0.112(11) 0.059(8) 0.145(11) -0.026(7) 0.055(9) -0.025(6) C1 0.048(7) 0.041(6) 0.048(7) -0.001(6) 0.012(6) 0.006(5) C2 0.047(7) 0.043(6) 0.054(8) 0.003(6) 0.016(6) 0.003(5) C3 0.053(7) 0.050(7) 0.050(7) 0.013(6) 0.017(6) 0.003(6) C4 0.057(8) 0.048(7) 0.053(8) 0.007(6) 0.016(6) 0.004(6) C5 0.056(8) 0.050(7) 0.050(8) -0.005(6) 0.010(6) 0.006(6) C6 0.055(8) 0.047(7) 0.047(7) -0.003(6) 0.013(6) 0.002(6) C7 0.051(7) 0.052(7) 0.051(8) 0.005(6) 0.015(6) 0.001(6) C8 0.081(10) 0.066(8) 0.064(9) -0.012(7) 0.027(7) 0.000(7) C9 0.051(8) 0.046(7) 0.059(8) -0.006(6) 0.009(6) 0.001(6) C10 0.044(7) 0.045(7) 0.046(7) -0.001(5) 0.013(6) -0.005(5) C11 0.050(8) 0.052(7) 0.048(7) -0.001(6) 0.016(6) 0.002(6) C12 0.050(7) 0.056(7) 0.049(7) 0.003(6) 0.005(6) 0.000(6) C13 0.055(8) 0.051(7) 0.048(7) 0.003(6) 0.013(6) -0.005(6) C14 0.053(8) 0.055(7) 0.056(8) -0.005(6) 0.010(6) -0.006(6) C15 0.048(7) 0.050(7) 0.045(7) -0.001(6) 0.014(6) -0.005(6) C16 0.052(8) 0.052(7) 0.057(8) 0.007(6) 0.008(6) 0.003(6) C17 0.082(10) 0.074(9) 0.055(8) 0.015(7) 0.010(7) -0.014(7) C18 0.043(7) 0.056(7) 0.052(8) -0.004(6) 0.014(6) 0.007(6) C19 0.055(8) 0.067(8) 0.075(9) 0.017(7) 0.017(7) -0.009(7) C20 0.056(8) 0.065(8) 0.060(8) 0.009(7) 0.007(6) -0.014(6) C21 0.050(7) 0.052(7) 0.058(8) -0.001(6) 0.010(6) -0.009(6) C22 0.048(7) 0.049(7) 0.056(8) -0.006(6) 0.016(6) 0.000(5) C23 0.048(7) 0.047(7) 0.057(8) 0.004(6) 0.010(6) -0.004(5) C24 0.042(7) 0.046(7) 0.066(8) 0.008(6) 0.017(6) 0.011(5) C25 0.044(7) 0.058(8) 0.064(9) 0.008(6) 0.011(6) 0.007(6) C26 0.051(8) 0.064(8) 0.062(8) -0.004(7) 0.019(6) 0.010(6) C27 0.053(7) 0.057(7) 0.057(8) -0.002(6) 0.021(6) 0.015(6) C28 0.050(7) 0.046(7) 0.051(7) 0.004(5) 0.015(6) 0.008(5) C29 0.047(7) 0.044(6) 0.048(7) -0.004(6) 0.012(5) 0.004(5) C30 0.048(7) 0.048(7) 0.051(7) 0.003(6) 0.009(6) 0.000(5) C31 0.051(7) 0.053(7) 0.065(9) -0.008(6) 0.017(6) -0.012(6) C32 0.055(8) 0.056(7) 0.064(9) -0.010(6) 0.010(6) -0.006(6) C33 0.056(8) 0.042(7) 0.063(8) 0.001(6) 0.023(6) 0.003(6) C34 0.045(7) 0.051(7) 0.056(8) -0.006(6) 0.012(6) -0.001(6) C35 0.065(9) 0.051(8) 0.072(9) -0.006(7) 0.027(7) 0.000(7) C36 0.134(17) 0.122(16) 0.146(19) 0.006(14) 0.002(14) -0.013(13) C37 0.15(2) 0.20(3) 0.22(3) -0.01(2) -0.06(2) 0.015(18) C38 0.14(4) 0.22(6) 0.15(4) 0.00(4) 0.01(3) -0.03(4) C39 0.18(5) 0.20(6) 0.16(5) 0.00(4) -0.02(4) 0.01(4) C40 0.15(4) 0.21(6) 0.18(5) 0.04(4) -0.02(4) 0.01(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 N8 2.005(9) . ? Ni1 N9 2.036(10) . ? Ni1 O1 2.061(7) . ? Ni1 O2 2.068(7) . ? Ni1 N7 2.122(8) . ? Ni1 O5 2.127(8) . ? Ni1 Ni3 2.9948(18) . ? Ni2 N4 2.014(9) . ? Ni2 N11 2.056(10) . ? Ni2 O4 2.056(7) . ? Ni2 O3 2.076(7) . ? Ni2 N3 2.101(8) . ? Ni2 N10 2.175(10) . ? Ni2 Ni4 2.9737(18) . ? Ni3 O1 1.836(7) . ? Ni3 N1 1.839(9) . ? Ni3 O2 1.844(7) . ? Ni3 N2 1.876(9) . ? Ni4 N5 1.820(9) . ? Ni4 O3 1.843(7) . ? Ni4 O4 1.846(7) . ? Ni4 N6 1.869(8) . ? N1 C7 1.271(13) . ? N1 C19 1.486(14) . ? N2 C20 1.475(13) . ? N2 C21 1.478(13) . ? N2 H2 0.9100 . ? N3 C23 1.492(12) . ? N3 C24 1.501(12) . ? N3 H3 0.9100 . ? N4 C16 1.272(13) . ? N4 C25 1.466(13) . ? N5 C18 1.271(13) . ? N5 C26 1.495(13) . ? N6 C27 1.471(12) . ? N6 C28 1.486(12) . ? N6 H6 0.9100 . ? N7 C31 1.483(12) . ? N7 C30 1.496(12) . ? N7 H7A 0.9100 . ? N8 C9 1.282(13) . ? N8 C32 1.461(13) . ? N9 C33 1.145(13) . ? N10 C34 1.164(13) . ? N11 C35 1.150(13) . ? O1 C1 1.320(12) . ? O2 C22 1.427(12) . ? O3 C10 1.333(12) . ? O4 C29 1.393(12) . ? O5 C36 1.417(18) . ? O5 H5 0.8200 . ? O6 C37 1.42(2) . ? O6 H6A 0.8200 . ? O7 C38 1.43(5) . ? O7 H7 0.8200 . ? O8 C39 1.43(5) . ? O8 H8 0.8200 . ? O9 C40 1.42(5) . ? O9 H9 0.8200 . ? S1 C33 1.620(13) . ? S2 C34 1.625(13) . ? S3 C35 1.634(19) . ? S3' C35 1.64(4) . ? C1 C6 1.415(14) . ? C1 C2 1.437(14) . ? C2 C3 1.376(15) . ? C2 C7 1.458(15) . ? C3 C4 1.392(15) . ? C3 H3A 0.9300 . ? C4 C5 1.371(15) . ? C4 C8 1.514(15) . ? C5 C6 1.393(14) . ? C5 H5A 0.9300 . ? C6 C9 1.474(15) . ? C7 H7B 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9300 . ? C10 C15 1.395(14) . ? C10 C11 1.407(14) . ? C11 C12 1.407(14) . ? C11 C16 1.476(15) . ? C12 C13 1.409(15) . ? C12 H12 0.9300 . ? C13 C14 1.355(15) . ? C13 C17 1.524(15) . ? C14 C15 1.411(15) . ? C14 H14 0.9300 . ? C15 C18 1.450(15) . