Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shie-Ming Peng' _publ_contact_author_address ; Department of Chemistry National Taiwan University No. 1, Sec. 4, Roosevelt Road Taipei 106 TAIWAN ; _publ_contact_author_email SMPENG@NTU.EDU.TW _publ_section_title ; New versatile ligand family, pyrazine-modulated oligo-alpha-pyridylamino ligands, from coordination polymer to extended metal atom chains ; loop_ _publ_author_name 'Shie-Ming Peng.' 'Rayyat H. Ismayilov' 'Gene-Hsiung Lee.' 'I.Po-Chun Liu' ; Rui-Ren Wang ; 'Wen-Zhen Wang.' 'Chen-Yu Yeh.' data_ic10166 _database_code_depnum_ccdc_archive 'CCDC 633377' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H7 N5' _chemical_formula_weight 173.19 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' _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 11.9865(7) _cell_length_b 3.7315(2) _cell_length_c 17.5501(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 784.97(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1276 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 21.38 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9074 _exptl_absorpt_correction_T_max 0.9980 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 6426 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.49 _reflns_number_total 1798 _reflns_number_gt 1551 _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^)+(0.0461P)^2^+0.1422P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.005(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 3(3) _refine_ls_number_reflns 1798 _refine_ls_number_parameters 119 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1266 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 N1 N 0.35449(18) -0.0611(7) 0.17002(11) 0.0395(6) Uani 1 1 d . . . N2 N 0.29092(15) -0.2349(6) 0.05332(12) 0.0358(5) Uani 1 1 d . . . H2A H 0.2264 -0.2142 0.0743 0.043 Uiso 1 1 calc R . . N3 N 0.38592(17) -0.4561(6) -0.05365(11) 0.0366(5) Uani 1 1 d . . . N4 N 0.56886(17) 0.0555(7) 0.11404(13) 0.0391(6) Uani 1 1 d . . . N5 N 0.18143(19) -0.5522(8) -0.12590(13) 0.0462(6) Uani 1 1 d . . . C1 C 0.4386(2) 0.0576(9) 0.21380(16) 0.0452(8) Uani 1 1 d . . . H1A H 0.4244 0.1023 0.2650 0.054 Uiso 1 1 calc R . . C2 C 0.5434(2) 0.1159(9) 0.18697(15) 0.0420(7) Uani 1 1 d . . . H2B H 0.5983 0.1992 0.2200 0.050 Uiso 1 1 calc R . . C3 C 0.4878(2) -0.0649(7) 0.06967(15) 0.0357(6) Uani 1 1 d . . . H3A H 0.5030 -0.1108 0.0186 0.043 Uiso 1 1 calc R . . C4 C 0.3802(2) -0.1249(7) 0.09705(12) 0.0305(5) Uani 1 1 d . . . C5 C 0.29135(19) -0.3733(7) -0.01938(13) 0.0306(6) Uani 1 1 d . . . C6 C 0.1879(2) -0.4246(8) -0.05654(16) 0.0388(6) Uani 1 1 d . . . H6A H 0.1225 -0.3659 -0.0309 0.047 Uiso 1 1 calc R . . C7 C 0.2778(2) -0.6307(9) -0.16082(15) 0.0463(8) Uani 1 1 d . . . H7A H 0.2765 -0.7174 -0.2105 0.056 Uiso 1 1 calc R . . C8 C 0.3774(2) -0.5858(9) -0.12499(16) 0.0436(7) Uani 1 1 d . . . H8A H 0.4424 -0.6472 -0.1509 0.052 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 N1 0.0298(11) 0.0616(16) 0.0272(13) -0.0026(11) 0.0017(9) 0.0021(11) N2 0.0203(9) 0.0574(14) 0.0297(10) -0.0048(10) 0.0043(8) -0.0015(9) N3 0.0306(11) 0.0462(14) 0.0331(12) -0.0056(11) 0.0022(9) 0.0008(10) N4 0.0260(11) 0.0527(14) 0.0388(14) -0.0065(12) -0.0013(10) 0.0003(10) N5 0.0375(14) 0.0623(16) 0.0386(14) -0.0109(13) -0.0042(10) -0.0074(12) C1 0.0388(15) 0.070(2) 0.0268(13) -0.0126(15) 0.0006(11) 0.0045(14) C2 0.0346(14) 0.0586(18) 0.0328(15) -0.0093(13) -0.0097(12) -0.0026(13) C3 0.0291(13) 0.0481(16) 0.0298(13) -0.0038(12) 0.0028(10) -0.0029(11) C4 0.0279(12) 0.0384(13) 0.0253(13) -0.0008(10) 0.0014(10) 0.0041(10) C5 0.0290(13) 0.0386(14) 0.0243(12) -0.0011(11) 0.0016(9) -0.0018(10) C6 0.0290(13) 0.0491(17) 0.0384(14) -0.0039(13) 0.0009(11) -0.0012(12) C7 0.0479(18) 0.060(2) 0.0310(16) -0.0109(14) 0.0007(12) -0.0046(15) C8 0.0377(15) 0.0598(17) 0.0332(15) -0.0085(14) 0.0041(12) 0.0013(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C4 1.339(3) . ? N1 C1 1.342(4) . ? N2 C5 1.376(3) . ? N2 C4 1.380(3) . ? N3 C5 1.320(3) . ? N3 C8 1.346(3) . ? N4 C3 1.324(3) . ? N4 C2 1.335(3) . ? N5 C6 1.309(3) . ? N5 C7 1.340(4) . ? C1 C2 1.359(4) . ? C3 C4 1.394(3) . ? C5 C6 1.414(3) . ? C7 C8 1.360(4) . ? 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 C4 N1 C1 115.7(2) . . ? C5 N2 C4 128.63(19) . . ? C5 N3 C8 116.3(2) . . ? C3 N4 C2 117.0(2) . . ? C6 N5 C7 117.0(2) . . ? N1 C1 C2 123.3(3) . . ? N4 C2 C1 121.1(2) . . ? N4 C3 C4 122.0(2) . . ? N1 C4 N2 114.0(2) . . ? N1 C4 C3 121.0(2) . . ? N2 C4 C3 125.0(2) . . ? N3 C5 N2 120.9(2) . . ? N3 C5 C6 120.8(2) . . ? N2 C5 C6 118.4(2) . . ? N5 C6 C5 122.0(2) . . ? N5 C7 C8 121.2(3) . . ? N3 C8 C7 122.7(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.188 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.041 data_i6511 _database_code_depnum_ccdc_archive 'CCDC 633378' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H22 Cl2 Cu N10 O12' _chemical_formula_weight 680.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.1795(4) _cell_length_b 10.8102(3) _cell_length_c 15.3382(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2516.90(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3900 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 23.37 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 1.163 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8179 _exptl_absorpt_correction_T_max 0.8925 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2216 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2216 _reflns_number_gt 1768 _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^)+(0.0421P)^2^+3.1038P] 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 2216 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Cu Cu 0.0000 -0.5000 0.0000 0.02712(16) Uani 1 2 d S . . O1 O -0.01516(16) -0.2937(2) -0.04673(14) 0.0510(6) Uani 1 1 d . . . H1B H -0.0038 -0.2671 -0.0948 0.076 Uiso 1 1 d R . . H1A H -0.0088 -0.2475 -0.0052 0.076 Uiso 1 1 d R . . N1 N -0.00490(13) -0.4449(2) 0.12546(14) 0.0280(5) Uani 1 1 d . . . N2 N 0.00056(17) -0.3442(3) 0.29245(16) 0.0442(7) Uani 1 1 d . . . N3 N -0.14047(14) -0.3435(2) 0.10360(14) 0.0325(5) Uani 1 1 d . . . H3 H -0.1621 -0.2701 0.1062 0.039 Uiso 1 1 calc R . . N4 N 0.13395(16) -0.4860(2) -0.00816(13) 0.0281(5) Uani 1 1 d . . . N5 N 0.31681(18) -0.4938(2) 0.00414(17) 0.0437(7) Uani 1 1 d . . . C1 C -0.06777(17) -0.3693(2) 0.15402(17) 0.0291(6) Uani 1 1 d . . . C2 C -0.0628(2) -0.3172(3) 0.23765(18) 0.0379(7) Uani 1 1 d . . . H2 H -0.1060 -0.2614 0.2548 0.045 Uiso 1 1 calc R . . C3 C 0.0607(2) -0.4268(3) 0.26489(19) 0.0428(7) Uani 1 1 d . . . H3A H 0.1052 -0.4513 0.3028 0.051 Uiso 1 1 calc R . . C4 C 0.05843(19) -0.4756(3) 0.18336(18) 0.0352(7) Uani 1 1 d . . . H4 H 0.1017 -0.5318 0.1669 0.042 Uiso 1 1 calc R . . C5 C 0.18097(18) -0.5721(3) -0.04910(16) 0.0292(6) Uani 1 1 d . . . C6 C 0.27258(19) -0.5774(3) -0.03955(18) 0.0374(7) Uani 1 1 d . . . H6 H 0.3031 -0.6425 -0.0651 0.045 Uiso 1 1 calc R . . C7 C 0.2698(2) -0.4008(3) 0.03932(19) 0.0415(7) Uani 1 1 d . . . H7 H 0.2992 -0.3372 0.0680 0.050 Uiso 1 1 calc R . . C8 C 0.18074(19) -0.3978(3) 0.03391(18) 0.0349(6) Uani 1 1 d . . . H8 H 0.1507 -0.3327 0.0601 0.042 Uiso 1 1 calc R . . Cl Cl -0.29244(5) -0.11763(7) 0.25575(5) 0.0420(2) Uani 1 1 d . . . O11 O -0.2708(2) -0.1750(3) 0.17591(18) 0.0991(12) Uani 1 1 d . . . O12 O -0.2443(2) -0.1717(3) 0.32530(16) 0.0753(8) Uani 1 1 d . . . O13 O -0.2704(2) 0.0099(2) 0.25149(19) 0.0769(9) Uani 1 1 d . . . O14 O -0.38410(19) -0.1239(3) 0.2690(2) 0.1014(11) Uani 1 1 d . . . O21 O 0.4860(2) -0.6051(3) 0.0705(2) 0.0926(10) Uani 1 1 d . . . H21A H 0.4502 -0.5566 0.0279 0.139 Uiso 1 1 d R . . H21B H 0.4641 -0.6135 0.1176 0.139 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.0246(3) 0.0369(3) 0.0198(2) -0.00537(18) 0.00197(18) 0.00175(19) O1 0.0830(17) 0.0394(12) 0.0305(11) 0.0066(10) 0.0082(11) 0.0009(11) N1 0.0297(12) 0.0338(12) 0.0206(11) -0.0009(9) 0.0025(9) -0.0012(10) N2 0.0467(16) 0.0581(17) 0.0278(13) -0.0123(12) 0.0015(11) -0.0112(13) N3 0.0338(13) 0.0306(12) 0.0330(12) -0.0049(10) 0.0014(10) 0.0055(10) N4 0.0269(12) 0.0332(12) 0.0243(11) -0.0014(9) 0.0027(9) -0.0010(10) N5 0.0298(14) 0.0574(18) 0.0438(16) -0.0007(13) -0.0026(11) -0.0029(12) C1 0.0303(14) 0.0323(14) 0.0248(13) -0.0020(11) 0.0050(11) -0.0043(11) C2 0.0411(17) 0.0426(17) 0.0299(15) -0.0095(13) 0.0068(13) -0.0029(13) C3 0.0379(17) 0.061(2) 0.0292(16) -0.0008(14) -0.0037(13) -0.0030(15) C4 0.0319(15) 0.0454(16) 0.0282(14) 