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18 0.9300 . ? C19 C20 1.558(16) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.539(14) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.512(14) . ? C22 H22 0.9800 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.487(15) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.522(15) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.555(13) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.500(14) . ? C29 H29 0.9800 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.536(15) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 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 N8 Ni1 N9 94.8(4) . . ? N8 Ni1 O1 87.1(3) . . ? N9 Ni1 O1 91.8(3) . . ? N8 Ni1 O2 160.5(3) . . ? N9 Ni1 O2 91.8(3) . . ? O1 Ni1 O2 74.4(3) . . ? N8 Ni1 N7 84.6(4) . . ? N9 Ni1 N7 87.2(3) . . ? O1 Ni1 N7 171.6(3) . . ? O2 Ni1 N7 114.0(3) . . ? N8 Ni1 O5 91.1(3) . . ? N9 Ni1 O5 174.1(3) . . ? O1 Ni1 O5 87.7(3) . . ? O2 Ni1 O5 82.4(3) . . ? N7 Ni1 O5 94.1(3) . . ? N8 Ni1 Ni3 124.1(3) . . ? N9 Ni1 Ni3 90.4(3) . . ? O1 Ni1 Ni3 37.11(19) . . ? O2 Ni1 Ni3 37.36(19) . . ? N7 Ni1 Ni3 151.2(2) . . ? O5 Ni1 Ni3 85.6(2) . . ? N4 Ni2 N11 91.4(4) . . ? N4 Ni2 O4 162.3(3) . . ? N11 Ni2 O4 90.8(3) . . ? N4 Ni2 O3 87.0(3) . . ? N11 Ni2 O3 92.0(3) . . ? O4 Ni2 O3 75.3(3) . . ? N4 Ni2 N3 84.4(4) . . ? N11 Ni2 N3 93.1(3) . . ? O4 Ni2 N3 113.0(3) . . ? O3 Ni2 N3 170.1(3) . . ? N4 Ni2 N10 89.4(4) . . ? N11 Ni2 N10 179.0(4) . . ? O4 Ni2 N10 88.5(3) . . ? O3 Ni2 N10 88.5(3) . . ? N3 Ni2 N10 86.5(3) . . ? N4 Ni2 Ni4 124.7(3) . . ? N11 Ni2 Ni4 88.3(3) . . ? O4 Ni2 Ni4 37.79(19) . . ? O3 Ni2 Ni4 37.81(19) . . ? N3 Ni2 Ni4 150.8(3) . . ? N10 Ni2 Ni4 91.6(2) . . ? O1 Ni3 N1 96.8(4) . . ? O1 Ni3 O2 85.4(3) . . ? N1 Ni3 O2 175.5(3) . . ? O1 Ni3 N2 174.2(3) . . ? N1 Ni3 N2 88.7(4) . . ? O2 Ni3 N2 89.0(3) . . ? O1 Ni3 Ni1 42.6(2) . . ? N1 Ni3 Ni1 139.4(3) . . ? O2 Ni3 Ni1 42.9(2) . . ? N2 Ni3 Ni1 131.9(3) . . ? N5 Ni4 O3 95.9(4) . . ? N5 Ni4 O4 176.3(4) . . ? O3 Ni4 O4 86.4(3) . . ? N5 Ni4 N6 88.4(4) . . ? O3 Ni4 N6 175.0(3) . . ? O4 Ni4 N6 89.1(3) . . ? N5 Ni4 Ni2 138.8(3) . . ? O3 Ni4 Ni2 43.7(2) . . ? O4 Ni4 Ni2 43.0(2) . . ? N6 Ni4 Ni2 131.6(3) . . ? C7 N1 C19 122.5(9) . . ? C7 N1 Ni3 125.7(8) . . ? C19 N1 Ni3 111.8(7) . . ? C20 N2 C21 116.8(9) . . ? C20 N2 Ni3 107.2(7) . . ? C21 N2 Ni3 105.6(6) . . ? C20 N2 H2 109.0 . . ? C21 N2 H2 109.0 . . ? Ni3 N2 H2 109.0 . . ? C23 N3 C24 109.9(8) . . ? C23 N3 Ni2 121.3(6) . . ? C24 N3 Ni2 104.1(6) . . ? C23 N3 H3 106.9 . . ? C24 N3 H3 106.9 . . ? Ni2 N3 H3 106.9 . . ? C16 N4 C25 121.0(10) . . ? C16 N4 Ni2 128.0(8) . . ? C25 N4 Ni2 110.9(7) . . ? C18 N5 C26 120.3(9) . . ? C18 N5 Ni4 127.3(8) . . ? C26 N5 Ni4 112.4(7) . . ? C27 N6 C28 116.6(8) . . ? C27 N6 Ni4 107.4(7) . . ? C28 N6 Ni4 105.4(6) . . ? C27 N6 H6 109.1 . . ? C28 N6 H6 109.1 . . ? Ni4 N6 H6 109.1 . . ? C31 N7 C30 111.1(8) . . ? C31 N7 Ni1 102.7(6) . . ? C30 N7 Ni1 119.6(6) . . ? C31 N7 H7A 107.6 . . ? C30 N7 H7A 107.6 . . ? Ni1 N7 H7A 107.6 . . ? C9 N8 C32 117.8(10) . . ? C9 N8 Ni1 129.8(8) . . ? C32 N8 Ni1 112.4(7) . . ? C33 N9 Ni1 172.4(9) . . ? C34 N10 Ni2 135.7(9) . . ? C35 N11 Ni2 160.1(9) . . ? C1 O1 Ni3 127.5(7) . . ? C1 O1 Ni1 132.3(7) . . ? Ni3 O1 Ni1 100.3(3) . . ? C22 O2 Ni3 111.9(6) . . ? C22 O2 Ni1 148.0(6) . . ? Ni3 O2 Ni1 99.8(3) . . ? C10 O3 Ni4 127.7(7) . . ? C10 O3 Ni2 133.3(7) . . ? Ni4 O3 Ni2 98.5(3) . . ? C29 O4 Ni4 113.1(6) . . ? C29 O4 Ni2 146.3(6) . . ? Ni4 O4 Ni2 99.2(3) . . ? C36 O5 Ni1 130.1(9) . . ? C36 O5 H5 109.5 . . ? Ni1 O5 H5 108.5 . . ? C37 O6 H6A 109.5 . . ? C38 O7 H7 109.5 . . ? C39 O8 H8 109.5 . . ? C40 O9 H9 109.5 . . ? O1 C1 C6 120.5(10) . . ? O1 C1 C2 122.6(10) . . ? C6 C1 C2 116.9(10) . . ? C3 C2 C1 121.2(11) . . ? C3 C2 C7 117.6(10) . . ? C1 C2 C7 121.3(10) . . ? C2 C3 C4 121.3(11) . . ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 . . ? C5 C4 C3 117.6(11) . . ? C5 C4 C8 121.9(11) . . ? C3 C4 C8 120.5(11) . . ? C4 C5 C6 123.8(11) . . ? C4 C5 H5A 118.1 . . ? C6 C5 H5A 118.1 . . ? C5 C6 C1 119.0(10) . . ? C5 C6 C9 116.1(10) . . ? C1 C6 C9 124.8(10) . . ? N1 C7 C2 126.1(10) . . ? N1 C7 H7B 116.9 . . ? C2 C7 H7B 116.9 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N8 C9 C6 125.3(11) . . ? N8 C9 H9A 117.3 . . ? C6 C9 H9A 117.3 . . ? O3 C10 C15 120.6(10) . . ? O3 C10 C11 118.2(9) . . ? C15 C10 C11 121.2(10) . . ? C12 C11 C10 118.1(10) . . ? C12 C11 C16 116.3(10) . . ? C10 C11 C16 125.5(10) . . ? C11 C12 C13 121.5(11) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C14 C13 C12 118.1(11) . . ? C14 C13 C17 123.3(11) . . ? C12 C13 C17 118.6(11) . . ? C13 C14 C15 123.3(11) . . ? C13 C14 H14 118.3 . . ? C15 C14 H14 118.3 . . ? C10 C15 C14 117.8(11) . . ? C10 C15 C18 124.6(10) . . ? C14 C15 C18 117.6(10) . . ? N4 C16 C11 127.4(11) . . ? N4 C16 H16 116.3 . . ? C11 C16 H16 116.3 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 C15 123.5(10) . . ? N5 C18 H18 118.2 . . ? C15 C18 H18 118.2 . . ? N1 C19 C20 105.9(9) . . ? N1 C19 H19A 110.6 . . ? C20 C19 H19A 110.6 . . ? N1 C19 H19B 110.6 . . ? C20 C19 H19B 110.6 . . ? H19A C19 H19B 108.7 . . ? N2 C20 C19 104.5(9) . . ? N2 C20 H20A 110.8 . . ? C19 C20 H20A 110.8 . . ? N2 C20 H20B 110.8 . . ? C19 C20 H20B 110.8 . . ? H20A C20 H20B 108.9 . . ? N2 C21 C22 105.9(8) . . ? N2 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? N2 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? O2 C22 C23 112.6(9) . . ? O2 C22 C21 106.6(9) . . ? C23 C22 C21 110.8(9) . . ? O2 C22 H22 108.9 . . ? C23 C22 H22 108.9 . . ? C21 C22 H22 108.9 . . ? N3 C23 C22 112.5(9) . . ? N3 C23 H23A 109.1 . . ? C22 C23 H23A 109.1 . . ? N3 C23 H23B 109.1 . . ? C22 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? C25 C24 N3 110.1(9) . . ? C25 C24 H24A 109.6 . . ? N3 C24 H24A 109.6 . . ? C25 C24 H24B 109.6 . . ? N3 C24 H24B 109.6 . . ? H24A C24 H24B 108.2 . . ? N4 C25 C24 109.3(9) . . ? N4 C25 H25A 109.8 . . ? C24 C25 H25A 109.8 . . ? N4 C25 H25B 109.8 . . ? C24 C25 H25B 109.8 . . ? H25A C25 H25B 108.3 . . ? N5 C26 C27 106.1(9) . . ? N5 C26 H26A 110.5 . . ? C27 C26 H26A 110.5 . . ? N5 C26 H26B 110.5 . . ? C27 C26 H26B 110.5 . . ? H26A C26 H26B 108.7 . . ? N6 C27 C26 105.9(9) . . ? N6 C27 H27A 110.6 . . ? C26 C27 H27A 110.6 . . ? N6 C27 H27B 110.6 . . ? C26 C27 H27B 110.6 . . ? H27A C27 H27B 108.7 . . ? N6 C28 C29 106.5(8) . . ? N6 C28 H28A 110.4 . . ? C29 C28 H28A 110.4 . . ? N6 C28 H28B 110.4 . . ? C29 C28 H28B 110.4 . . ? H28A C28 H28B 108.6 . . ? O4 C29 C30 111.8(9) . . ? O4 C29 C28 107.9(8) . . ? C30 C29 C28 110.7(9) . . ? O4 C29 H29 108.8 . . ? C30 C29 H29 108.8 . . ? C28 C29 H29 108.8 . . ? N7 C30 C29 108.7(9) . . ? N7 C30 H30A 109.9 . . ? C29 C30 H30A 109.9 . . ? N7 C30 H30B 109.9 . . ? C29 C30 H30B 109.9 . . ? H30A C30 H30B 108.3 . . ? N7 C31 C32 110.8(9) . . ? N7 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N7 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? N8 C32 C31 107.6(9) . . ? N8 C32 H32A 110.2 . . ? C31 C32 H32A 110.2 . . ? N8 C32 H32B 110.2 . . ? C31 C32 H32B 110.2 . . ? H32A C32 H32B 108.5 . . ? N9 C33 S1 179.1(12) . . ? N10 C34 S2 178.2(11) . . ? N11 C35 S3 171.3(16) . . ? N11 C35 S3' 163(2) . . ? S3 C35 S3' 24.9(11) . . ? O5 C36 H36A 109.5 . . ? O5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O6 C37 H37A 109.5 . . ? O6 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O6 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O7 C38 H38A 109.5 . . ? O7 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O7 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O8 C39 H39A 109.5 . . ? O8 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O8 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O9 C40 H40A 109.5 . . ? O9 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O9 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Ni1 Ni3 O1 -3.6(4) . . . . ? N9 Ni1 Ni3 O1 92.5(4) . . . . ? O2 Ni1 Ni3 O1 -175.1(4) . . . . ? N7 Ni1 Ni3 O1 177.5(6) . . . . ? O5 Ni1 Ni3 O1 -91.9(4) . . . . ? N8 Ni1 Ni3 N1 -2.8(5) . . . . ? N9 Ni1 Ni3 N1 93.3(5) . . . . ? O1 Ni1 Ni3 N1 0.8(5) . . . . ? O2 Ni1 Ni3 N1 -174.3(5) . . . . ? N7 Ni1 Ni3 N1 178.3(6) . . . . ? O5 Ni1 Ni3 N1 -91.1(5) . . . . ? N8 Ni1 Ni3 O2 171.5(4) . . . . ? N9 Ni1 Ni3 O2 -92.5(4) . . . . ? O1 Ni1 Ni3 O2 175.1(4) . . . . ? N7 Ni1 Ni3 O2 -7.5(6) . . . . ? O5 Ni1 Ni3 O2 83.2(4) . . . . ? N8 Ni1 Ni3 N2 173.9(5) . . . . ? N9 Ni1 Ni3 N2 -90.1(4) . . . . ? O1 Ni1 Ni3 N2 177.4(5) . . . . ? O2 Ni1 Ni3 N2 2.4(5) . . . . ? N7 Ni1 Ni3 N2 -5.1(6) . . . . ? O5 Ni1 Ni3 N2 85.6(4) . . . . ? N4 Ni2 Ni4 N5 8.9(5) . . . . ? N11 Ni2 Ni4 N5 -81.7(5) . . . . ? O4 Ni2 Ni4 N5 -175.2(5) . . . . ? O3 Ni2 Ni4 N5 13.8(5) . . . . ? N3 Ni2 Ni4 N5 -175.0(6) . . . . ? N10 Ni2 Ni4 N5 99.3(5) . . . . ? N4 Ni2 Ni4 O3 -4.9(4) . . . . ? N11 Ni2 Ni4 O3 -95.4(4) . . . . ? O4 Ni2 Ni4 O3 