0.0001(12) 0.0000(12) 0.0005(13) C5 0.0301(15) 0.0346(15) 0.0229(13) 0.0039(11) 0.0037(11) -0.0008(12) C6 0.0330(16) 0.0446(17) 0.0347(15) 0.0024(14) 0.0034(13) 0.0052(14) C7 0.0367(17) 0.0479(18) 0.0397(16) -0.0047(14) -0.0032(13) -0.0087(15) C8 0.0380(16) 0.0376(16) 0.0291(14) -0.0035(12) 0.0021(12) -0.0028(13) Cl 0.0389(4) 0.0446(4) 0.0425(4) -0.0032(3) 0.0017(3) 0.0093(3) O11 0.125(3) 0.118(3) 0.0547(16) -0.0262(18) -0.0012(17) 0.067(2) O12 0.097(2) 0.0755(18) 0.0537(15) 0.0180(14) -0.0025(15) 0.0294(16) O13 0.085(2) 0.0551(16) 0.090(2) 0.0129(15) -0.0194(17) -0.0029(14) O14 0.0445(16) 0.115(3) 0.144(3) -0.028(2) 0.0128(18) -0.0114(17) O21 0.126(3) 0.079(2) 0.073(2) -0.0198(18) -0.0117(18) 0.0124(19) _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 Cu N1 2.016(2) . ? Cu N1 2.016(2) 5_545 ? Cu N4 2.043(2) . ? Cu N4 2.043(2) 5_545 ? Cu O1 2.354(2) . ? Cu O1 2.354(2) 5_545 ? N1 C1 1.330(3) . ? N1 C4 1.350(3) . ? N2 C2 1.310(4) . ? N2 C3 1.345(4) . ? N3 C1 1.376(3) . ? N3 C5 1.381(3) 5_545 ? N4 C5 1.331(3) . ? N4 C8 1.353(4) . ? N5 C6 1.310(4) . ? N5 C7 1.345(4) . ? C1 C2 1.403(4) . ? C3 C4 1.358(4) . ? C5 N3 1.381(3) 5_545 ? C5 C6 1.399(4) . ? C7 C8 1.355(4) . ? Cl O14 1.408(3) . ? Cl O11 1.411(3) . ? Cl O12 1.419(3) . ? Cl O13 1.420(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu N1 180.00(4) . 5_545 ? N1 Cu N4 94.21(8) . . ? N1 Cu N4 85.79(8) 5_545 . ? N1 Cu N4 85.79(8) . 5_545 ? N1 Cu N4 94.21(8) 5_545 5_545 ? N4 Cu N4 180.0 . 5_545 ? N1 Cu O1 90.40(9) . . ? N1 Cu O1 89.60(9) 5_545 . ? N4 Cu O1 90.49(8) . . ? N4 Cu O1 89.51(8) 5_545 . ? N1 Cu O1 89.60(9) . 5_545 ? N1 Cu O1 90.40(9) 5_545 5_545 ? N4 Cu O1 89.51(8) . 5_545 ? N4 Cu O1 90.49(8) 5_545 5_545 ? O1 Cu O1 180.00(10) . 5_545 ? C1 N1 C4 116.4(2) . . ? C1 N1 Cu 121.48(18) . . ? C4 N1 Cu 121.93(18) . . ? C2 N2 C3 116.4(3) . . ? C1 N3 C5 124.3(2) . 5_545 ? C5 N4 C8 115.9(2) . . ? C5 N4 Cu 120.74(18) . . ? C8 N4 Cu 123.06(18) . . ? C6 N5 C7 116.7(3) . . ? N1 C1 N3 121.0(2) . . ? N1 C1 C2 120.6(3) . . ? N3 C1 C2 118.4(2) . . ? N2 C2 C1 122.5(3) . . ? N2 C3 C4 122.0(3) . . ? N1 C4 C3 121.9(3) . . ? N4 C5 N3 120.6(2) . 5_545 ? N4 C5 C6 120.8(3) . . ? N3 C5 C6 118.6(2) 5_545 . ? N5 C6 C5 122.3(3) . . ? N5 C7 C8 121.5(3) . . ? N4 C8 C7 122.4(3) . . ? O14 Cl O11 109.6(2) . . ? O14 Cl O12 112.3(2) . . ? O11 Cl O12 110.58(17) . . ? O14 Cl O13 106.6(2) . . ? O11 Cl O13 109.4(2) . . ? O12 Cl O13 108.28(18) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.395 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.061 # Attachment 'cif_comp_3.cif' data_ic11589 _database_code_depnum_ccdc_archive 'CCDC 633379' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H14 Co N12 S2' _chemical_formula_weight 521.46 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' S S 0.1246 0.1234 '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(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 9.2206(2) _cell_length_b 7.7428(2) _cell_length_c 14.8613(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.7248(12) _cell_angle_gamma 90.00 _cell_volume 1058.76(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 530 _exptl_absorpt_coefficient_mu 1.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.829 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 13071 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2422 _reflns_number_gt 1850 _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^)+(0.0881P)^2^+7.5610P] 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 2422 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2518 _refine_ls_wR_factor_gt 0.2430 _refine_ls_goodness_of_fit_ref 1.254 _refine_ls_restrained_S_all 1.254 _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 Co Co 0.0000 0.0000 0.0000 0.0217(4) Uani 1 2 d S . . S1 S -0.19516(19) -0.4862(2) -0.16500(12) 0.0340(5) Uani 1 1 d . . . N1 N -0.0673(6) -0.1672(7) 0.1113(3) 0.0253(11) Uani 1 1 d . . . N2 N -0.0235(6) -0.2168(8) 0.3543(4) 0.0301(12) Uani 1 1 d . . . H2A H 0.0546 -0.1519 0.3623 0.036 Uiso 1 1 calc R . . N3 N -0.1670(7) -0.3750(8) 0.2479(4) 0.0348(13) Uani 1 1 d . . . N4 N 0.0031(6) -0.2655(8) 0.5070(4) 0.0305(12) Uani 1 1 d . . . N5 N -0.2787(5) -0.3978(7) 0.5089(3) 0.0243(11) Uani 1 1 d . . . N6 N -0.0646(6) -0.1842(7) -0.0956(3) 0.0267(11) Uani 1 1 d . . . C1 C -0.1606(8) -0.2954(10) 0.0930(5) 0.0346(15) Uani 1 1 d . . . H1A H -0.1936 -0.3178 0.0322 0.042 Uiso 1 1 calc R . . C2 C -0.2097(8) -0.3954(10) 0.1605(5) 0.0394(17) Uani 1 1 d . . . H2B H -0.2777 -0.4843 0.1446 0.047 Uiso 1 1 calc R . . C3 C -0.0736(7) -0.2470(8) 0.2655(4) 0.0265(13) Uani 1 1 d . . . C4 C -0.0239(7) -0.1427(8) 0.1971(4) 0.0263(13) Uani 1 1 d . . . H4A H 0.0426 -0.0521 0.2125 0.032 Uiso 1 1 calc R . . C5 C -0.0825(7) -0.2775(8) 0.4316(4) 0.0270(13) Uani 1 1 d . . . C6 C -0.2256(7) -0.3395(8) 0.4329(4) 0.0263(13) Uani 1 1 d . . . H6A H -0.2860 -0.3400 0.3786 0.032 Uiso 1 1 calc R . . C7 C -0.1906(7) -0.3927(9) 0.5842(4) 0.0299(14) Uani 1 1 d . . . H7A H -0.2234 -0.4362 0.6391 0.036 Uiso 1 1 calc R . . C8 C -0.0513(7) -0.3238(9) 0.5825(5) 0.0325(15) Uani 1 1 d . . . H8A H 0.0076 -0.3180 0.6373 0.039 Uiso 1 1 calc R . . C9 C -0.1171(7) -0.3084(8) -0.1262(4) 0.0251(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0213(6) 0.0226(6) 0.0218(6) -0.0001(4) 0.0055(4) 0.0001(4) S1 0.0309(9) 0.0276(8) 0.0430(10) -0.0076(7) 0.0000(7) 0.0004(6) N1 0.025(3) 0.026(3) 0.026(3) 0.002(2) 0.004(2) 0.002(2) N2 0.024(3) 0.037(3) 0.030(3) 0.006(2) 0.004(2) -0.007(2) N3 0.041(3) 0.033(3) 0.031(3) 0.002(2) 0.009(2) -0.010(3) N4 0.027(3) 0.032(3) 0.032(3) 0.001(2) 0.004(2) -0.001(2) N5 0.023(3) 0.025(3) 0.026(2) 0.001(2) 0.011(2) -0.001(2) N6 0.026(3) 0.028(3) 0.027(3) -0.001(2) 0.010(2) -0.003(2) C1 0.035(4) 0.041(4) 0.028(3) -0.002(3) 0.003(3) -0.014(3) C2 0.041(4) 0.043(4) 0.034(4) -0.004(3) 0.007(3) -0.019(3) C3 0.023(3) 0.025(3) 0.032(3) 0.003(3) 0.009(2) 0.001(2) C4 0.025(3) 0.027(3) 0.028(3) 0.004(3) 0.007(2) -0.002(2) C5 0.025(3) 0.029(3) 0.027(3) 0.003(3) 0.004(2) 0.005(3) C6 0.024(3) 0.029(3) 0.026(3) 0.001(3) 0.006(2) -0.004(2) C7 0.031(3) 0.033(3) 0.026(3) 0.002(3) 0.010(3) 0.000(3) C8 0.030(3) 0.037(4) 0.031(3) 0.001(3) 0.002(3) 0.001(3) C9 0.024(3) 0.029(3) 0.023(3) 0.001(3) 0.008(2) 0.005(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 Co N6 2.073(5) 3 ? Co N6 2.073(5) . ? Co N5 2.184(5) 2_455 ? Co N5 2.184(5) 4_655 ? Co N1 2.220(5) . ? Co N1 2.220(5) 3 ? S1 C9 1.641(7) . ? N1 C4 1.326(8) . ? N1 C1 1.330(9) . ? N2 C5 1.385(8) . ? N2 C3 1.388(8) . ? N3 C3 1.328(8) . ? N3 C2 1.342(9) . ? N4 C5 1.331(8) . ? N4 C8 1.338(9) . ? N5 C6 1.338(8) . ? N5 C7 1.341(8) . ? N5 Co 2.184(5) 2_445 ? N6 C9 1.156(8) . ? C1 C2 1.367(10) . ? C3 C4 1.399(9) . ? C5 C6 1.406(9) . ? C7 C8 1.393(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Co N6 180.0(3) 3 . ? N6 Co N5 91.0(2) 3 2_455 ? N6 Co N5 89.0(2) . 2_455 ? N6 Co N5 89.0(2) 3 4_655 ? N6 Co N5 91.0(2) . 4_655 ? N5 Co N5 180.00(10) 2_455 4_655 ? N6 Co N1 88.4(2) 3 . ? N6 Co N1 91.6(2) . . ? N5 Co N1 87.20(19) 2_455 . ? N5 Co N1 92.80(19) 4_655 . ? N6 Co N1 91.6(2) 3 3 ? N6 Co N1 88.4(2) . 3 ? N5 Co N1 92.80(19) 2_455 3 ? N5 Co N1 87.20(19) 4_655 3 ? N1 Co N1 180.0(4) . 3 ? C4 N1 C1 117.0(6) . . ? C4 N1 Co 123.5(4) . . ? C1 N1 Co 119.5(4) . . ? C5 N2 C3 127.3(6) . . ? C3 N3 C2 115.1(6) . . ? C5 N4 C8 116.6(6) . . ? C6 N5 C7 117.4(5) . . ? C6 N5 Co 117.6(4) . 2_445 ? C7 N5 Co 125.0(4) . 