171.0(4) . . . . ? N3 Ni2 Ni4 O3 171.2(6) . . . . ? N10 Ni2 Ni4 O3 85.5(4) . . . . ? N4 Ni2 Ni4 O4 -175.9(4) . . . . ? N11 Ni2 Ni4 O4 93.5(4) . . . . ? O3 Ni2 Ni4 O4 -171.0(4) . . . . ? N3 Ni2 Ni4 O4 0.2(6) . . . . ? N10 Ni2 Ni4 O4 -85.5(4) . . . . ? N4 Ni2 Ni4 N6 172.7(5) . . . . ? N11 Ni2 Ni4 N6 82.1(4) . . . . ? O4 Ni2 Ni4 N6 -11.4(5) . . . . ? O3 Ni2 Ni4 N6 177.6(5) . . . . ? N3 Ni2 Ni4 N6 -11.2(6) . . . . ? N10 Ni2 Ni4 N6 -96.9(4) . . . . ? O1 Ni3 N1 C7 0.1(10) . . . . ? O2 Ni3 N1 C7 -119(4) . . . . ? N2 Ni3 N1 C7 -178.0(9) . . . . ? Ni1 Ni3 N1 C7 -0.5(11) . . . . ? O1 Ni3 N1 C19 179.0(7) . . . . ? O2 Ni3 N1 C19 60(5) . . . . ? N2 Ni3 N1 C19 1.0(7) . . . . ? Ni1 Ni3 N1 C19 178.5(5) . . . . ? O1 Ni3 N2 C20 -133(3) . . . . ? N1 Ni3 N2 C20 27.1(7) . . . . ? O2 Ni3 N2 C20 -149.1(7) . . . . ? Ni1 Ni3 N2 C20 -150.8(6) . . . . ? O1 Ni3 N2 C21 -8(4) . . . . ? N1 Ni3 N2 C21 152.2(7) . . . . ? O2 Ni3 N2 C21 -24.0(7) . . . . ? Ni1 Ni3 N2 C21 -25.6(8) . . . . ? N4 Ni2 N3 C23 -104.7(8) . . . . ? N11 Ni2 N3 C23 -13.6(8) . . . . ? O4 Ni2 N3 C23 78.6(8) . . . . ? O3 Ni2 N3 C23 -134.6(16) . . . . ? N10 Ni2 N3 C23 165.5(8) . . . . ? Ni4 Ni2 N3 C23 78.5(9) . . . . ? N4 Ni2 N3 C24 19.7(6) . . . . ? N11 Ni2 N3 C24 110.8(7) . . . . ? O4 Ni2 N3 C24 -157.0(6) . . . . ? O3 Ni2 N3 C24 -10(2) . . . . ? N10 Ni2 N3 C24 -70.1(7) . . . . ? Ni4 Ni2 N3 C24 -157.1(5) . . . . ? N11 Ni2 N4 C16 96.1(10) . . . . ? O4 Ni2 N4 C16 -1.0(18) . . . . ? O3 Ni2 N4 C16 4.1(10) . . . . ? N3 Ni2 N4 C16 -171.0(10) . . . . ? N10 Ni2 N4 C16 -84.4(10) . . . . ? Ni4 Ni2 N4 C16 7.2(11) . . . . ? N11 Ni2 N4 C25 -86.5(7) . . . . ? O4 Ni2 N4 C25 176.3(9) . . . . ? O3 Ni2 N4 C25 -178.5(7) . . . . ? N3 Ni2 N4 C25 6.4(7) . . . . ? N10 Ni2 N4 C25 93.0(7) . . . . ? Ni4 Ni2 N4 C25 -175.5(6) . . . . ? O3 Ni4 N5 C18 -3.8(10) . . . . ? O4 Ni4 N5 C18 -132(5) . . . . ? N6 Ni4 N5 C18 178.7(10) . . . . ? Ni2 Ni4 N5 C18 -13.3(12) . . . . ? O3 Ni4 N5 C26 176.8(7) . . . . ? O4 Ni4 N5 C26 49(6) . . . . ? N6 Ni4 N5 C26 -0.7(7) . . . . ? Ni2 Ni4 N5 C26 167.3(5) . . . . ? N5 Ni4 N6 C27 26.6(7) . . . . ? O3 Ni4 N6 C27 -123(4) . . . . ? O4 Ni4 N6 C27 -150.6(7) . . . . ? Ni2 Ni4 N6 C27 -142.8(6) . . . . ? N5 Ni4 N6 C28 151.6(7) . . . . ? O3 Ni4 N6 C28 2(4) . . . . ? O4 Ni4 N6 C28 -25.6(6) . . . . ? Ni2 Ni4 N6 C28 -17.8(8) . . . . ? N8 Ni1 N7 C31 22.6(7) . . . . ? N9 Ni1 N7 C31 -72.5(7) . . . . ? O1 Ni1 N7 C31 11(2) . . . . ? O2 Ni1 N7 C31 -163.3(6) . . . . ? O5 Ni1 N7 C31 113.2(7) . . . . ? Ni3 Ni1 N7 C31 -158.3(5) . . . . ? N8 Ni1 N7 C30 -101.0(8) . . . . ? N9 Ni1 N7 C30 164.0(8) . . . . ? O1 Ni1 N7 C30 -112(2) . . . . ? O2 Ni1 N7 C30 73.2(8) . . . . ? O5 Ni1 N7 C30 -10.3(8) . . . . ? Ni3 Ni1 N7 C30 78.2(9) . . . . ? N9 Ni1 N8 C9 -85.9(10) . . . . ? O1 Ni1 N8 C9 5.7(10) . . . . ? O2 Ni1 N8 C9 23.5(17) . . . . ? N7 Ni1 N8 C9 -172.6(10) . . . . ? O5 Ni1 N8 C9 93.3(10) . . . . ? Ni3 Ni1 N8 C9 7.9(11) . . . . ? N9 Ni1 N8 C32 90.9(7) . . . . ? O1 Ni1 N8 C32 -177.5(7) . . . . ? O2 Ni1 N8 C32 -159.8(9) . . . . ? N7 Ni1 N8 C32 4.1(7) . . . . ? O5 Ni1 N8 C32 -89.9(7) . . . . ? Ni3 Ni1 N8 C32 -175.4(6) . . . . ? N8 Ni1 N9 C33 -66(7) . . . . ? O1 Ni1 N9 C33 -153(7) . . . . ? O2 Ni1 N9 C33 133(7) . . . . ? N7 Ni1 N9 C33 19(7) . . . . ? O5 Ni1 N9 C33 122(7) . . . . ? Ni3 Ni1 N9 C33 170(7) . . . . ? N4 Ni2 N10 C34 4.6(12) . . . . ? N11 Ni2 N10 C34 153(20) . . . . ? O4 Ni2 N10 C34 -157.8(12) . . . . ? O3 Ni2 N10 C34 -82.5(12) . . . . ? N3 Ni2 N10 C34 89.0(12) . . . . ? Ni4 Ni2 N10 C34 -120.2(12) . . . . ? N4 Ni2 N11 C35 91(3) . . . . ? O4 Ni2 N11 C35 -107(3) . . . . ? O3 Ni2 N11 C35 178(3) . . . . ? N3 Ni2 N11 C35 6(3) . . . . ? N10 Ni2 N11 C35 -58(21) . . . . ? Ni4 Ni2 N11 C35 -145(3) . . . . ? N1 Ni3 O1 C1 0.4(9) . . . . ? O2 Ni3 O1 C1 176.5(8) . . . . ? N2 Ni3 O1 C1 161(3) . . . . ? Ni1 Ni3 O1 C1 179.9(10) . . . . ? N1 Ni3 O1 Ni1 -179.5(3) . . . . ? O2 Ni3 O1 Ni1 -3.4(3) . . . . ? N2 Ni3 O1 Ni1 -19(4) . . . . ? N8 Ni1 O1 C1 -2.8(9) . . . . ? N9 Ni1 O1 C1 91.9(9) . . . . ? O2 Ni1 O1 C1 -176.8(9) . . . . ? N7 Ni1 O1 C1 8(3) . . . . ? O5 Ni1 O1 C1 -94.0(9) . . . . ? Ni3 Ni1 O1 C1 -179.9(10) . . . . ? N8 Ni1 O1 Ni3 177.0(4) . . . . ? N9 Ni1 O1 Ni3 -88.3(4) . . . . ? O2 Ni1 O1 Ni3 3.1(3) . . . . ? N7 Ni1 O1 Ni3 -171.6(19) . . . . ? O5 Ni1 O1 Ni3 85.9(3) . . . . ? O1 Ni3 O2 C22 178.1(7) . . . . ? N1 Ni3 O2 C22 -62(5) . . . . ? N2 Ni3 O2 C22 -3.5(7) . . . . ? Ni1 Ni3 O2 C22 174.8(8) . . . . ? O1 Ni3 O2 Ni1 3.4(3) . . . . ? N1 Ni3 O2 Ni1 123(5) . . . . ? N2 Ni3 O2 Ni1 -178.2(4) . . . . ? N8 Ni1 O2 C22 167.7(12) . . . . ? N9 Ni1 O2 C22 -82.5(12) . . . . ? O1 Ni1 O2 C22 -173.9(12) . . . . ? N7 Ni1 O2 C22 5.3(13) . . . . ? O5 Ni1 O2 C22 96.4(12) . . . . ? Ni3 Ni1 O2 C22 -170.8(14) . . . . ? N8 Ni1 O2 Ni3 -21.5(11) . . . . ? N9 Ni1 O2 Ni3 88.3(4) . . . . ? O1 Ni1 O2 Ni3 -3.1(3) . . . . ? N7 Ni1 O2 Ni3 176.1(3) . . . . ? O5 Ni1 O2 Ni3 -92.8(3) . . . . ? N5 Ni4 O3 C10 2.0(9) . . . . ? O4 Ni4 O3 C10 179.1(8) . . . . ? N6 Ni4 O3 C10 152(4) . . . . ? Ni2 Ni4 O3 C10 172.9(10) . . . . ? N5 Ni4 O3 Ni2 -170.9(3) . . . . ? O4 Ni4 O3 Ni2 6.1(3) . . . . ? N6 Ni4 O3 Ni2 -21(4) . . . . ? N4 Ni2 O3 C10 3.6(9) . . . . ? N11 Ni2 O3 C10 -87.6(9) . . . . ? O4 Ni2 O3 C10 -178.0(9) . . . . ? N3 Ni2 O3 C10 33(2) . . . . ? N10 Ni2 O3 C10 93.2(9) . . . . ? Ni4 Ni2 O3 C10 -172.3(10) . . . . ? N4 Ni2 O3 Ni4 176.0(4) . . . . ? N11 Ni2 O3 Ni4 84.7(4) . . . . ? O4 Ni2 O3 Ni4 -5.7(3) . . . . ? N3 Ni2 O3 Ni4 -154.3(17) . . . . ? N10 Ni2 O3 Ni4 -94.5(4) . . . . ? N5 Ni4 O4 C29 -48(6) . . . . ? O3 Ni4 O4 C29 -176.5(7) . . . . ? N6 Ni4 O4 C29 1.1(7) . . . . ? Ni2 Ni4 O4 C29 -170.4(8) . . . . ? N5 Ni4 O4 Ni2 122(5) . . . . ? O3 Ni4 O4 Ni2 -6.2(3) . . . . ? N6 Ni4 O4 Ni2 171.5(3) . . . . ? N4 Ni2 O4 C29 174.9(11) . . . . ? N11 Ni2 O4 C29 77.7(11) . . . . ? O3 Ni2 O4 C29 169.5(12) . . . . ? N3 Ni2 O4 C29 -16.0(12) . . . . ? N10 Ni2 O4 C29 -101.6(11) . . . . ? Ni4 Ni2 O4 C29 163.9(13) . . . . ? N4 Ni2 O4 Ni4 11.0(12) . . . . ? N11 Ni2 O4 Ni4 -86.2(4) . . . . ? O3 Ni2 O4 Ni4 5.7(3) . . . . ? N3 Ni2 O4 Ni4 -179.9(3) . . . . ? N10 Ni2 O4 Ni4 94.5(3) . . . . ? N8 Ni1 O5 C36 -12.6(12) . . . . ? N9 Ni1 O5 C36 160(3) . . . . ? O1 Ni1 O5 C36 74.4(12) . . . . ? O2 Ni1 O5 C36 149.0(12) . . . . ? N7 Ni1 O5 C36 -97.3(12) . . . . ? Ni3 Ni1 O5 C36 111.5(12) . . . . ? Ni3 O1 C1 C6 -179.3(7) . . . . ? Ni1 O1 C1 C6 0.6(14) . . . . ? Ni3 O1 C1 C2 0.8(14) . . . . ? Ni1 O1 C1 C2 -179.4(7) . . . . ? O1 C1 C2 C3 177.7(10) . . . . ? C6 C1 C2 C3 -2.2(15) . . . . ? O1 C1 C2 C7 -2.5(16) . . . . ? C6 C1 C2 C7 177.5(9) . . . . ? C1 C2 C3 C4 1.9(16) . . . . ? C7 C2 C3 C4 -177.8(10) . . . . ? C2 C3 C4 C5 -1.3(16) . . . . ? C2 C3 C4 C8 177.3(10) . . . . ? C3 C4 C5 C6 1.1(17) . . . . ? C8 C4 C5 C6 -177.5(10) . . . . ? C4 C5 C6 C1 -1.5(17) . . . . ? C4 C5 C6 C9 179.7(10) . . . . ? O1 C1 C6 C5 -178.0(9) . . . . ? C2 C1 C6 C5 1.9(15) . . . . ? O1 C1 C6 C9 0.7(16) . . . . ? C2 C1 C6 C9 -179.4(10) . . . . ? C19 N1 C7 C2 179.4(10) . . . . ? Ni3 N1 C7 C2 -1.8(16) . . . . ? C3 C2 C7 N1 -177.1(10) . . . . ? C1 C2 C7 N1 3.2(17) . . . . ? C32 N8 C9 C6 176.9(10) . . . . ? Ni1 N8 C9 C6 -6.5(17) . . . . ? C5 C6 C9 N8 -178.9(11) . . . . ? C1 C6 C9 N8 2.4(18) . . . . ? Ni4 O3 C10 C15 2.1(14) . . . . ? Ni2 O3 C10 C15 172.5(7) . . . . ? Ni4 O3 C10 C11 -178.6(7) . . . . ? Ni2 O3 C10 C11 -8.2(14) . . . . ? O3 C10 C11 C12 -176.8(9) . . . . ? C15 C10 C11 C12 2.5(16) . . . . ? O3 C10 C11 C16 5.8(16) . . . . ? C15 C10 C11 C16 -174.9(10) . . . . ? C10 C11 C12 C13 -1.1(16) . . . . ? C16 C11 C12 C13 176.6(10) . . . . ? C11 C12 C13 C14 -0.6(17) . . . . ? C11 C12 C13 C17 -178.3(10) . . . . ? C12 C13 C14 C15 0.9(17) . . . . ? C17 C13 C14 C15 178.5(10) . . . . ? O3 C10 C15 C14 177.0(9) . . . . ? C11 C10 C15 C14 -2.3(16) . . . . ? O3 C10 C15 C18 -5.7(16) . . . . ? C11 C10 C15 C18 175.0(10) . . . . ? C13 C14 C15 C10 0.5(17) . . . . ? C13 C14 C15 C18 -176.9(10) . . . . ? C25 N4 C16 C11 175.8(10) . . . . ? Ni2 N4 C16 C11 -7.1(17) . . . . ? C12 C11 C16 N4 -175.7(11) . . . . ? C10 C11 C16 N4 1.8(19) . . . . ? C26 N5 C18 C15 -179.2(10) . . . . ? Ni4 N5 C18 C15 1.5(16) . . . . ? C10 C15 C18 N5 4.0(18) . . . . ? C14 C15 C18 N5 -178.7(10) . . . . ? C7 N1 C19 C20 152.1(10) . . . . ? Ni3 N1 C19 C20 -26.9(10) . . . . ? C21 N2 C20 C19 -164.6(9) . . . . ? Ni3 N2 C20 C19 -46.4(10) . . . . ? N1 C19 C20 N2 46.9(11) . . . . ? C20 N2 C21 C22 163.0(9) . . . . ? Ni3 N2 C21 C22 44.0(9) . . . . ? Ni3 O2 C22 C23 -92.8(8) . . . . ? Ni1 O2 C22 C23 77.5(14) . . . . ? Ni3 O2 C22 C21 28.9(9) . . . . ? Ni1 O2 C22 C21 -160.9(9) . . . . ? N2 C21 C22 O2 -47.6(11) . . . . ? N2 C21 C22 C23 75.1(11) . . . . ? C24 N3 C23 C22 170.1(9) . . . . ? Ni2 N3 C23 C22 -68.3(11) . . . . ? O2 C22 C23 N3 -59.6(12) . . . . ? C21 C22 C23 N3 -178.8(9) . . . . ? C23 