2_445 ? C9 N6 Co 159.4(5) . . ? N1 C1 C2 120.9(6) . . ? N3 C2 C1 123.6(7) . . ? N3 C3 N2 119.0(6) . . ? N3 C3 C4 121.8(6) . . ? N2 C3 C4 119.2(6) . . ? N1 C4 C3 121.6(6) . . ? N4 C5 N2 115.5(6) . . ? N4 C5 C6 121.2(6) . . ? N2 C5 C6 123.2(6) . . ? N5 C6 C5 121.5(6) . . ? N5 C7 C8 120.4(6) . . ? N4 C8 C7 122.8(6) . . ? N6 C9 S1 177.2(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.961 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.173 # Attachment 'cif_comp_4.cif' data_ic10670 _database_code_depnum_ccdc_archive 'CCDC 633380' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.25 H32 Cl2.50 N20 Ni3 O0.75' _chemical_formula_weight 1012.56 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 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 19.2247(3) _cell_length_b 10.3082(2) _cell_length_c 21.5836(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.0440(13) _cell_angle_gamma 90.00 _cell_volume 4066.90(13) _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 dark-purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.598 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.927 _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 42288 _diffrn_reflns_av_R_equivalents 0.0870 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9312 _reflns_number_gt 5403 _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^)+(0.0627P)^2^+2.5164P] 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 9312 _refine_ls_number_parameters 543 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1128 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 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 0.39625(3) 0.22965(5) 0.29296(2) 0.02732(15) Uani 1 1 d . . . Ni2 Ni 0.5000 0.23362(7) 0.2500 0.02460(18) Uani 1 2 d S . . Cl1 Cl 0.29640(6) 0.22476(11) 0.32970(5) 0.0382(3) Uani 1 1 d . . . N1 N 0.34197(19) 0.2972(3) 0.19982(16) 0.0289(8) Uani 1 1 d . . . N2 N 0.45342(18) 0.3633(3) 0.18988(15) 0.0261(8) Uani 1 1 d . . . N3 N 0.56434(19) 0.4160(3) 0.17453(15) 0.0281(8) Uani 1 1 d . . . N4 N 0.2691(2) 0.3695(4) 0.07125(17) 0.0383(9) Uani 1 1 d . . . N5 N 0.5103(2) 0.6592(3) 0.12458(17) 0.0368(9) Uani 1 1 d . . . N6 N 0.38679(19) 0.0406(3) 0.25516(16) 0.0289(8) Uani 1 1 d . . . N7 N 0.45505(18) 0.1042(3) 0.18908(15) 0.0256(8) Uani 1 1 d . . . N8 N 0.5248(2) 0.1634(3) 0.12323(16) 0.0295(8) Uani 1 1 d . . . N9 N 0.3733(2) -0.2100(3) 0.20376(18) 0.0366(9) Uani 1 1 d . . . N10 N 0.4134(2) 0.0906(4) 0.01120(17) 0.0423(10) Uani 1 1 d . . . C1 C 0.2692(2) 0.2780(4) 0.1721(2) 0.0333(10) Uani 1 1 d . . . H1A H 0.2420 0.2386 0.1971 0.040 Uiso 1 1 calc R . . C2 C 0.2336(3) 0.3138(4) 0.1090(2) 0.0375(11) Uani 1 1 d . . . H2A H 0.1825 0.2988 0.0915 0.045 Uiso 1 1 calc R . . C3 C 0.3398(2) 0.3886(4) 0.0976(2) 0.0333(10) Uani 1 1 d . . . H3A H 0.3663 0.4266 0.0716 0.040 Uiso 1 1 calc R . . C4 C 0.3785(2) 0.3547(4) 0.16306(19) 0.0288(9) Uani 1 1 d . . . C5 C 0.4946(2) 0.4509(4) 0.16886(19) 0.0276(9) Uani 1 1 d . . . C6 C 0.4703(3) 0.5757(4) 0.1460(2) 0.0327(10) Uani 1 1 d . . . H6A H 0.4229 0.6018 0.1458 0.039 Uiso 1 1 calc R . . C7 C 0.5780(3) 0.6198(4) 0.1279(2) 0.0384(11) Uani 1 1 d . . . H7A H 0.6079 0.6751 0.1117 0.046 Uiso 1 1 calc R . . C8 C 0.6052(2) 0.5021(4) 0.15408(19) 0.0317(10) Uani 1 1 d . . . H8A H 0.6544 0.4806 0.1579 0.038 Uiso 1 1 calc R . . C9 C 0.3537(2) -0.0538(4) 0.2777(2) 0.0330(10) Uani 1 1 d . . . H9A H 0.3352 -0.0357 0.3128 0.040 Uiso 1 1 calc R . . C10 C 0.3457(2) -0.1764(4) 0.2516(2) 0.0355(11) Uani 1 1 d . . . H10A H 0.3198 -0.2395 0.2679 0.043 Uiso 1 1 calc R . . C11 C 0.4077(2) -0.1179(4) 0.1825(2) 0.0333(10) Uani 1 1 d . . . H11A H 0.4284 -0.1384 0.1491 0.040 Uiso 1 1 calc R . . C12 C 0.4151(2) 0.0097(4) 0.20727(19) 0.0280(9) Uani 1 1 d . . . C13 C 0.4624(2) 0.1088(4) 0.1275(2) 0.0283(9) Uani 1 1 d . . . C14 C 0.4073(3) 0.0717(4) 0.0704(2) 0.0358(11) Uani 1 1 d . . . H14A H 0.3643 0.0317 0.0742 0.043 Uiso 1 1 calc R . . C15 C 0.4755(3) 0.1458(4) 0.0082(2) 0.0382(11) Uani 1 1 d . . . H15A H 0.4815 0.1606 -0.0333 0.046 Uiso 1 1 calc R . . C16 C 0.5303(3) 0.1815(4) 0.0628(2) 0.0357(11) Uani 1 1 d . . . H16A H 0.5734 0.2199 0.0583 0.043 Uiso 1 1 calc R . . Ni3 Ni -0.01476(3) 0.70549(5) 0.13361(2) 0.02321(14) Uani 1 1 d . . . Ni4 Ni 0.0000 0.70347(7) 0.2500 0.02077(17) Uani 1 2 d S . . Cl2 Cl -0.02882(6) 0.70887(10) 0.02368(5) 0.0330(3) Uani 1 1 d . . . N11 N 0.02915(18) 0.8936(3) 0.15525(15) 0.0255(8) Uani 1 1 d . . . N12 N 0.07232(18) 0.8335(3) 0.26405(14) 0.0233(7) Uani 1 1 d . . . N13 N 0.11946(18) 0.7680(3) 0.37193(15) 0.0246(7) Uani 1 1 d . . . N14 N 0.0964(2) 1.1366(3) 0.18449(17) 0.0403(10) Uani 1 1 d . . . N15 N 0.2618(2) 0.8259(4) 0.37208(17) 0.0389(9) Uani 1 1 d . . . N16 N -0.05359(18) 0.5176(3) 0.13903(14) 0.0251(8) Uani 1 1 d . . . N17 N -0.07207(17) 0.5730(3) 0.23723(14) 0.0227(7) Uani 1 1 d . . . N18 N -0.09206(18) 0.6357(3) 0.33315(14) 0.0240(7) Uani 1 1 d . . . N19 N -0.1056(2) 0.2669(3) 0.14578(18) 0.0399(10) Uani 1 1 d . . . N20 N -0.23875(19) 0.5584(3) 0.28563(17) 0.0324(8) Uani 1 1 d . . . C17 C 0.0223(3) 0.9851(4) 0.1094(2) 0.0354(11) Uani 1 1 d . . . H17A H -0.0070 0.9673 0.0659 0.042 Uiso 1 1 calc R . . C18 C 0.0565(3) 1.1035(4) 0.1234(2) 0.0451(13) Uani 1 1 d . . . H18A H 0.0518 1.1638 0.0890 0.054 Uiso 1 1 calc R . . C19 C 0.1009(2) 1.0492(4) 0.2302(2) 0.0309(10) Uani 1 1 d . . . H19A H 0.1269 1.0709 0.2740 0.037 Uiso 1 1 calc R . . C20 C 0.0689(2) 0.9247(4) 0.21697(18) 0.0245(9) Uani 1 1 d . . . C21 C 0.1318(2) 0.8228(4) 0.31947(18) 0.0227(9) Uani 1 1 d . . . C22 C 0.2037(2) 0.8529(4) 0.3214(2) 0.0319(10) Uani 1 1 d . . . H22A H 0.2111 0.8948 0.2848 0.038 Uiso 1 1 calc R . . C23 C 0.2481(3) 0.7695(5) 0.4231(2) 0.0381(11) Uani 1 1 d . . . H23A H 0.2880 0.7479 0.4604 0.046 Uiso 1 1 calc R . . C24 C 0.1779(2) 0.7418(4) 0.42327(19) 0.0314(10) Uani 1 1 d . . . H24A H 0.1709 0.7031 0.4608 0.038 Uiso 1 1 calc R . . C25 C -0.0563(2) 0.4281(4) 0.09284(19) 0.0327(10) Uani 1 1 d . . . H25A H -0.0392 0.4504 0.0574 0.039 Uiso 1 1 calc R . . C26 C -0.0828(3) 0.3067(4) 0.0958(2) 0.0395(12) Uani 1 1 d . . . H26A H -0.0854 0.2477 0.0613 0.047 Uiso 1 1 calc R . . C27 C -0.1028(2) 0.3539(4) 0.1915(2) 0.0319(10) Uani 1 1 d . . . H27A H -0.1182 0.3290 0.2276 0.038 Uiso 1 1 calc R . . C28 C -0.0782(2) 0.4814(4) 0.18900(17) 0.0234(9) Uani 1 1 d . . . C29 C -0.1186(2) 0.5772(4) 0.27428(18) 0.0250(9) Uani 1 1 d . . . C30 C -0.1924(2) 0.5372(4) 0.2524(2) 0.0301(10) Uani 1 1 d . . . H30A H -0.2096 0.4930 0.2119 0.036 Uiso 1 1 calc R . . C31 C -0.2115(2) 0.6189(4) 0.3437(2) 0.0323(10) Uani 1 1 d . . . H31A H -0.2431 0.6367 0.3688 0.039 Uiso 1 1 calc R . . C32 C -0.1400(2) 0.6549(4) 0.36713(19) 0.0275(9) Uani 1 1 d . . . H32A H -0.1230 0.6950 0.4088 0.033 Uiso 1 1 calc R . . O1 O 0.2526(3) 0.8331(6) 0.0332(3) 0.1125(19) Uiso 0.75 1 d PD A 1 C33 C 0.2944(6) 0.6610(8) -0.0115(5) 0.092(3) Uiso 0.75 1 d PD A 1 H33A H 0.3260 0.6372 -0.0377 0.138 Uiso 0.75 1 calc PR A 1 H33B H 0.2498 0.6082 -0.0248 0.138 Uiso 0.75 1 calc PR A 1 H33C H 0.3205 0.6455 0.0347 0.138 Uiso 0.75 1 calc PR A 1 C34 C 0.2739(6) 0.8058(8) -0.0219(4) 0.093(3) Uiso 0.75 1 d PD A 1 H34A H 0.3164 0.8592 -0.0229 0.111 Uiso 0.75 1 calc PR A 1 H34B H 0.2332 0.8197 -0.0627 0.111 Uiso 0.75 1 calc PR A 1 C35 C 0.2113(6) 0.9408(10) 0.0037(5) 0.084(4) Uiso 0.75 1 d PD A 1 H35A H 0.1767 0.9164 -0.0392 0.101 Uiso 0.75 1 calc PR A 1 H35B H 0.2437 1.0103 -0.0030 0.101 Uiso 0.75 1 calc PR A 1 C36 C 0.1696(8) 0.9873(15) 0.0489(7) 0.170(7) Uiso 0.75 1 d PD A 1 H36B H 0.1542 1.0774 0.0385 0.256 Uiso 0.75 1 calc PR A 1 H36C H 0.2014 0.9819 0.0942 0.256 Uiso 0.75 1 calc PR A 1 H36D H 0.1264 0.9326 0.0433 0.256 Uiso 0.75 1 calc PR A 1 C37 C 0.2526(3) 0.8331(6) 0.0332(3) 0.1125(19) Uiso 0.25 1 d PD B 2 H37A H 0.2147 0.7660 0.0296 0.135 Uiso 0.25 1 calc PR B 2 H37B H 0.2765 0.8422 0.0807 0.135 Uiso 0.25 1 calc PR B 2 Cl3 Cl 0.3154(4) 0.7411(7) 0.0157(4) 0.083(2) Uiso 0.25 1 d PD B 2 Cl4 Cl 0.2000(7) 0.9619(10) 0.0213(7) 0.123(4) Uiso 0.25 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 0.0261(3) 0.0244(3) 0.0329(3) -0.0017(2) 0.0112(2) -0.0004(2) Ni2 0.0254(4) 0.0194(4) 0.0290(4) 0.000 0.0084(3) 0.000 Cl1 0.0345(6) 0.0391(7) 0.0454(6) -0.0029(5) 0.0187(5) -0.0008(5) N1 0.027(2) 0.0221(19) 0.0365(19) -0.0041(15) 0.0082(16) 0.0002(15) N2 0.026(2) 0.0211(18) 0.0304(18) 0.0008(14) 0.0067(15) 0.0000(15) N3 0.028(2) 0.0272(19) 0.0284(18) -0.0005(15) 0.0069(15) -0.0050(16) N4 0.034(2) 0.037(2) 0.037(2) -0.0032(17) 0.0014(18) 0.0019(18) N5 0.041(2) 0.026(2) 0.043(2) 0.0048(17) 0.0116(18) 0.0003(18) N6 0.026(2) 0.029(2) 0.0334(19) -0.0002(16) 0.0123(16) -0.0019(16) N7 0.0248(19) 0.0243(19) 0.0280(18) 0.0006(14) 0.0087(15) 0.0000(15) N8 0.036(2) 0.0238(19) 0.0301(19) 0.0017(15) 0.0121(16) 0.0031(16) N9 0.039(2) 0.024(2) 0.050(2) -0.0034(17) 0.0188(19) -0.0036(17) N10 0.044(3) 0.044(2) 0.036(2) -0.0005(18) 0.0072(19) 0.006(2) C1 0.029(3) 0.026(2) 0.044(3) -0.006(2) 0.012(2) 0.000(2) C2 0.027(3) 0.040(3) 0.042(3) -0.008(2) 0.007(2) -0.002(2) C3 0.034(3) 0.032(3) 0.032(2) -0.0033(19) 0.008(2) 0.001(2) C4 0.035(3) 0.018(2) 0.034(2) -0.0037(18) 0.011(2) 0.0005(19) C5 0.028(2) 0.027(2) 0.028(2) -0.0046(18) 0.0081(18) -0.0006(18) C6 0.036(3) 0.023(2) 0.039(2) 0.0026(19) 0.010(2) 0.002(2) C7 0.041(3) 0.032(3) 0.042(3) 0.007(2) 0.013(2) -0.005(2) C8 0.030(2) 0.030(2) 0.035(2) -0.0001(19) 0.0095(19) -0.003(2) C9 0.027(2) 0.034(3) 0.038(2) 0.004(2) 0.009(2) -0.003(2) C10 0.037(3) 0.028(2) 0.044(3) 0.000(2) 0.016(2) -0.004(2) C11 0.034(3) 0.025(2) 0.044(3) -0.0049(19) 0.016(2) -0.002(2) C12 0.026(2) 0.025(2) 0.032(2) 0.0015(18) 0.0060(19) 0.0004(18) C13 0.031(2) 0.017(2) 0.038(2) 0.0010(17) 0.012(2) 0.0030(18) C14 0.035(3) 0.036(3) 0.033(2) -0.001(2) 0.006(2) 0.002(2) C15 0.049(3) 0.037(3) 0.030(2) 0.001(2) 0.015(2) 0.004(2) C16 0.046(3) 0.028(3) 0.038(3) 0.0054(19) 0.022(2) 0.004(2) Ni3 0.0268(3) 0.0230(3) 0.0205(3) 0.0002(2) 0.0082(2) 0.0016(2) Ni4 0.0232(4) 0.0189(4) 0.0207(3) 0.000 0.0074(3) 0.000 Cl2 0.0414(7) 0.0357(6) 0.0231(5) 0.0016(4) 0.0119(4) 0.0043(5) N11 0.031(2) 0.0237(18) 0.0235(17) 0.0030(14) 0.0101(15) 0.0011(15) N12 0.0275(19) 0.0198(17) 0.0238(17) -0.0021(14) 0.0098(15) -0.0024(15) N13 0.0257(19) 0.0234(18) 0.0243(17) -0.0001(14) 0.0073(14) -0.0034(15) N14 0.059(3) 0.025(2) 0.038(2) 0.0019(17) 0.016(2) -0.0080(19) N15 0.030(2) 0.051(3) 0.035(2) 0.0005(18) 0.0084(17) -0.0054(18) N16 0.027(2) 0.0238(18) 0.0230(17) -0.0012(14) 0.0053(15) 0.0005(15) N17 0.0268(19) 0.0207(18) 0.0221(16) -0.0014(14) 0.0099(15) -0.0011(15) N18 0.029(2) 0.0208(18) 0.0232(17) 0.0013(14) 0.0095(15) -0.0005(15) N19 0.055(3) 0.027(2) 0.041(2) -0.0087(17) 0.019(2) -0.0074(19) N20 0.028(2) 0.028(2) 0.044(2) 0.0036(17) 0.0151(17) -0.0015(16) C17 0.048(3) 0.034(3) 0.026(2) 0.0072(19) 0.014(2) 0.006(2) C18 0.073(4) 0.028(3) 0.035(3) 0.006(2) 0.018(3) -0.009(3) C19 0.043(3) 0.022(2) 0.028(2) 0.0013(18) 0.011(2) -0.002(2) C20 0.028(2) 0.023(2) 0.025(2) 0.0008(17) 0.0106(18) 0.0009(18) C21 0.024(2) 0.020(2) 0.025(2) -0.0032(16) 0.0083(17) -0.0021(17) C22 0.029(2) 0.035(3) 0.032(2) 0.0026(19) 0.010(2) -0.006(2) C23 0.030(3) 0.050(3) 0.030(2) 0.005(2) 0.0044(19) -0.005(2) C24 0.037(3) 0.034(3) 0.021(2) 0.0029(18) 0.0049(19) -0.004(2) C25 0.041(3) 0.031(3) 0.027(2) -0.0046(18) 0.013(2) 0.002(2) C26 0.062(3) 0.027(3) 0.035(2) -0.0111(19) 0.024(2) -0.005(2) C27 0.040(3) 0.025(2) 0.036(2) 0.0007(19) 0.019(2) -0.001(2) C28 0.024(2) 0.022(2) 0.0213(19) 0.0003(16) 0.0032(17) -0.0002(17) C29 0.031(2) 0.017(2) 0.026(2) 0.0044(16) 0.0088(18) 0.0014(17) C30 0.033(3) 0.025(2) 0.031(2) -0.0023(18) 0.009(2) -0.0004(19) C31 0.033(3) 0.031(2) 0.038(2) -0.002(2) 0.017(2) -0.003(2) C32 0.036(3) 0.026(2) 0.025(2) -0.0002(17) 0.0152(19) 0.0015(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.077(3) . ? Ni1 N8 2.084(3) 2_655 ? Ni1 N6 2.099(3) . ? Ni1 N3 2.104(3) 2_655 ? Ni1 Cl1 2.2934(12) . ? Ni1 Ni2 2.4464(5) . ? Ni2 N7 1.885(3) 2_655 ? Ni2 N7 1.885(3) . ? Ni2 N2 1.885(3) 2_655 ? Ni2 N2 1.885(3) . ? Ni2 Ni1 2.4464(5) 2_655 ? N1 C4 1.350(5) . ? N1 C1 1.355(5) . ? N2 C5 1.368(5) . ? N2 C4 1.378(5) . ? N3 C8 1.346(5) . ? N3 C5 1.356(5) . ? N3 Ni1 2.104(3) 2_655 ? N4 C3 1.316(5) . ? N4 C2 1.343(6) . ? N5 C6 1.327(5) . ? N5 C7 1.344(6) . ? N6 C9 1.334(5) . ? N6 C12 1.347(5) . ? N7 C12 1.371(5) . ? N7 C13 1.381(5) . ? N8 C13 1.353(5) . ? N8 C16 1.353(5) . ? N8 Ni1 2.084(3) 2_655 ? N9 C11 1.317(5) . ? N9 C10 1.344(5) . ? N10 C14 1.333(5) . ? N10 C15 1.342(6) . ? C1 C2 1.372(6) . ? C3 C4 1.422(6) . ? C5 C6 1.406(6) . ? C7 C8 1.371(6) . ? C9 C10 1.372(6) . ? C11 C12 1.410(6) . ? C13 C14 1.406(6) . ? C15 C16 1.366(6) . ? Ni3 N13 2.081(3) 2 ? Ni3 N18 2.082(3) 2 ? Ni3 N16 2.092(3) . ? Ni3 N11 2.108(3) . ? Ni3 Cl2 2.3035(10) . ? Ni3 Ni4 2.4393(5) . ? Ni4 N12 1.887(3) . ? Ni4 N12 1.887(3) 2 ? Ni4 N17 1.889(3) 2 ? Ni4 N17 1.889(3) . ? Ni4 Ni3 2.4393(5) 2 ? N11 C17 1.344(5) . ? N11 C20 1.353(5) . ? N12 C20 1.370(5) . ? N12 C21 1.380(5) . ? N13 C24 1.339(5) . ? N13 C21 1.350(5) . ? N13 Ni3 2.081(3) 2 ? N14 C19 1.318(5) . ? N14 C18 1.348(6) . ? N15 C22 1.328(5) . ? N15 C23 1.342(5) . ? N16 C25 1.347(5) . ? N16 C28 1.357(5) . ? N17 C29 1.373(5) . ? N17 C28 1.383(5) . ? N18 C29 1.355(5) . ? N18 C32 1.359(5) . ? N18 Ni3 2.082(3) 2 ? N19 C27 1.321(5) . ? N19 C26 1.348(5) . ? N20 C30 1.324(5) . ? N20 C31 1.351(5) . ? C17 C18 1.375(6) . ? C19 C20 1.414(6) . ? C21 C22 1.404(6) . ? C23 C24 1.379(6) . ? C25 C26 1.361(6) . ? C27 C28 1.404(6) . ? C29 C30 1.411(6) . ? C31 C32 1.360(6) . ? O1 C35 1.397(8) . ? O1 C34 1.401(7) . ? C33 C34 1.543(8) . ? C35 C36 1.519(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N8 164.25(14) . 2_655 ? N1 Ni1 N6 88.74(13) . . ? N8 Ni1 N6 89.15(13) 2_655 . ? N1 Ni1 N3 92.16(13) . 2_655 ? N8 Ni1 N3 85.39(13) 2_655 2_655 ? N6 Ni1 N3 163.01(13) . 2_655 ? N1 Ni1 Cl1 96.81(10) . . ? N8 Ni1 Cl1 98.94(10) 2_655 . ? N6 Ni1 Cl1 97.64(10) . . ? N3 Ni1 Cl1 99.10(10) 2_655 . ? N1 Ni1 Ni2 81.48(10) . . ? N8 Ni1 Ni2 82.77(10) 2_655 . ? N6 Ni1 Ni2 81.43(9) . . ? N3 Ni1 Ni2 81.93(9) 2_655 . ? Cl1 Ni1 Ni2 178.05(4) . . ? N7 Ni2 N7 89.85(19) 2_655 . ? N7 Ni2 N2 90.26(14) 2_655 2_655 ? N7 Ni2 N2 178.77(14) . 2_655 ? N7 Ni2 N2 178.77(14) 2_655 . ? N7 Ni2 N2 90.26(14) . . ? N2 Ni2 N2 89.7(2) 2_655 . ? N7 Ni2 Ni1 88.57(10) 2_655 . ? N7 Ni2 Ni1 90.07(10) . . ? N2 Ni2 Ni1 91.16(10) 2_655 . ? N2 Ni2 Ni1 90.20(10) . . ? N7 Ni2 Ni1 90.07(10) 2_655 2_655 ? N7 Ni2 Ni1 88.57(10) . 2_655 ? N2 Ni2 Ni1 90.20(10) 2_655 2_655 ? N2 Ni2 Ni1 91.16(10) . 2_655 ? Ni1 Ni2 Ni1 178.08(4) . 2_655 ? C4 N1 C1 117.4(4) . . ? C4 N1 Ni1 121.3(3) . . ? C1 N1 Ni1 121.2(3) . . ? C5 N2 C4 122.7(3) . . ? C5 N2 Ni2 119.7(3) . . ? C4 N2 Ni2 117.1(3) . . ? C8 N3 C5 117.1(4) . . ? C8 N3 Ni1 121.6(3) . 2_655 ? C5 N3 Ni1 121.0(3) . 2_655 ? C3 N4 C2 116.9(4) . . ? C6 N5 C7 116.2(4) . . ? C9 N6 C12 117.3(4) . . ? C9 N6 Ni1 122.0(3) . . ? C12 N6 Ni1 120.7(3) . . ? C12 N7 C13 122.3(3) . . ? C12 N7 Ni2 118.7(3) . . ? C13 N7 Ni2 119.1(3) . . ? C13 N8 C16 117.3(4) . . ? C13 N8 Ni1 120.0(3) . 2_655 ? C16 N8 Ni1 122.5(3) . 2_655 ? C11 N9 C10 116.2(4) . . ? C14 N10 C15 116.8(4) . . ? N1 C1 C2 121.8(4) . . ? N4 C2 C1 121.8(4) . . ? N4 C3 C4 123.0(4) . . ? N1 C4 N2 116.6(4) . . ? N1 C4 C3 119.0(4) . . ? N2 C4 C3 124.0(4) . . ? N3 C5 N2 116.9(4) . . ? N3 C5 C6 119.1(4) . . ? N2 C5 C6 123.9(4) . . ? N5 C6 C5 123.4(4) . . ? N5 C7 C8 121.9(4) . . ? N3 C8 C7 122.1(4) . . ? N6 C9 C10 121.9(4) . . ? N9 C10 C9 122.1(4) . . ? N9 C11 C12 122.9(4) . . ? N6 C12 N7 116.6(4) . . ? N6 C12 C11 119.6(4) . . ? N7 C12 C11 123.6(4) . . ? N8 C13 N7 115.9(4) . . ? N8 C13 C14 119.8(4) . . ? N7 C13 C14 124.1(4) . . ? N10 C14 C13 122.3(4) . . ? N10 C15 C16 122.2(4) . . ? N8 C16 C15 121.6(4) . . ? N13 Ni3 N18 163.67(12) 2 2 ? N13 Ni3 N16 86.25(13) 2 . ? N18 Ni3 N16 89.53(13) 2 . ? N13 Ni3 N11 92.38(13) 2 . ? N18 Ni3 N11 87.52(13) 2 . ? N16 Ni3 N11 164.64(12) . . ? N13 Ni3 Cl2 97.66(9) 2 . ? N18 Ni3 Cl2 98.55(9) 2 . ? N16 Ni3 Cl2 98.14(9) . . ? N11 Ni3 Cl2 97.21(9) . . ? N13 Ni3 Ni4 82.17(9) 2 . ? N18 Ni3 Ni4 81.63(8) 2 . ? N16 Ni3 Ni4 82.20(8) . . ? N11 Ni3 Ni4 82.46(8) . . ? Cl2 Ni3 Ni4 179.62(4) . . ? N12 Ni4 N12 89.5(2) . 2 ? N12 Ni4 N17 90.69(14) . 2 ? N12 Ni4 N17 179.19(13) 2 2 ? N12 Ni4 N17 179.19(13) . . ? N12 Ni4 N17 90.69(14) 2 . ? N17 Ni4 N17 89.2(2) 2 . ? N12 Ni4 Ni3 89.06(9) . 2 ? N12 Ni4 Ni3 90.25(9) 2 2 ? N17 Ni4 Ni3 90.55(9) 2 2 ? N17 Ni4 Ni3 90.14(9) . 2 ? N12 Ni4 Ni3 90.25(9) . . ? N12 Ni4 Ni3 89.06(9) 2 . ? N17 Ni4 Ni3 90.14(9) 2 . ? N17 Ni4 Ni3 90.55(9) . . ? Ni3 Ni4 Ni3 179.02(4) 2 . ? C17 N11 C20 117.1(4) . . ? C17 N11 Ni3 122.7(3) . . ? C20 N11 Ni3 120.1(3) . . ? C20 N12 C21 122.3(3) . . ? C20 N12 Ni4 120.3(3) . . ? C21 N12 Ni4 117.0(2) . . ? C24 N13 C21 117.3(3) . . ? C24 N13 Ni3 122.3(3) . 2 ? C21 N13 Ni3 119.9(3) . 2 ? C19 N14 C18 116.4(4) . . ? C22 N15 C23 115.9(4) . . ? C25 N16 C28 117.2(3) . . ? C25 N16 Ni3 121.6(3) . . ? C28 N16 Ni3 121.1(2) . . ? C29 N17 C28 122.8(3) . . ? C29 N17 Ni4 118.2(2) . . ? C28 N17 Ni4 118.9(3) . . ? C29 N18 C32 116.7(3) . . ? C29 N18 Ni3 121.4(3) . 2 ? C32 N18 Ni3 121.7(3) . 