N3 C24 C25 88.5(10) . . . . ? Ni2 N3 C24 C25 -42.9(10) . . . . ? C16 N4 C25 C24 145.4(10) . . . . ? Ni2 N4 C25 C24 -32.2(10) . . . . ? N3 C24 C25 N4 51.1(12) . . . . ? C18 N5 C26 C27 156.2(10) . . . . ? Ni4 N5 C26 C27 -24.3(11) . . . . ? C28 N6 C27 C26 -163.1(9) . . . . ? Ni4 N6 C27 C26 -45.2(10) . . . . ? N5 C26 C27 N6 44.2(11) . . . . ? C27 N6 C28 C29 161.2(9) . . . . ? Ni4 N6 C28 C29 42.2(9) . . . . ? Ni4 O4 C29 C30 -99.2(8) . . . . ? Ni2 O4 C29 C30 98.2(12) . . . . ? Ni4 O4 C29 C28 22.8(10) . . . . ? Ni2 O4 C29 C28 -139.8(9) . . . . ? N6 C28 C29 O4 -42.7(11) . . . . ? N6 C28 C29 C30 79.9(11) . . . . ? C31 N7 C30 C29 168.4(9) . . . . ? Ni1 N7 C30 C29 -72.2(10) . . . . ? O4 C29 C30 N7 -58.5(11) . . . . ? C28 C29 C30 N7 -178.8(8) . . . . ? C30 N7 C31 C32 83.8(11) . . . . ? Ni1 N7 C31 C32 -45.2(10) . . . . ? C9 N8 C32 C31 147.7(10) . . . . ? Ni1 N8 C32 C31 -29.4(10) . . . . ? N7 C31 C32 N8 51.4(12) . . . . ? Ni1 N9 C33 S1 -153(72) . . . . ? Ni2 N10 C34 S2 56(38) . . . . ? Ni2 N11 C35 S3 123(8) . . . . ? Ni2 N11 C35 S3' -83(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.731 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.122 #END data_0406cm _database_code_depnum_ccdc_archive 'CCDC 886468' #TrackingRef '- 3-Xie-CCDC 886465-886468.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H112 Cl2 Cu8 N22 O28 S6' _chemical_formula_weight 2481.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 27.5390(9) _cell_length_b 27.5390(9) _cell_length_c 13.4753(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10219.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5088 _exptl_absorpt_coefficient_mu 1.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6298 _exptl_absorpt_correction_T_max 0.6602 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34882 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4423 _reflns_number_gt 3521 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1616P)^2^+53.9386P] 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 4423 _refine_ls_number_parameters 360 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2401 _refine_ls_wR_factor_gt 0.2194 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.96605(3) 0.84897(3) 0.03132(6) 0.0424(3) Uani 1 1 d . . . Cu2 Cu 1.05569(3) 0.85934(3) 0.15306(6) 0.0516(3) Uani 1 1 d . . . Cl1 Cl 1.0000 0.7500 -0.1250 0.0404(6) Uani 1 4 d S . . Cl2 Cl 1.0000 0.7500 0.3750 0.0923(16) Uani 1 4 d S . . S1 S 0.7322(7) 0.6585(13) 0.266(2) 0.128(3) Uani 0.424(19) 1 d P A 1 S2 S 0.7133(10) 0.7079(13) 0.106(2) 0.128(3) Uani 0.161(9) 1 d P B 2 S3 S 0.7381(4) 0.6913(6) 0.1154(9) 0.128(3) Uani 0.396(9) 1 d P C 3 S4 S 0.7529(6) 0.7306(9) 0.3426(14) 0.128(3) Uani 0.224(9) 1 d P D 4 S5 S 0.7402(7) 0.6822(10) 0.279(3) 0.115(10) Uani 0.294(19) 1 d P E 5 N1 N 0.94052(19) 0.88935(19) -0.0741(4) 0.0442(12) Uani 1 1 d . . . N2 N 0.90152(19) 0.8132(2) 0.0196(5) 0.0470(13) Uani 1 1 d . . . H2 H 0.905 0.790 -0.027 0.056 Uiso 1 1 calc . . . N3 N 0.9074(3) 0.6752(3) 0.2593(5) 0.0641(17) Uani 1 1 d . . . H3 H 0.929 0.686 0.305 0.077 Uiso 1 1 calc . . . N4 N 0.8915(2) 0.5970(3) 0.1493(5) 0.0635(17) Uani 1 1 d . . . N5 N 0.7518(9) 0.6590(13) 0.061(2) 0.105(6) Uani 0.424(19) 1 d P A 1 N6 N 0.737(5) 0.665(10) 0.296(12) 0.105(6) Uani 0.161(9) 1 d P B 2 N7 N 0.7690(8) 0.6014(13) 0.029(2) 0.105(6) Uani 0.396(9) 1 d P C 3 N8 N 0.7371(16) 0.627(3) 0.340(5) 0.105(6) Uani 0.224(9) 1 d P D 4 N9 N 0.7195(9) 0.5797(15) 0.293(3) 0.098(12) Uani 0.294(19) 1 d P E 5 O1 O 1.02363(16) 0.89187(16) 0.0423(3) 0.0475(11) Uani 1 1 d . . . O2 O 0.90565(18) 0.71024(17) 0.0530(4) 0.0535(12) Uani 1 1 d . . . H2C H 0.9316 0.7124 0.0233 0.064 Uiso 1 1 calc R . . O3 O 1.01180(18) 0.79161(18) -0.0632(4) 0.0583(13) Uani 1 1 d . . . O4 O 0.9681(3) 0.7805(3) 0.3144(5) 0.110(3) Uani 1 1 d . . . O5 O 0.99577(19) 0.8256(2) 0.1472(4) 0.0605(13) Uani 1 1 d . . . H5 H 0.9870 0.8114 0.2003 0.073 Uiso 1 1 d R . . O6 O 0.7785(3) 0.5387(5) 0.8921(10) 0.160(5) Uani 1 1 d . . . H6C H 0.7761 0.5597 0.9381 0.192 Uiso 1 1 d R . . H6D H 0.7744 0.5107 0.9175 0.192 Uiso 1 1 d R . . O7 O 0.7650(3) 0.9535(4) 0.0274(8) 0.136(3) Uani 1 1 d . . . H7C H 0.7733 0.9505 -0.0330 0.163 Uiso 1 1 d R . . H7D H 0.7635 0.9255 0.0538 0.163 Uiso 1 1 d R . . C1 C 1.0377(2) 0.9299(2) -0.0077(5) 0.0449(14) Uani 1 1 d . . . C2 C 1.0810(3) 0.9547(3) 0.0106(6) 0.0553(17) Uani 1 1 d . . . C3 C 1.0950(3) 0.9940(2) -0.0464(6) 0.0564(18) Uani 1 1 d . . . H3A H 1.1246 1.0089 -0.0329 0.068 Uiso 1 1 calc R . . C4 C 1.0667(3) 1.0121(3) -0.1225(6) 0.0567(18) Uani 1 1 d . . . C5 C 1.0232(3) 0.9892(3) -0.1407(5) 0.0521(16) Uani 1 1 d . . . H5A H 1.0035 1.0013 -0.1911 0.063 Uiso 1 1 calc R . . C6 C 1.0067(2) 0.9484(2) -0.0869(5) 0.0449(14) Uani 1 1 d . . . C7 C 0.9609(3) 0.9278(2) -0.1125(5) 0.0465(15) Uani 1 1 d . . . H7 H 0.9435 0.9436 -0.1622 0.056 Uiso 1 1 calc R . . C8 C 0.8947(3) 0.8738(3) -0.1100(5) 0.0512(16) Uani 1 1 d . . . H8A H 0.8989 0.8507 -0.1637 0.061 Uiso 1 1 calc R . . H8B H 0.8762 0.9012 -0.1345 0.061 Uiso 1 1 calc R . . C9 C 0.8682(2) 0.8497(2) -0.0223(5) 0.0478(15) Uani 1 1 d . . . H9A H 0.8599 0.8738 0.0274 0.057 Uiso 1 1 calc R . . H9B H 0.8385 0.8343 -0.0450 0.057 Uiso 1 1 calc R . . C10 C 0.8806(3) 0.7897(3) 0.1085(5) 0.0536(17) Uani 1 1 d . . . H10A H 0.8464 0.7833 0.0968 0.064 Uiso 1 1 calc R . . H10B H 0.8830 0.8118 0.1643 0.064 Uiso 1 1 calc R . . C11 C 0.9056(3) 0.7429(3) 0.1344(5) 0.0528(16) Uani 1 1 d . . . H11 H 0.9392 0.7498 0.1537 0.063 Uiso 1 1 calc R . . C12 C 0.8801(3) 0.7178(3) 0.2194(6) 0.0620(19) Uani 1 1 d . . . H12A H 0.8752 0.7410 0.2725 0.074 Uiso 1 1 calc R . . H12B H 0.8484 0.7070 0.1972 0.074 Uiso 1 1 calc R . . C13 C 0.8764(4) 0.6386(4) 0.3057(7) 0.077(3) Uani 1 1 d . . . H13A H 0.8519 0.6541 0.3466 0.093 Uiso 1 1 calc R . . H13B H 0.8956 0.6173 0.3474 0.093 Uiso 1 1 calc R . . C14 C 0.8526(3) 0.6100(4) 0.2233(8) 0.088(3) Uani 1 1 d . . . H14A H 0.8378 0.5807 0.2497 0.106 Uiso 1 1 calc R . . H14B H 0.8275 0.6293 0.1917 0.106 Uiso 1 1 calc R . . C15 C 0.8854(3) 0.5592(3) 0.0877(6) 0.064(2) Uani 1 1 d . . . H15 H 0.8574 0.5406 0.0953 0.077 Uiso 1 1 calc R . . C16 C 1.0832(4) 1.0550(3) -0.1848(7) 0.078(2) Uani 1 1 d . . . H16A H 1.0793 1.0474 -0.2539 0.117 Uiso 1 1 calc R . . H16B H 1.1167 1.0618 -0.1713 0.117 Uiso 1 1 calc R . . H16C H 1.0639 1.0829 -0.1686 0.117 Uiso 1 1 calc R . . C17 C 0.7433(9) 0.6512(14) 0.142(3) 0.102(8) Uani 0.424(19) 1 d P A 1 C18 C 0.722(3) 0.680(4) 0.217(7) 0.102(8) Uani 0.161(9) 1 d P B 2 C19 C 0.7618(11) 0.637(2) 0.071(3) 0.102(8) Uani 0.396(9) 1 d P C 3 C20 C 0.743(2) 0.670(4) 0.337(6) 0.102(8) Uani 0.224(9) 1 d P D 4 C21 C 0.7216(15) 0.622(3) 0.290(4) 0.107(17) Uani 0.294(19) 1 d P E 5 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0410(5) 0.0456(5) 0.0406(5) 0.0015(3) -0.0071(3) 0.0000(3) Cu2 0.0505(5) 0.0556(6) 0.0488(6) -0.0041(4) -0.0162(4) 0.0020(4) Cl1 0.0434(9) 0.0434(9) 0.0345(14) 0.000 0.000 0.000 Cl2 0.123(3) 0.123(3) 0.0303(18) 0.000 0.000 0.000 S1 0.083(5) 0.182(9) 0.119(5) 0.040(5) 0.019(4) 0.011(5) S2 0.083(5) 0.182(9) 0.119(5) 0.040(5) 0.019(4) 0.011(5) S3 0.083(5) 0.182(9) 0.119(5) 0.040(5) 0.019(4) 0.011(5) S4 0.083(5) 0.182(9) 0.119(5) 0.040(5) 0.019(4) 0.011(5) S5 0.054(8) 0.18(2) 0.114(14) 0.055(17) 0.034(10) 0.034(11) N1 0.043(3) 0.042(3) 0.047(3) -0.004(2) -0.007(2) 0.008(2) N2 0.040(3) 0.047(3) 0.054(3) -0.006(3) -0.001(2) 0.002(2) N3 0.066(4) 0.073(4) 0.053(4) 0.012(3) 0.024(3) 0.017(3) N4 0.054(4) 0.063(4) 0.074(4) 0.016(3) 0.025(3) -0.002(3) N5 0.049(7) 0.144(16) 0.122(14) 0.035(13) -0.007(8) 0.011(8) N6 0.049(7) 0.144(16) 0.122(14) 0.035(13) -0.007(8) 0.011(8) N7 0.049(7) 0.144(16) 0.122(14) 0.035(13) -0.007(8) 0.011(8) N8 0.049(7) 0.144(16) 0.122(14) 0.035(13) -0.007(8) 0.011(8) N9 0.038(13) 0.13(3) 0.13(3) 0.04(2) 0.035(14) 0.008(15) O1 0.049(2) 0.042(2) 0.051(3) 0.0025(19) -0.013(2) -0.0014(19) O2 0.057(3) 0.055(3) 0.049(3) -0.004(2) 0.011(2) -0.003(2) O3 0.055(3) 0.059(3) 0.061(3) -0.022(2) -0.014(2) 0.011(2) O4 0.114(6) 0.161(8) 0.054(4) 0.042(4) -0.016(4) -0.010(5) O5 0.057(3) 0.074(3) 0.051(3) 0.010(2) -0.014(2) -0.014(3) O6 0.080(5) 0.197(11) 0.204(11) 0.098(9) -0.026(6) 0.033(6) O7 0.105(6) 0.141(8) 0.161(9) 0.036(7) -0.010(6) -0.006(6) C1 0.043(3) 0.043(3) 0.048(4) -0.010(3) 0.002(3) 0.003(3) C2 0.055(4) 0.047(4) 0.063(4) -0.018(3) 0.006(3) -0.001(3) C3 0.057(4) 0.042(4) 0.070(5) -0.012(3) 0.011(4) -0.002(3) C4 0.067(5) 0.045(4) 0.058(4) -0.008(3) 0.018(4) 0.002(3) C5 0.058(4) 0.045(4) 0.053(4) -0.005(3) 0.005(3) 0.006(3) C6 0.048(3) 0.039(3) 0.049(4) -0.005(3) 0.001(3) 0.003(3) C7 0.054(4) 0.042(3) 0.044(3) 0.000(3) -0.005(3) 0.008(3) C8 0.053(4) 0.051(4) 0.050(4) -0.002(3) -0.006(3) -0.002(3) C9 0.044(3) 0.049(4) 