2 ? C27 N19 C26 116.3(4) . . ? C30 N20 C31 116.4(4) . . ? N11 C17 C18 122.0(4) . . ? N14 C18 C17 121.9(4) . . ? N14 C19 C20 123.1(4) . . ? N11 C20 N12 116.8(3) . . ? N11 C20 C19 119.4(3) . . ? N12 C20 C19 123.7(3) . . ? N13 C21 N12 116.6(3) . . ? N13 C21 C22 119.6(4) . . ? N12 C21 C22 123.5(3) . . ? N15 C22 C21 123.2(4) . . ? N15 C23 C24 122.2(4) . . ? N13 C24 C23 121.8(4) . . ? N16 C25 C26 121.6(4) . . ? N19 C26 C25 122.4(4) . . ? N19 C27 C28 122.9(4) . . ? N16 C28 N17 116.2(3) . . ? N16 C28 C27 119.5(3) . . ? N17 C28 C27 124.2(3) . . ? N18 C29 N17 115.9(4) . . ? N18 C29 C30 119.4(4) . . ? N17 C29 C30 124.4(3) . . ? N20 C30 C29 123.1(4) . . ? N20 C31 C32 121.9(4) . . ? N18 C32 C31 122.4(4) . . ? C35 O1 C34 92.8(7) . . ? O1 C34 C33 101.5(7) . . ? O1 C35 C36 107.3(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.970 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.101 # Attachment 'cif_comp_6.cif' data_ic11282 _database_code_depnum_ccdc_archive 'CCDC 633381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H29 Cl3 Cr3 N20 O1.50' _chemical_formula_weight 992.11 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' _cell_length_a 13.7908(3) _cell_length_b 10.3096(2) _cell_length_c 14.7425(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.5009(11) _cell_angle_gamma 90.00 _cell_volume 2082.58(7) _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 27.50 _exptl_crystal_description needle _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 0.978 _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 21559 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.0764 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8791 _reflns_number_gt 6379 _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^)+(0.1134P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_number_reflns 8791 _refine_ls_number_parameters 562 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0908 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1788 _refine_ls_wR_factor_gt 0.1604 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 Cr1 Cr -0.10974(6) 0.01869(8) 0.11390(6) 0.0305(2) Uani 1 1 d . . . Cr2 Cr 0.0000 0.01611(12) 0.0000 0.0288(3) Uani 1 2 d S . . Cl1 Cl -0.22274(11) 0.02309(15) 0.23037(11) 0.0449(4) Uani 1 1 d . . . N1 N -0.0513(3) -0.1665(5) 0.1473(3) 0.0300(10) Uani 1 1 d . . . N2 N 0.0812(3) -0.1213(5) 0.0708(3) 0.0303(11) Uani 1 1 d . . . N3 N 0.2098(3) -0.0607(5) -0.0086(3) 0.0353(11) Uani 1 1 d . . . N4 N 0.0220(4) -0.4138(5) 0.1952(4) 0.0447(13) Uani 1 1 d . . . N5 N 0.3445(4) -0.1385(6) 0.1401(4) 0.0524(15) Uani 1 1 d . . . N6 N -0.1453(3) 0.2083(4) 0.0628(3) 0.0316(11) Uani 1 1 d . . . N7 N -0.0794(3) 0.1547(5) -0.0691(3) 0.0307(10) Uani 1 1 d . . . N8 N -0.0101(4) 0.0985(5) -0.1988(3) 0.0338(11) Uani 1 1 d . . . N9 N -0.1770(4) 0.4632(5) 0.0042(3) 0.0391(12) Uani 1 1 d . . . N10 N -0.1716(4) 0.1945(5) -0.3111(3) 0.0481(15) Uani 1 1 d . . . C1 C -0.1012(5) -0.2525(6) 0.1938(4) 0.0370(14) Uani 1 1 d . . . H1A H -0.1634 -0.2285 0.2102 0.044 Uiso 1 1 calc R . . C2 C -0.0652(5) -0.3723(6) 0.2178(5) 0.0443(16) Uani 1 1 d . . . H2A H -0.1024 -0.4284 0.2515 0.053 Uiso 1 1 calc R . . C3 C 0.0705(4) -0.3322(6) 0.1483(4) 0.0388(13) Uani 1 1 d . . . H3A H 0.1314 -0.3591 0.1302 0.047 Uiso 1 1 calc R . . C4 C 0.0358(4) -0.2054(6) 0.1236(4) 0.0319(13) Uani 1 1 d . . . C5 C 0.1787(4) -0.1168(6) 0.0687(4) 0.0328(13) Uani 1 1 d . . . C6 C 0.2506(5) -0.1537(7) 0.1406(5) 0.0448(16) Uani 1 1 d . . . H6A H 0.2287 -0.1925 0.1931 0.054 Uiso 1 1 calc R . . C7 C 0.3730(5) -0.0861(8) 0.0645(5) 0.059(2) Uani 1 1 d . . . H7A H 0.4408 -0.0734 0.0613 0.070 Uiso 1 1 calc R . . C8 C 0.3076(5) -0.0497(7) -0.0094(5) 0.0467(17) Uani 1 1 d . . . H8A H 0.3321 -0.0160 -0.0623 0.056 Uiso 1 1 calc R . . C9 C -0.1860(4) 0.2996(6) 0.1149(4) 0.0393(15) Uani 1 1 d . . . H9A H -0.2030 0.2762 0.1734 0.047 Uiso 1 1 calc R . . C10 C -0.2021(5) 0.4224(6) 0.0840(5) 0.0421(16) Uani 1 1 d . . . H10A H -0.2326 0.4820 0.1209 0.051 Uiso 1 1 calc R . . C11 C -0.1386(4) 0.3758(6) -0.0476(4) 0.0362(14) Uani 1 1 d . . . H11A H -0.1204 0.4015 -0.1052 0.043 Uiso 1 1 calc R . . C12 C -0.1243(4) 0.2460(6) -0.0194(4) 0.0322(13) Uani 1 1 d . . . C13 C -0.0840(4) 0.1574(6) -0.1623(4) 0.0312(12) Uani 1 1 d . . . C14 C -0.1667(5) 0.2016(5) -0.2211(4) 0.0379(15) Uani 1 1 d . . . H14A H -0.2203 0.2375 -0.1946 0.045 Uiso 1 1 calc R . . C15 C -0.0948(5) 0.1393(7) -0.3453(4) 0.0479(17) Uani 1 1 d . . . H15A H -0.0954 0.1340 -0.4097 0.057 Uiso 1 1 calc R . . C16 C -0.0163(5) 0.0905(6) -0.2910(4) 0.0420(15) Uani 1 1 d . . . H16A H 0.0351 0.0502 -0.3185 0.050 Uiso 1 1 calc R . . Cr3 Cr -0.42227(6) 0.66187(9) 0.36269(6) 0.0291(2) Uani 1 1 d . . . Cr4 Cr -0.5000 0.66551(13) 0.5000 0.0288(3) Uani 1 2 d S . . Cl2 Cl -0.34336(10) 0.65220(16) 0.21936(10) 0.0397(3) Uani 1 1 d . . . N11 N -0.5548(3) 0.5806(5) 0.3031(3) 0.0286(10) Uani 1 1 d . . . N12 N -0.5933(3) 0.5280(5) 0.4465(3) 0.0301(10) Uani 1 1 d . . . N13 N -0.6277(3) 0.4743(5) 0.5921(3) 0.0305(11) Uani 1 1 d . . . N14 N -0.7315(4) 0.4870(5) 0.2220(3) 0.0393(12) Uani 1 1 d . . . N15 N -0.6827(4) 0.2214(5) 0.5363(4) 0.0445(13) Uani 1 1 d . . . N16 N -0.4877(3) 0.8468(4) 0.3417(3) 0.0290(10) Uani 1 1 d . . . N17 N -0.5958(3) 0.8034(5) 0.4469(3) 0.0291(11) Uani 1 1 d . . . N18 N -0.6960(3) 0.7491(5) 0.5553(3) 0.0314(11) Uani 1 1 d . . . N19 N -0.5639(4) 1.0980(5) 0.3126(4) 0.0452(13) Uani 1 1 d . . . N20 N -0.8598(4) 0.8540(6) 0.4521(4) 0.0486(14) Uani 1 1 d . . . C17 C -0.5795(4) 0.5877(6) 0.2136(4) 0.0354(13) Uani 1 1 d . . . H17A H -0.5354 0.6270 0.1768 0.042 Uiso 1 1 calc R . . C18 C -0.6652(5) 0.5412(7) 0.1729(4) 0.0420(15) Uani 1 1 d . . . H18A H -0.6790 0.5467 0.1084 0.050 Uiso 1 1 calc R . . C19 C -0.7071(4) 0.4807(6) 0.3096(4) 0.0354(14) Uani 1 1 d . . . H19A H -0.7526 0.4432 0.3457 0.042 Uiso 1 1 calc R . . C20 C -0.6192(4) 0.5249(6) 0.3542(4) 0.0299(12) Uani 1 1 d . . . C21 C -0.6284(4) 0.4376(6) 0.5044(4) 0.0307(13) Uani 1 1 d . . . C22 C -0.6542(5) 0.3072(6) 0.4778(4) 0.0393(15) Uani 1 1 d . . . H22A H -0.6507 0.2815 0.4163 0.047 Uiso 1 1 calc R . . C23 C -0.6837(5) 0.2609(7) 0.6212(5) 0.0444(16) Uani 1 1 d . . . H23A H -0.7045 0.2022 0.6648 0.053 Uiso 1 1 calc R . . C24 C -0.6557(4) 0.3844(6) 0.6491(4) 0.0366(14) Uani 1 1 d . . . H24A H -0.6563 0.4065 0.7116 0.044 Uiso 1 1 calc R . . C25 C -0.4501(5) 0.9327(6) 0.2839(4) 0.0359(14) Uani 1 1 d . . . H25A H -0.3958 0.9079 0.2535 0.043 Uiso 1 1 calc R . . C26 C -0.4894(5) 1.0535(6) 0.2695(5) 0.0431(16) Uani 1 1 d . . . H26A H -0.4630 1.1089 0.2270 0.052 Uiso 1 1 calc R . . C27 C -0.5994(4) 1.0187(6) 0.3695(4) 0.0404(14) Uani 1 1 d . . . H27A H -0.6506 1.0480 0.4023 0.049 Uiso 1 1 calc R . . C28 C -0.5639(4) 0.8888(6) 0.3842(4) 0.0326(13) Uani 1 1 d . . . C29 C -0.6865(4) 0.8079(6) 0.4757(4) 0.0317(13) Uani 1 1 d . . . C30 C -0.7711(5) 0.8570(6) 0.4237(4) 0.0407(15) Uani 1 1 d . . . H30A H -0.7645 0.8941 0.3657 0.049 Uiso 1 1 calc R . . C31 C -0.8649(5) 0.8036(8) 0.5357(5) 0.0512(18) Uani 1 1 d . . . H31A H -0.9253 0.8057 0.5609 0.061 Uiso 1 1 calc R . . C32 C -0.7850(4) 0.7494(7) 0.5854(4) 0.0412(15) Uani 1 1 d . . . H32A H -0.7925 0.7108 0.6428 0.049 Uiso 1 1 calc R . . C33 C -1.0000 0.459(3) 0.5000 0.167(9) Uiso 1 2 d S . . Cl3 Cl -0.9064(4) 0.3782(6) 0.5795(4) 0.0558(14) Uani 0.33 1 d P . . Cl4 Cl -1.1035(4) 0.4085(10) 0.4955(8) 0.110(4) Uani 0.33 1 d P . . Cl5 Cl -0.9461(4) 0.5102(7) 0.4136(4) 0.0692(17) Uani 0.33 1 d P . . O1 O -0.5807(5) 1.2634(4) 0.0626(5) 0.091(2) Uani 1 1 d . . . H1 H -0.5251 1.2838 0.1024 0.136 Uiso 1 1 d . . . H1' H -0.5819 1.2772 0.0159 0.136 Uiso 1 1 d . . . O2 O -0.4545(4) 0.4786(5) 0.0354(4) 0.0473(14) Uani 0.50 1 d P . . C34 C -0.4545(4) 0.4786(5) 0.0354(4) 0.0473(14) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0306(4) 0.0271(5) 0.0355(5) -0.0033(4) 0.0114(4) -0.0021(4) Cr2 0.0285(6) 0.0248(6) 0.0332(6) 0.000 0.0035(5) 0.000 Cl1 0.0487(9) 0.0384(8) 0.0534(9) -0.0089(8) 0.0304(7) -0.0067(8) N1 0.029(2) 0.032(3) 0.030(2) -0.004(2) 0.010(2) 0.001(2) N2 0.025(2) 0.027(2) 0.041(3) 0.001(2) 0.013(2) 0.002(2) N3 0.024(2) 0.037(3) 0.046(3) 0.011(2) 0.009(2) 0.000(2) N4 0.048(3) 0.035(3) 0.053(3) 0.007(3) 0.012(3) -0.005(3) N5 0.034(3) 0.055(4) 0.068(4) 0.015(3) 0.004(3) -0.002(3) N6 0.025(2) 0.029(3) 0.043(3) -0.004(2) 0.011(2) 0.0048(19) N7 0.030(2) 0.031(3) 0.032(2) -0.002(2) 0.0044(19) 0.005(2) N8 0.037(3) 0.034(3) 0.031(3) -0.004(2) 0.004(2) -0.002(2) N9 0.044(3) 0.032(3) 0.041(3) -0.004(2) 0.003(2) 0.003(2) N10 0.063(4) 0.047(3) 0.032(3) -0.002(2) -0.009(3) 0.012(3) C1 0.042(4) 0.033(3) 0.038(3) 0.000(3) 0.013(3) -0.006(3) C2 0.053(4) 0.035(4) 0.047(4) 0.003(3) 0.017(3) -0.012(3) C3 0.036(3) 0.036(3) 0.046(3) 0.001(3) 0.014(3) 0.001(3) C4 0.033(3) 0.032(3) 0.031(3) 0.002(2) 0.006(2) -0.004(3) C5 0.030(3) 0.029(3) 0.040(3) -0.003(3) 0.009(3) 0.001(2) C6 0.034(3) 0.043(4) 0.056(4) 0.009(3) 0.003(3) -0.005(3) C7 0.020(3) 0.081(6) 0.075(5) 0.017(4) 0.006(3) 0.005(3) C8 0.030(3) 0.054(4) 0.059(4) 0.016(4) 0.016(3) 0.001(3) C9 0.035(3) 0.043(4) 0.042(3) -0.009(3) 0.014(3) 0.001(3) C10 0.037(4) 0.039(4) 0.051(4) -0.016(3) 0.008(3) 0.008(3) C11 0.032(3) 0.034(3) 0.042(3) 0.000(3) -0.001(3) 0.008(3) C12 0.024(3) 0.034(3) 0.039(3) -0.008(3) 0.005(2) 0.000(2) C13 0.033(3) 0.026(3) 0.036(3) -0.001(3) 0.008(2) 0.000(3) C14 0.046(4) 0.027(3) 0.040(3) -0.002(2) 0.001(3) 0.004(3) C15 0.056(4) 0.054(4) 0.033(3) -0.003(3) 0.001(3) 0.004(4) C16 0.052(4) 0.041(4) 0.034(3) -0.002(3) 0.011(3) 0.007(3) Cr3 0.0247(4) 0.0298(5) 0.0333(4) -0.0007(4) 0.0062(3) -0.0006(4) Cr4 0.0256(6) 0.0263(6) 0.0345(6) 0.000 0.0033(5) 0.000 Cl2 0.0331(7) 0.0497(9) 0.0384(7) -0.0022(8) 0.0131(6) -0.0023(8) N11 0.023(2) 0.032(3) 0.031(2) -0.002(2) 0.004(2) -0.001(2) N12 0.029(2) 0.033(3) 0.029(2) 0.001(2) 0.0087(19) -0.006(2) N13 0.025(2) 0.031(3) 0.036(2) 0.003(2) 0.008(2) -0.0007(19) N14 0.038(3) 0.041(3) 0.037(3) 0.000(2) -0.002(2) -0.005(2) N15 0.050(3) 0.034(3) 0.051(3) 0.009(3) 0.013(3) -0.006(3) N16 0.029(2) 0.030(3) 0.030(2) 0.005(2) 0.012(2) -0.001(2) N17 0.026(3) 0.030(3) 0.032(2) 0.004(2) 0.006(2) 0.000(2) N18 0.023(2) 0.037(3) 0.035(3) 0.002(2) 0.005(2) 0.002(2) N19 0.049(3) 0.032(3) 0.057(3) 0.014(3) 0.014(3) -0.008(3) N20 0.032(3) 0.062(4) 0.052(3) 0.008(3) 0.007(3) 0.011(3) C17 0.036(3) 0.034(3) 0.035(3) 0.004(3) 0.003(3) 0.000(3) C18 0.045(4) 0.048(4) 0.033(3) 0.004(3) 0.006(3) -0.005(3) C19 0.028(3) 0.042(3) 0.036(3) -0.001(3) 0.005(3) -0.006(3) C20 0.025(3) 0.026(3) 0.040(3) -0.003(3) 0.009(2) -0.001(3) C21 0.029(3) 0.033(3) 0.030(3) 0.008(2) 0.004(2) -0.003(2) C22 0.047(4) 0.031(3) 0.041(3) 0.004(3) 0.011(3) -0.003(3) C23 0.051(4) 0.036(4) 0.049(4) 0.014(3) 0.017(3) -0.005(3) C24 0.035(3) 0.041(4) 0.036(3) 0.008(3) 0.012(3) -0.004(3) C25 0.035(3) 0.042(4) 0.032(3) 0.006(3) 0.007(3) -0.003(3) C26 0.043(4) 0.041(4) 0.047(4) 0.013(3) 0.013(3) -0.005(3) C27 0.043(3) 0.033(3) 0.047(3) 0.010(3) 0.013(3) 0.006(3) C28 0.031(3) 0.032(3) 0.036(3) 0.000(3) 0.006(3) -0.003(3) C29 0.027(3) 0.034(3) 0.036(3) -0.001(3) 0.008(2) 0.001(2) C30 0.038(4) 0.048(4) 0.037(3) 0.004(3) 0.008(3) -0.001(3) C31 0.028(3) 0.073(5) 0.054(4) 0.014(4) 0.010(3) 0.008(3) C32 0.030(3) 0.055(4) 0.040(3) 0.011(3) 0.011(3) -0.002(3) Cl3 0.049(3) 0.072(4) 0.044(3) 0.000(3) -0.007(3) 0.020(3) Cl4 0.025(3) 0.130(7) 0.173(9) 0.097(7) 0.000(4) -0.012(4) Cl5 0.075(4) 0.078(4) 0.064(3) 0.018(3) 0.048(3) 0.018(4) O1 0.068(4) 0.016(2) 0.193(7) 0.030(3) 0.042(4) 0.006(2) O2 0.032(3) 0.057(3) 0.057(3) -0.035(3) 0.020(2) -0.018(2) C34 0.032(3) 0.057(3) 0.057(3) -0.035(3) 0.020(2) -0.018(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 Cr1 N1 2.109(5) . ? Cr1 N3 2.122(5) 2 ? Cr1 N8 2.123(5) 2 ? Cr1 N6 2.132(5) . ? Cr1 Cr2 2.3846(9) . ? Cr1 Cl1 2.4462(16) . ? Cr2 N7 2.007(5) 2 ? Cr2 N7 2.007(5) . ? Cr2 N2 2.021(5) 2 ? Cr2 N2 2.021(5) . ? Cr2 Cr1 2.3846(9) 2 ? N1 C4 1.349(7) . ? N1 C1 1.355(8) . ? N2 C5 1.349(7) . ? N2 C4 1.364(7) . ? N3 C8 1.354(8) . ? N3 C5 1.389(8) . ? N3 Cr1 2.122(5) 2 ? N4 C3 1.318(8) . ? N4 C2 1.353(9) . ? N5 C6 1.305(8) . ? N5 C7 1.338(9) . ? N6 C12 1.335(8) . ? N6 C9 1.374(8) . ? N7 C13 1.368(7) . ? N7 C12 1.381(7) . ? N8 C13 1.349(7) . ? N8 C16 1.355(7) . ? N8 Cr1 2.123(5) 2 ? N9 C11 1.330(8) . ? N9 C10 1.332(8) . ? N10 C14 1.323(8) . ? N10 C15 1.349(9) . ? C1 C2 1.363(9) . ? C3 C4 1.425(9) . ? C5 C6 1.419(9) . ? C7 C8 1.385(9) . ? C9 C10 1.356(9) . ? C11 C12 1.408(9) . ? C13 C14 1.427(8) . ? C15 C16 1.368(9) . ? Cr3 N11 2.110(4) . ? Cr3 N16 2.117(5) . ? Cr3 N18 2.117(5) 2_456 ? Cr3 N13 2.135(5) 2_456 ? Cr3 Cr4 2.3957(8) . ? Cr3 Cl2 2.4860(16) . ? Cr4 N12 2.014(5) . ? Cr4 N12 2.014(5) 2_456 ? Cr4 N17 2.036(5) 2_456 ? Cr4 N17 2.036(5) . ? Cr4 Cr3 2.3957(9) 2_456 ? N11 C17 1.328(7) . ? N11 C20 1.355(7) . ? N12 C20 1.367(7) . ? N12 C21 1.388(7) . ? N13 C24 1.338(7) . ? N13 C21 1.346(7) . ? N13 Cr3 2.135(5) 2_456 ? N14 C19 1.299(7) . ? N14 C18 1.351(8) . ? N15 C23 1.318(9) . ? N15 C22 1.326(8) . ? N16 C28 1.354(7) . ? N16 C25 1.371(7) . ? N17 C29 1.366(7) . ? N17 C28 1.384(8) . ? N18 C29 1.341(7) . ? N18 C32 1.352(7) . ? N18 Cr3 2.117(5) 2_456 ? N19 C27 1.307(8) . ? N19 C26 1.347(9) . ? N20 C30 1.338(8) . ? N20 C31 1.346(9) . ? C17 C18 1.351(9) . ? C19 C20 1.390(8) . ? C21 C22 1.433(9) . ? C23 C24 1.379(9) . ? C25 C26 1.366(9) . ? C27 C28 1.434(9) . ? C29 C30 1.415(9) . ? C31 C32 1.371(9) . ? C33 Cl4 1.513(12) . ? C33 Cl4 1.513(12) 2_356 ? C33 Cl5 1.632(10) 2_356 ? C33 Cl5 1.632(10) . ? C33 Cl3 1.842(14) 2_356 ? C33 Cl3 1.842(14) . ? Cl3 Cl4 1.172(12) 2_356 ? Cl3 Cl5 2.459(9) 2_356 ? Cl4 Cl3 1.172(12) 2_356 ? Cl4 Cl5 1.775(14) 2_356 ? Cl5 Cl4 1.775(14) 2_356 ? Cl5 Cl3 2.459(9) 2_356 ? O2 C34 1.538(10) 2_455 ? O2 O2 1.538(10) 2_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cr1 N3 91.24(19) . 2 ? N1 Cr1 N8 87.79(19) . 2 ? N3 Cr1 N8 168.40(19) 2 2 ? N1 Cr1 N6 168.27(18) . . ? N3 Cr1 N6 89.44(19) 2 . ? N8 Cr1 N6 89.19(19) 2 . ? N1 Cr1 Cr2 84.15(13) . . ? N3 Cr1 Cr2 83.82(13) 2 . ? N8 Cr1 Cr2 84.58(14) 2 . ? N6 Cr1 Cr2 84.28(13) . . ? N1 Cr1 Cl1 96.30(13) . . ? N3 Cr1 Cl1 96.18(14) 2 . ? N8 Cr1 Cl1 95.42(14) 2 . ? N6 Cr1 Cl1 95.26(13) . . ? Cr2 Cr1 Cl1 179.54(6) . . ? N7 Cr2 N7 89.2(3) 2 . ? N7 Cr2 N2 179.1(2) 2 2 ? N7 Cr2 N2 89.93(18) . 2 ? N7 Cr2 N2 89.93(18) 2 . ? N7 Cr2 N2 179.1(2) . . ? N2 Cr2 N2 91.0(3) 2 . ? N7 Cr2 Cr1 89.77(13) 2 2 ? N7 Cr2 Cr1 89.32(13) . 2 ? N2 Cr2 Cr1 90.16(13) 2 2 ? N2 Cr2 Cr1 90.74(13) . 2 ? N7 Cr2 Cr1 89.32(13) 2 . ? N7 Cr2 Cr1 89.77(13) . . ? N2 Cr2 Cr1 90.74(13) 2 . ? N2 Cr2 Cr1 90.16(13) . . ? Cr1 Cr2 Cr1 178.72(7) 2 . ? C4 N1 C1 117.1(5) . . ? C4 N1 Cr1 122.4(4) . . ? C1 N1 Cr1 120.5(4) . . ? C5 N2 C4 123.9(5) . . ? C5 N2 Cr2 117.3(4) . . ? C4 N2 Cr2 118.5(4) . . ? C8 N3 C5 116.3(5) . . ? C8 N3 Cr1 121.8(4) . 2 ? C5 N3 Cr1 121.7(4) . 2 ? C3 N4 C2 116.5(6) . . ? C6 N5 C7 116.0(6) . . ? C12 N6 C9 116.9(5) . . ? C12 N6 Cr1 121.5(4) . . ? C9 N6 Cr1 121.4(4) . . ? C13 N7 C12 123.1(5) . . ? C13 N7 Cr2 119.0(4) . . ? C12 N7 Cr2 117.9(4) . . ? C13 N8 C16 117.6(5) . . ? C13 N8 Cr1 120.8(4) . 2 ? C16 N8 Cr1 121.6(4) . 2 ? C11 N9 C10 117.0(5) . . ? C14 N10 C15 116.4(5) . . ? N1 C1 C2 122.2(6) . . ? N4 C2 C1 122.0(6) . . ? N4 C3 C4 122.9(6) . . ? N1 C4 N2 116.0(5) . . ? N1 C4 C3 119.3(5) . . ? N2 C4 C3 124.5(5) . . ? N2 C5 N3 115.7(5) . . ? N2 C5 C6 126.1(6) . . ? N3 C5 C6 118.0(5) . . ? N5 C6 C5 125.0(6) . . ? N5 C7 C8 122.5(6) . . ? N3 C8 C7 122.1(6) . . ? C10 C9 N6 120.9(6) . . ? N9 C10 C9 122.9(6) . . ? N9 C11 C12 121.8(6) . . ? N6 C12 N7 116.0(5) . . ? N6 C12 C11 120.5(5) . . ? N7 C12 C11 123.2(6) . . ? N8 C13 N7 116.1(5) . . ? N8 C13 C14 119.2(5) . . ? N7 C13 C14 124.0(5) . . ? N10 C14 C13 122.6(6) . . ? N10 C15 C16 122.7(6) . . ? N8 C16 C15 121.3(6) . . ? N11 Cr3 N16 87.82(18) . . ? N11 Cr3 N18 168.94(18) . 2_456 ? N16 Cr3 N18 89.40(19) . 2_456 ? N11 Cr3 N13 90.24(18) . 2_456 ? N16 Cr3 N13 168.21(18) . 2_456 ? N18 Cr3 N13 90.31(19) 2_456 2_456 ? N11 Cr3 Cr4 84.75(13) . . ? N16 Cr3 Cr4 83.42(12) . . ? N18 Cr3 Cr4 84.30(13) 2_456 . ? N13 Cr3 Cr4 84.82(13) 2_456 . ? N11 Cr3 Cl2 94.14(13) . . ? N16 Cr3 Cl2 97.60(13) . . ? N18 Cr3 Cl2 96.83(13) 2_456 . ? N13 Cr3 Cl2 94.14(13) 2_456 . ? Cr4 Cr3 Cl2 178.48(6) . . ? N12 Cr4 N12 90.6(3) . 2_456 ? N12 Cr4 N17 179.2(2) . 2_456 ? N12 Cr4 N17 89.02(18) 2_456 2_456 ? N12 Cr4 N17 89.02(18) . . ? N12 Cr4 N17 179.2(2) 2_456 . ? N17 Cr4 N17 91.4(3) 2_456 . ? N12 Cr4 Cr3 89.57(13) . 2_456 ? N12 Cr4 Cr3 89.17(13) 2_456 2_456 ? N17 Cr4 Cr3 91.09(14) 2_456 2_456 ? N17 Cr4 Cr3 90.16(14) . 2_456 ? N12 Cr4 Cr3 89.17(13) . . ? N12 Cr4 Cr3 89.57(13) 2_456 . ? N17 Cr4 Cr3 90.16(14) 2_456 . ? N17 Cr4 Cr3 91.09(14) . . ? Cr3 Cr4 Cr3 178.21(7) 2_456 . ? C17 N11 C20 117.8(5) . . ? C17 N11 Cr3 120.3(4) . . ? C20 N11 Cr3 121.9(4) . . ? C20 N12 C21 121.7(5) . . ? C20 N12 Cr4 119.3(4) . . ? C21 N12 Cr4 119.0(4) . . ? C24 N13 C21 116.0(5) . . ? C24 N13 Cr3 122.5(4) . 2_456 ? C21 N13 Cr3 121.5(4) . 2_456 ? C19 N14 C18 116.0(5) . . ? C23 N15 C22 116.6(6) . . ? C28 N16 C25 116.7(5) . . ? C28 N16 Cr3 124.1(4) . . ? C25 N16 Cr3 119.2(4) . . ? C29 N17 C28 123.9(5) . . ? C29 N17 Cr4 118.8(4) . . ? C28 N17 Cr4 117.4(4) . . ? C29 N18 C32 118.0(5) . . ? C29 N18 Cr3 123.1(4) . 2_456 ? C32 N18 Cr3 118.9(4) . 2_456 ? C27 N19 C26 116.8(6) . . ? C30 N20 C31 116.1(6) . . ? N11 C17 C18 122.3(6) . . ? N14 C18 C17 121.4(6) . . ? N14 C19 C20 124.7(6) . . ? N11 C20 N12 115.5(5) . . ? N11 C20 C19 117.8(5) . . ? N12 C20 C19 126.5(5) . . ? N13 C21 N12 115.9(5) . . ? N13 C21 C22 120.1(5) . . ? N12 C21 C22 123.7(5) . . ? N15 C22 C21 122.0(6) . . ? N15 C23 C24 122.4(6) . . ? N13 C24 C23 122.9(6) . . ? C26 C25 N16 120.9(6) . . ? N19 C26 C25 123.2(6) . . ? N19 C27 C28 122.4(6) . . ? N16 C28 N17 115.3(5) . . ? N16 C28 C27 119.9(5) . . ? N17 C28 C27 124.5(5) . . ? N18 C29 N17 116.1(5) . . ? N18 C29 C30 118.6(5) . . ? N17 C29 C30 124.9(5) . . ? N20 C30 C29 123.3(6) . . ? N20 C31 C32 121.7(6) . . ? N18 C32 C31 122.0(6) . . ? Cl4 C33 Cl4 140(2) . 2_356 ? Cl4 C33 Cl5 68.6(5) . 