0.051(4) -0.003(3) -0.004(3) 0.003(3) C10 0.054(4) 0.054(4) 0.053(4) 0.000(3) 0.012(3) -0.001(3) C11 0.045(4) 0.063(4) 0.050(4) -0.003(3) 0.016(3) 0.001(3) C12 0.072(5) 0.059(4) 0.055(4) 0.008(3) 0.021(4) 0.007(4) C13 0.083(6) 0.083(6) 0.065(5) 0.016(4) 0.036(5) 0.013(5) C14 0.064(5) 0.104(7) 0.096(7) 0.019(6) 0.034(5) 0.007(5) C15 0.055(4) 0.066(5) 0.071(5) 0.023(4) 0.016(4) 0.002(4) C16 0.092(6) 0.059(5) 0.084(6) 0.003(4) 0.017(5) -0.018(4) C17 0.049(11) 0.14(2) 0.118(19) 0.038(16) -0.008(9) 0.016(11) C18 0.049(11) 0.14(2) 0.118(19) 0.038(16) -0.008(9) 0.016(11) C19 0.049(11) 0.14(2) 0.118(19) 0.038(16) -0.008(9) 0.016(11) C20 0.049(11) 0.14(2) 0.118(19) 0.038(16) -0.008(9) 0.016(11) C21 0.06(2) 0.15(5) 0.11(4) 0.04(4) 0.01(2) 0.01(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 Cu1 O5 1.877(5) . ? Cu1 N1 1.937(5) . ? Cu1 O1 1.983(4) . ? Cu1 N2 2.038(6) . ? Cu1 O3 2.389(5) . ? Cu1 Cu2 2.9778(11) . ? Cu2 N4 1.887(7) 6_664 ? Cu2 O5 1.896(5) . ? Cu2 O1 1.952(4) . ? Cu2 N3 1.997(6) 6_664 ? Cl1 O3 1.453(5) 16_755 ? Cl1 O3 1.453(5) . ? Cl1 O3 1.453(5) 11_675 ? Cl1 O3 1.453(5) 6_664 ? Cl2 O4 1.463(8) 11_676 ? Cl2 O4 1.463(8) 6_664 ? Cl2 O4 1.463(8) 16_756 ? Cl2 O4 1.463(8) . ? S1 C17 1.71(4) . ? S2 C18 1.69(10) . ? S3 C19 1.73(6) . ? S4 C20 1.70(11) . ? S5 C21 1.73(8) . ? N1 C7 1.305(9) . ? N1 C8 1.418(9) . ? N2 C9 1.475(8) . ? N2 C10 1.478(9) . ? N3 C13 1.463(11) . ? N3 C12 1.492(10) . ? N3 Cu2 1.997(6) 6_664 ? N4 C15 1.342(11) . ? N4 C14 1.506(11) . ? N4 Cu2 1.887(7) 6_664 ? N5 C17 1.15(4) . ? N6 C18 1.21(18) . ? N7 C19 1.16(5) . ? N8 C20 1.18(11) . ? N9 C21 1.18(7) . ? O1 C1 1.303(8) . ? O2 C11 1.418(9) . ? C1 C2 1.397(10) . ? C1 C6 1.459(9) . ? C2 C3 1.382(11) . ? C2 C15 1.443(11) 6_664 ? C3 C4 1.380(12) . ? C4 C5 1.376(11) . ? C4 C16 1.519(11) . ? C5 C6 1.413(10) . ? C6 C7 1.427(10) . ? C8 C9 1.539(10) . ? C10 C11 1.504(10) . ? C11 C12 1.510(10) . ? C13 C14 1.511(15) . ? C15 C2 1.443(11) 6_664 ? 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 O5 Cu1 N1 165.0(2) . . ? O5 Cu1 O1 78.1(2) . . ? N1 Cu1 O1 90.2(2) . . ? O5 Cu1 N2 106.2(2) . . ? N1 Cu1 N2 84.5(2) . . ? O1 Cu1 N2 172.3(2) . . ? O5 Cu1 O3 89.3(2) . . ? N1 Cu1 O3 100.4(2) . . ? O1 Cu1 O3 90.68(18) . . ? N2 Cu1 O3 95.7(2) . . ? O5 Cu1 Cu2 38.11(16) . . ? N1 Cu1 Cu2 130.55(17) . . ? O1 Cu1 Cu2 40.44(12) . . ? N2 Cu1 Cu2 144.27(17) . . ? O3 Cu1 Cu2 85.42(12) . . ? N4 Cu2 O5 169.1(3) 6_664 . ? N4 Cu2 O1 92.0(2) 6_664 . ? O5 Cu2 O1 78.4(2) . . ? N4 Cu2 N3 86.1(3) 6_664 6_664 ? O5 Cu2 N3 103.8(3) . 6_664 ? O1 Cu2 N3 175.6(3) . 6_664 ? N4 Cu2 Cu1 133.2(2) 6_664 . ? O5 Cu2 Cu1 37.66(15) . . ? O1 Cu2 Cu1 41.21(13) . . ? N3 Cu2 Cu1 140.4(2) 6_664 . ? O3 Cl1 O3 109.2(2) 16_755 . ? O3 Cl1 O3 110.1(4) 16_755 11_675 ? O3 Cl1 O3 109.2(2) . 11_675 ? O3 Cl1 O3 109.2(2) 16_755 6_664 ? O3 Cl1 O3 110.1(4) . 6_664 ? O3 Cl1 O3 109.2(2) 11_675 6_664 ? O4 Cl2 O4 108.1(3) 11_676 6_664 ? O4 Cl2 O4 112.2(7) 11_676 16_756 ? O4 Cl2 O4 108.1(3) 6_664 16_756 ? O4 Cl2 O4 108.1(3) 11_676 . ? O4 Cl2 O4 112.2(7) 6_664 . ? O4 Cl2 O4 108.1(3) 16_756 . ? C7 N1 C8 119.5(6) . . ? C7 N1 Cu1 126.9(5) . . ? C8 N1 Cu1 113.5(4) . . ? C9 N2 C10 111.5(5) . . ? C9 N2 Cu1 104.1(4) . . ? C10 N2 Cu1 119.3(5) . . ? C13 N3 C12 113.6(7) . . ? C13 N3 Cu2 106.0(5) . 6_664 ? C12 N3 Cu2 111.9(5) . 6_664 ? C15 N4 C14 120.3(7) . . ? C15 N4 Cu2 127.4(5) . 6_664 ? C14 N4 Cu2 112.3(6) . 6_664 ? C1 O1 Cu2 129.0(4) . . ? C1 O1 Cu1 132.7(4) . . ? Cu2 O1 Cu1 98.4(2) . . ? Cl1 O3 Cu1 135.2(3) . . ? Cu1 O5 Cu2 104.2(2) . . ? O1 C1 C2 123.7(6) . . ? O1 C1 C6 119.0(6) . . ? C2 C1 C6 117.2(6) . . ? C3 C2 C1 121.5(7) . . ? C3 C2 C15 115.4(7) . 6_664 ? C1 C2 C15 123.0(7) . 6_664 ? C4 C3 C2 122.6(7) . . ? C5 C4 C3 117.2(7) . . ? C5 C4 C16 121.2(8) . . ? C3 C4 C16 121.6(8) . . ? C4 C5 C6 123.6(7) . . ? C5 C6 C7 118.5(6) . . ? C5 C6 C1 117.8(6) . . ? C7 C6 C1 123.7(6) . . ? N1 C7 C6 127.3(6) . . ? N1 C8 C9 107.0(6) . . ? N2 C9 C8 107.0(5) . . ? N2 C10 C11 112.6(6) . . ? O2 C11 C10 111.4(6) . . ? O2 C11 C12 107.3(6) . . ? C10 C11 C12 110.9(6) . . ? N3 C12 C11 113.5(6) . . ? N3 C13 C14 107.4(7) . . ? N4 C14 C13 107.6(7) . . ? N4 C15 C2 124.8(7) . 6_664 ? N5 C17 S1 162(4) . . ? N6 C18 S2 168(10) . . ? N7 C19 S3 165(3) . . ? N8 C20 S4 175(7) . . ? N9 C21 S5 165(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.773 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.157 #END