2_356 ? Cl4 C33 Cl5 126.0(5) 2_356 2_356 ? Cl4 C33 Cl5 126.0(5) . . ? Cl4 C33 Cl5 68.6(5) 2_356 . ? Cl5 C33 Cl5 142(2) 2_356 . ? Cl4 C33 Cl3 39.4(6) . 2_356 ? Cl4 C33 Cl3 117.5(13) 2_356 2_356 ? Cl5 C33 Cl3 107.1(4) 2_356 2_356 ? Cl5 C33 Cl3 89.9(4) . 2_356 ? Cl4 C33 Cl3 117.5(13) . . ? Cl4 C33 Cl3 39.4(6) 2_356 . ? Cl5 C33 Cl3 89.9(4) 2_356 . ? Cl5 C33 Cl3 107.1(4) . . ? Cl3 C33 Cl3 126.2(16) 2_356 . ? Cl4 Cl3 C33 55.0(4) 2_356 . ? Cl4 Cl3 Cl5 94.3(5) 2_356 2_356 ? C33 Cl3 Cl5 41.6(3) . 2_356 ? Cl3 Cl4 C33 85.6(6) 2_356 . ? Cl3 Cl4 Cl5 142.5(6) 2_356 2_356 ? C33 Cl4 Cl5 58.9(7) . 2_356 ? C33 Cl5 Cl4 52.5(6) . 2_356 ? C33 Cl5 Cl3 48.5(5) . 2_356 ? Cl4 Cl5 Cl3 83.8(3) 2_356 2_356 ? C34 O2 O2 0.0(5) 2_455 2_455 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.370 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.128 # Attachment 'comp. 5 B700533D revised.cif' data_ic10193 _database_code_depnum_ccdc_archive 'CCDC 637998' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H25 N22 Ni3 O0.50 S2' _chemical_formula_weight 990.01 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.4859(3) _cell_length_b 16.6988(3) _cell_length_c 25.1757(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7771.5(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4024 _exptl_absorpt_coefficient_mu 1.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 0.871 _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 61025 _diffrn_reflns_av_R_equivalents 0.0870 _diffrn_reflns_av_sigmaI/netI 0.0813 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8917 _reflns_number_gt 5376 _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^)+(0.0993P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0039(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8917 _refine_ls_number_parameters 560 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1210 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1808 _refine_ls_wR_factor_gt 0.1470 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.40478(3) 0.21230(3) 0.05063(2) 0.02841(19) Uani 1 1 d . . . Ni2 Ni 0.48525(3) 0.25577(3) 0.12183(2) 0.02645(19) Uani 1 1 d . . . Ni3 Ni 0.56421(3) 0.29911(4) 0.19407(2) 0.0302(2) Uani 1 1 d . . . S1 S 0.26454(7) 0.08141(8) -0.08008(5) 0.0406(3) Uani 1 1 d . . . S2 S 0.66891(10) 0.4132(3) 0.34569(10) 0.0669(13) Uani 0.889(10) 1 d P . . S2' S 0.6774(11) 0.3651(17) 0.3599(8) 0.063(6) Uiso 0.111(10) 1 d P . . N1 N 0.4864(2) 0.2569(2) 0.00222(16) 0.0309(9) Uani 1 1 d . . . N2 N 0.5311(2) 0.3277(2) 0.07476(16) 0.0331(10) Uani 1 1 d . . . N3 N 0.5767(2) 0.4001(2) 0.14676(17) 0.0335(10) Uani 1 1 d . . . N4 N 0.5950(3) 0.3184(3) -0.0631(2) 0.0583(14) Uani 1 1 d . . . N5 N 0.5838(3) 0.5393(3) 0.0851(2) 0.0535(13) Uani 1 1 d . . . N6 N 0.4605(2) 0.1048(2) 0.06227(15) 0.0307(9) Uani 1 1 d . . . N7 N 0.5524(2) 0.1748(2) 0.10270(15) 0.0302(9) Uani 1 1 d . . . N8 N 0.6430(2) 0.2423(2) 0.14978(16) 0.0314(9) Uani 1 1 d . . . N9 N 0.5263(2) -0.0417(2) 0.08455(17) 0.0382(10) Uani 1 1 d . . . N10 N 0.7507(2) 0.1623(3) 0.09397(18) 0.0440(11) Uani 1 1 d . . . N11 N 0.3381(2) 0.1795(2) 0.11357(15) 0.0293(9) Uani 1 1 d . . . N12 N 0.4390(2) 0.1832(2) 0.16846(15) 0.0305(9) Uani 1 1 d . . . N13 N 0.5393(2) 0.1866(2) 0.22330(15) 0.0314(9) Uani 1 1 d . . . N14 N 0.2496(2) 0.1361(3) 0.19818(17) 0.0435(11) Uani 1 1 d . . . N15 N 0.5141(3) 0.0307(3) 0.25722(19) 0.0503(12) Uani 1 1 d . . . N16 N 0.3666(2) 0.3281(2) 0.05798(15) 0.0281(9) Uani 1 1 d . . . N17 N 0.4176(2) 0.3357(2) 0.14098(15) 0.0298(9) Uani 1 1 d . . . N18 N 0.4671(2) 0.3398(2) 0.22624(15) 0.0299(9) Uani 1 1 d . . . N19 N 0.3137(2) 0.4848(2) 0.06491(18) 0.0427(11) Uani 1 1 d . . . N20 N 0.3339(2) 0.3849(3) 0.26932(16) 0.0377(10) Uani 1 1 d . . . N21 N 0.3405(2) 0.1745(2) -0.00704(16) 0.0357(10) Uani 1 1 d . . . N22 N 0.6252(2) 0.3338(3) 0.25444(18) 0.0415(11) Uani 1 1 d . . . C1 C 0.4920(3) 0.2367(3) -0.0496(2) 0.0432(14) Uani 1 1 d . . . H1A H 0.4581 0.2001 -0.0643 0.052 Uiso 1 1 calc R . . C2 C 0.5445(3) 0.2673(4) -0.0813(2) 0.0557(16) Uani 1 1 d . . . H2A H 0.5457 0.2520 -0.1176 0.067 Uiso 1 1 calc R . . C3 C 0.5912(3) 0.3383(3) -0.0122(2) 0.0514(15) Uani 1 1 d . . . H3A H 0.6269 0.3732 0.0019 0.062 Uiso 1 1 calc R . . C4 C 0.5365(3) 0.3099(3) 0.0218(2) 0.0358(12) Uani 1 1 d . . . C5 C 0.5567(3) 0.4002(3) 0.0952(2) 0.0354(12) Uani 1 1 d . . . C6 C 0.5579(3) 0.4720(3) 0.0663(2) 0.0424(13) Uani 1 1 d . . . H6A H 0.5391 0.4717 0.0312 0.051 Uiso 1 1 calc R . . C7 C 0.6089(4) 0.5363(3) 0.1344(3) 0.0566(17) Uani 1 1 d . . . H7A H 0.6308 0.5828 0.1490 0.068 Uiso 1 1 calc R . . C8 C 0.6045(3) 0.4681(3) 0.1652(2) 0.0429(13) Uani 1 1 d . . . H8A H 0.6218 0.4697 0.2007 0.051 Uiso 1 1 calc R . . C9 C 0.4288(3) 0.0350(3) 0.0488(2) 0.0365(12) Uani 1 1 d . . . H9A H 0.3831 0.0358 0.0316 0.044 Uiso 1 1 calc R . . C10 C 0.4612(3) -0.0374(3) 0.0596(2) 0.0408(13) Uani 1 1 d . . . H10A H 0.4375 -0.0855 0.0493 0.049 Uiso 1 1 calc R . . C11 C 0.5567(3) 0.0271(3) 0.0977(2) 0.0361(12) Uani 1 1 d . . . H11A H 0.6019 0.0261 0.1156 0.043 Uiso 1 1 calc R . . C12 C 0.5248(2) 0.1023(3) 0.08626(19) 0.0308(11) Uani 1 1 d . . . C13 C 0.6258(3) 0.1870(3) 0.1127(2) 0.0368(12) Uani 1 1 d . . . C14 C 0.6817(3) 0.1491(3) 0.0848(2) 0.0412(13) Uani 1 1 d . . . H14A H 0.6690 0.1118 0.0578 0.049 Uiso 1 1 calc R . . C15 C 0.7661(3) 0.2158(3) 0.1315(2) 0.0389(13) Uani 1 1 d . . . H15A H 0.8153 0.2260 0.1401 0.047 Uiso 1 1 calc R . . C16 C 0.7132(3) 0.2562(3) 0.1580(2) 0.0399(13) Uani 1 1 d . . . H16A H 0.7268 0.2958 0.1832 0.048 Uiso 1 1 calc R . . C17 C 0.2663(3) 0.1684(3) 0.1075(2) 0.0371(12) Uani 1 1 d . . . H17A H 0.2451 0.1758 0.0735 0.044 Uiso 1 1 calc R . . C18 C 0.2236(3) 0.1469(3) 0.1490(2) 0.0383(12) Uani 1 1 d . . . H18A H 0.1734 0.1391 0.1429 0.046 Uiso 1 1 calc R . . C19 C 0.3193(3) 0.1481(3) 0.2046(2) 0.0382(12) Uani 1 1 d . . . H19A H 0.3390 0.1428 0.2393 0.046 Uiso 1 1 calc R . . C20 C 0.3657(2) 0.1681(3) 0.16306(19) 0.0309(11) Uani 1 1 d . . . C21 C 0.4810(3) 0.1454(3) 0.20631(18) 0.0314(11) Uani 1 1 d . . . C22 C 0.4699(3) 0.0664(3) 0.2238(2) 0.0385(12) Uani 1 1 d . . . H22A H 0.4290 0.0378 0.2110 0.046 Uiso 1 1 calc R . . C23 C 0.5702(3) 0.0728(3) 0.2725(2) 0.0567(17) Uani 1 1 d . . . H23A H 0.6031 0.0489 0.2968 0.068 Uiso 1 1 calc R . . C24 C 0.5842(3) 0.1476(3) 0.2560(2) 0.0492(15) Uani 1 1 d . . . H24A H 0.6270 0.1736 0.2678 0.059 Uiso 1 1 calc R . . C25 C 0.3305(3) 0.3638(3) 0.0176(2) 0.0382(12) Uani 1 1 d . . . H25A H 0.3235 0.3350 -0.0145 0.046 Uiso 1 1 calc R . . C26 C 0.3040(3) 0.4394(3) 0.0216(2) 0.0438(14) Uani 1 1 d . . . H26A H 0.2776 0.4610 -0.0075 0.053 Uiso 1 1 calc R . . C27 C 0.3506(3) 0.4503(3) 0.1042(2) 0.0444(14) Uani 1 1 d . . . H27A H 0.3598 0.4807 0.1354 0.053 Uiso 1 1 calc R . . C28 C 0.3769(3) 0.3711(3) 0.10191(19) 0.0328(11) Uani 1 1 d . . . C29 C 0.4088(3) 0.3524(3) 0.1943(2) 0.0354(12) Uani 1 1 d . . . C30 C 0.3428(3) 0.3744(3) 0.2184(2) 0.0399(13) Uani 1 1 d . . . H30A H 0.3021 0.3819 0.1960 0.048 Uiso 1 1 calc R . . C31 C 0.3927(3) 0.3725(3) 0.3001(2) 0.0391(12) Uani 1 1 d . . . H31A H 0.3890 0.3794 0.3375 0.047 Uiso 1 1 calc R . . C32 C 0.4577(3) 0.3502(3) 0.27836(19) 0.0354(12) Uani 1 1 d . . . H32A H 0.4977 0.3419 0.3014 0.042 Uiso 1 1 calc R . . C33 C 0.3075(3) 0.1356(3) -0.03758(19) 0.0326(11) Uani 1 1 d . . . C34 C 0.6433(3) 0.3647(3) 0.2932(2) 0.0397(13) Uani 1 1 d . . . O1 O 0.2264(5) 0.0480(6) 0.3002(4) 0.083(3) Uiso 0.50 1 d P . . H1 H 0.2482 0.0619 0.2738 0.125 Uiso 0.50 1 d PR . . H1' H 0.2097 0.0928 0.3190 0.125 Uiso 0.50 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 0.0260(4) 0.0313(4) 0.0279(4) -0.0003(3) -0.0009(3) -0.0009(3) Ni2 0.0222(3) 0.0270(3) 0.0302(4) 0.0008(3) 0.0002(3) -0.0005(2) Ni3 0.0228(4) 0.0313(4) 0.0363(4) -0.0013(3) -0.0026(3) -0.0006(3) S1 0.0416(8) 0.0389(7) 0.0415(8) -0.0006(6) -0.0077(6) -0.0082(6) S2 0.0424(11) 0.101(3) 0.0569(15) -0.0369(16) -0.0077(9) 0.0085(11) N1 0.031(2) 0.030(2) 0.033(2) 0.0001(18) 0.0038(18) 0.0011(18) N2 0.029(2) 0.034(2) 0.037(2) 0.0002(19) -0.0011(18) -0.0047(18) N3 0.026(2) 0.030(2) 0.044(3) -0.002(2) 0.0035(19) -0.0038(18) N4 0.063(4) 0.062(3) 0.050(3) -0.010(3) 0.023(3) -0.018(3) N5 0.067(3) 0.034(3) 0.059(3) 0.004(2) 0.014(3) -0.008(2) N6 0.031(2) 0.030(2) 0.031(2) -0.0071(18) 0.0013(18) -0.0012(18) N7 0.025(2) 0.030(2) 0.036(2) -0.0015(18) -0.0022(18) 0.0019(17) N8 0.022(2) 0.034(2) 0.039(2) -0.001(2) -0.0007(18) -0.0021(17) N9 0.037(3) 0.035(2) 0.043(3) -0.001(2) 0.002(2) 0.003(2) N10 0.029(2) 0.053(3) 0.050(3) 0.005(2) 0.002(2) 0.004(2) N11 0.028(2) 0.029(2) 0.031(2) 0.0000(18) -0.0008(17) -0.0004(17) N12 0.027(2) 0.032(2) 0.032(2) 0.0032(18) -0.0001(18) -0.0042(18) N13 0.026(2) 0.035(2) 0.032(2) 0.0040(19) -0.0046(18) -0.0002(18) N14 0.027(2) 0.058(3) 0.046(3) 0.009(2) 0.004(2) -0.003(2) N15 0.055(3) 0.042(3) 0.054(3) 0.014(2) -0.007(3) 0.002(2) N16 0.025(2) 0.031(2) 0.028(2) 0.0027(18) -0.0011(17) 0.0009(17) N17 0.029(2) 0.032(2) 0.028(2) -0.0017(18) -0.0041(17) 0.0047(18) N18 0.027(2) 0.028(2) 0.035(2) -0.0018(18) -0.0011(18) -0.0002(17) N19 0.052(3) 0.036(2) 0.040(3) 0.005(2) -0.003(2) 0.006(2) N20 0.033(2) 0.046(2) 0.034(2) -0.005(2) 0.0022(19) 0.006(2) N21 0.038(2) 0.038(2) 0.030(2) 0.001(2) -0.003(2) 0.001(2) N22 0.031(2) 0.044(3) 0.049(3) -0.002(2) -0.007(2) -0.002(2) C1 0.048(4) 0.041(3) 0.040(3) -0.005(3) 0.002(3) -0.005(3) C2 0.061(4) 0.068(4) 0.038(3) -0.010(3) 0.019(3) -0.017(3) C3 0.047(3) 0.054(4) 0.053(4) -0.012(3) 0.017(3) -0.012(3) C4 0.035(3) 0.037(3) 0.036(3) 0.003(2) 0.006(2) 0.001(2) C5 0.026(3) 0.033(3) 0.048(3) -0.001(2) 0.002(2) -0.002(2) C6 0.044(3) 0.039(3) 0.045(3) 0.009(3) -0.001(3) -0.003(3) C7 0.072(4) 0.038(3) 0.060(4) -0.009(3) 0.017(3) -0.023(3) C8 0.041(3) 0.037(3) 0.051(3) -0.011(3) 0.005(3) -0.007(3) C9 0.037(3) 0.036(3) 0.037(3) -0.001(2) 0.000(2) 0.000(2) C10 0.043(3) 0.034(3) 0.046(3) -0.005(2) 0.006(3) -0.004(3) C11 0.029(3) 0.036(3) 0.044(3) 0.002(2) 0.000(2) 0.005(2) C12 0.027(3) 0.034(3) 0.030(3) -0.002(2) 0.003(2) 0.000(2) C13 0.030(3) 0.039(3) 0.042(3) 0.005(2) 0.002(2) 0.007(2) C14 0.035(3) 0.047(3) 0.041(3) -0.001(3) 0.004(2) 0.006(3) C15 0.019(3) 0.041(3) 0.056(3) 0.003(3) 0.001(2) 0.001(2) C16 0.027(3) 0.040(3) 0.053(3) -0.002(3) -0.005(2) -0.004(2) C17 0.026(3) 0.045(3) 0.040(3) 0.002(2) -0.005(2) -0.001(2) C18 0.021(3) 0.055(3) 0.038(3) 0.000(3) -0.003(2) -0.002(2) C19 0.033(3) 0.052(3) 0.029(3) 0.003(2) 0.000(2) -0.003(3) C20 0.026(3) 0.031(3) 0.036(3) 0.002(2) -0.005(2) -0.002(2) C21 0.027(3) 0.039(3) 0.028(3) 0.005(2) -0.001(2) -0.001(2) C22 0.043(3) 0.034(3) 0.039(3) 0.005(2) -0.004(2) -0.004(2) C23 0.057(4) 0.049(4) 0.064(4) 0.015(3) -0.031(3) -0.001(3) C24 0.041(3) 0.045(3) 0.061(4) 0.013(3) -0.018(3) 0.000(3) C25 0.037(3) 0.042(3) 0.036(3) 0.005(2) -0.002(2) -0.001(2) C26 0.040(3) 0.043(3) 0.049(3) 0.013(3) -0.013(3) 0.003(3) C27 0.057(4) 0.032(3) 0.044(3) -0.002(3) -0.006(3) 0.008(3) C28 0.032(3) 0.031(3) 0.035(3) -0.002(2) -0.001(2) 0.001(2) C29 0.036(3) 0.028(3) 0.042(3) -0.003(2) -0.003(2) 0.001(2) C30 0.027(3) 0.050(3) 0.043(3) -0.006(3) -0.002(2) 0.004(2) C31 0.045(3) 0.043(3) 0.030(3) -0.005(2) 0.004(2) -0.007(3) C32 0.036(3) 0.040(3) 0.030(3) -0.002(2) -0.003(2) 0.000(2) C33 0.030(3) 0.036(3) 0.033(3) 0.005(2) 0.002(2) 0.001(2) C34 0.025(3) 0.049(3) 0.045(3) -0.010(3) 0.000(2) 0.001(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 N21 1.980(4) . ? Ni1 N16 2.067(4) . ? Ni1 N1 2.077(4) . ? Ni1 N11 2.081(4) . ? Ni1 N6 2.090(4) . ? Ni1 Ni2 2.4400(8) . ? Ni2 N2 1.888(4) . ? Ni2 N17 1.891(4) . ? Ni2 N12 1.891(4) . ? Ni2 N7 1.898(4) . ? Ni2 Ni3 2.4417(8) . ? Ni3 N22 1.979(5) . ? Ni3 N8 2.064(4) . ? Ni3 N13 2.070(4) . ? Ni3 N3 2.077(4) . ? Ni3 N18 2.083(4) . ? S1 C33 1.611(5) . ? S2 S2' 0.89(3) . ? S2 C34 1.621(6) . ? S2' C34 1.79(2) . ? N1 C1 1.352(7) . ? N1 C4 1.373(6) . ? N2 C4 1.371(6) . ? N2 C5 1.398(6) . ? N3 C8 1.330(6) . ? N3 C5 1.349(6) . ? N4 C3 1.324(7) . ? N4 C2 1.345(7) . ? N5 C6 1.311(7) . ? N5 C7 1.326(8) . ? N6 C12 1.334(6) . ? N6 C9 1.349(6) . ? N7 C12 1.377(6) . ? N7 C13 1.394(6) . ? N8 C16 1.335(6) . ? N8 C13 1.350(6) . ? N9 C11 1.321(6) . ? N9 C10 1.360(7) . ? N10 C14 1.317(6) . ? N10 C15 1.330(7) . ? N11 C17 1.348(6) . ? N11 C20 1.360(6) . ? N12 C21 1.381(6) . ? N12 C20 1.385(6) . ? N13 C24 1.338(6) . ? N13 C21 1.347(6) . ? N14 C19 1.314(6) . ? N14 C18 1.339(6) . ? N15 C23 1.311(7) . ? N15 C22 1.316(6) . ? N16 C28 1.332(6) . ? N16 C25 1.353(6) . ? N17 C28 1.373(6) . ? N17 C29 1.382(6) . ? N18 C32 1.335(6) . ? N18 C29 1.360(6) . ? N19 C27 1.333(6) . ? N19 C26 1.339(7) . ? N20 C30 1.305(6) . ? N20 C31 1.352(6) . ? N21 C33 1.176(6) . ? N22 C34 1.153(6) . ? C1 C2 1.356(8) . ? C3 C4 1.407(7) . ? C5 C6 1.402(7) . ? C7 C8 1.380(8) . ? C9 C10 1.375(7) . ? C11 C12 1.418(6) . ? C13 C14 1.402(7) . ? C15 C16 1.363(7) . ? C17 C18 1.357(7) . ? C19 C20 1.394(7) . ? C21 C22 1.406(7) . ? C23 C24 1.342(8) . ? C25 C26 1.359(7) . ? C27 C28 1.410(7) . ? C29 C30 1.410(7) . ? C31 C32 1.372(7) . ? 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 N21 Ni1 N16 99.14(16) . . ? N21 Ni1 N1 96.89(16) . . ? N16 Ni1 N1 87.97(14) . . ? N21 Ni1 N11 96.82(16) . . ? N16 Ni1 N11 88.64(15) . . ? N1 Ni1 N11 166.24(15) . . ? N21 Ni1 N6 97.19(16) . . ? N16 Ni1 N6 163.57(15) . . ? N1 Ni1 N6 91.86(15) . . ? N11 Ni1 N6 87.65(15) . . ? N21 Ni1 Ni2 178.68(12) . . ? N16 Ni1 Ni2 82.18(11) . . ? N1 Ni1 Ni2 83.20(11) . . ? N11 Ni1 Ni2 83.12(11) . . ? N6 Ni1 Ni2 81.49(11) . . ? N2 Ni2 N17 90.43(17) . . ? N2 Ni2 N12 179.48(17) . . ? N17 Ni2 N12 89.73(17) . . ? N2 Ni2 N7 90.05(16) . . ? N17 Ni2 N7 179.43(17) . . ? N12 Ni2 N7 89.79(17) . . ? N2 Ni2 Ni1 90.10(12) . . ? N17 Ni2 Ni1 89.66(11) . . ? N12 Ni2 Ni1 89.41(12) . . ? N7 Ni2 Ni1 90.03(12) . . ? N2 Ni2 Ni3 90.62(12) . . ? N17 Ni2 Ni3 89.78(12) . . ? N12 Ni2 Ni3 89.87(12) . . ? N7 Ni2 Ni3 90.52(12) . . ? Ni1 Ni2 Ni3 179.10(3) . . ? N22 Ni3 N8 98.47(17) . . ? N22 Ni3 N13 96.88(16) . . ? N8 Ni3 N13 86.12(15) . . ? N22 Ni3 N3 98.02(17) . . ? N8 Ni3 N3 89.14(15) . . ? N13 Ni3 N3 164.87(16) . . ? N22 Ni3 N18 95.59(16) . . ? N8 Ni3 N18 165.31(15) . . ? N13 Ni3 N18 88.02(15) . . ? N3 Ni3 N18 93.09(15) . . ? N22 Ni3 Ni2 177.92(13) . . ? N8 Ni3 Ni2 83.28(11) . . ? N13 Ni3 Ni2 82.10(11) . . ? N3 Ni3 Ni2 83.09(11) . . ? N18 Ni3 Ni2 82.59(11) . . ? S2' S2 C34 85.9(12) . . ? S2 S2' C34 64.4(13) . . ? C1 N1 C4 117.1(4) . . ? C1 N1 Ni1 122.2(3) . . ? C4 N1 Ni1 120.8(3) . . ? C4 N2 C5 121.5(4) . . ? C4 N2 Ni2 120.4(3) . . ? C5 N2 Ni2 118.1(3) . . ? C8 N3 C5 116.1(4) . . ? C8 N3 Ni3 122.4(4) . . ? C5 N3 Ni3 121.5(3) . . ? C3 N4 C2 116.8(5) . . ? C6 N5 C7 115.8(5) . . ? C12 N6 C9 118.3(4) . . ? C12 N6 Ni1 122.0(3) . . ? C9 N6 Ni1 119.6(3) . . ? C12 N7 C13 123.0(4) . . ? C12 N7 Ni2 117.3(3) . . ? C13 N7 Ni2 119.1(3) . . ? C16 N8 C13 117.0(4) . . ? C16 N8 Ni3 121.5(3) . . ? C13 N8 Ni3 121.4(3) . . ? C11 N9 C10 116.5(4) . . ? C14 N10 C15 116.4(5) . . ? C17 N11 C20 117.0(4) . . ? C17 N11 Ni1 122.2(3) . . ? C20 N11 Ni1 120.8(3) . . ? C21 N12 C20 122.3(4) . . ? C21 N12 Ni2 117.8(3) . . ? C20 N12 Ni2 119.9(3) . . ? C24 N13 C21 116.3(4) . . ? C24 N13 Ni3 121.5(3) . . ? C21 N13 Ni3 121.9(3) . . ? C19 N14 C18 116.4(4) . . ? C23 N15 C22 115.8(4) . . ? C28 N16 C25 117.2(4) . . ? C28 N16 Ni1 122.0(3) . . ? C25 N16 Ni1 120.8(3) . . ? C28 N17 C29 123.0(4) . . ? C28 N17 Ni2 119.0(3) . . ? C29 N17 Ni2 118.0(3) . . ? C32 N18 C29 117.2(4) . . ? C32 N18 Ni3 122.5(3) . . ? C29 N18 Ni3 120.2(3) . . ? C27 N19 C26 115.4(4) . . ? C30 N20 C31 116.1(4) . . ? C33 N21 Ni1 165.0(4) . . ? C34 N22 Ni3 161.0(4) . . ? N1 C1 C2 121.9(5) . . ? N4 C2 C1 122.4(5) . . ? N4 C3 C4 122.8(5) . . ? N2 C4 N1 116.0(4) . . ? N2 C4 C3 124.9(5) . . ? N1 C4 C3 119.0(5) . . ? N3 C5 N2 116.5(4) . . ? N3 C5 C6 119.8(5) . . ? N2 C5 C6 123.6(5) . . ? N5 C6 C5 123.4(5) . . ? N5 C7 C8 122.4(5) . . ? N3 C8 C7 122.1(5) . . ? N6 C9 C10 121.4(5) . . ? N9 C10 C9 121.6(5) . . ? N9 C11 C12 122.9(5) . . ? N6 C12 N7 116.1(4) . . ? N6 C12 C11 119.3(4) . . ? N7 C12 C11 124.3(4) . . ? N8 C13 N7 117.0(4) . . ? N8 C13 C14 118.8(5) . . ? N7 C13 C14 124.0(5) . . ? N10 C14 C13 123.4(5) . . ? N10 C15 C16 121.8(5) . . ? N8 C16 C15 122.4(5) . . ? N11 C17 C18 121.4(5) . . ? N14 C18 C17 122.6(5) . . ? N14 C19 C20 123.2(5) . . ? N11 C20 N12 115.6(4) . . ? N11 C20 C19 119.3(4) . . ? N12 C20 C19 124.9(4) . . ? N13 C21 N12 115.8(4) . . ? N13 C21 C22 119.8(4) . . ? N12 C21 C22 124.2(4) . . ? N15 C22 C21 122.3(5) . . ? N15 C23 C24 124.1(5) . . ? N13 C24 C23 121.6(5) . . ? N16 C25 C26 122.1(5) . . ? N19 C26 C25 122.5(5) . . ? N19 C27 C28 123.4(5) . . ? N16 C28 N17 116.1(4) . . ? N16 C28 C27 119.4(4) . . ? N17 C28 C27 124.3(4) . . ? N18 C29 N17 116.7(4) . . ? N18 C29 C30 118.1(4) . . ? N17 C29 C30 124.9(5) . . ? N20 C30 C29 124.6(5) . . ? N20 C31 C32 121.1(4) . . ? N18 C32 C31 122.8(5) . . ? N21 C33 S1 178.4(5) . . ? N22 C34 S2 176.5(5) . . ? N22 C34 S2' 153.6(10) . . ? S2 C34 S2' 29.8(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.196 _refine_diff_density_min -1.456 _refine_diff_density_rms 0.422