Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global loop_ _publ_author_name 'Kazuyuki Tatsumi' 'Rong Cao' _publ_contact_author_name 'Prof Kazuyuki Tatsumi' _publ_contact_author_address ; Department of Chemistry Nagoya University Research Center for Materials Scien Nagoya 464-8602 JAPAN ; _publ_contact_author_email I45100A@NUCC.CC.NAGOYA-U.AC.JP data_(Cp*WS2)2(NCN) _database_code_CSD 183859 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 N2 S4 W2' _chemical_formula_weight 806.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'W' 'W' -0.8490 6.8722 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7039(7) _cell_length_b 12.2666(12) _cell_length_c 7.3201(5) _cell_angle_alpha 99.980(2) _cell_angle_beta 111.0130(10) _cell_angle_gamma 96.228(4) _cell_volume 624.93(9) _cell_formula_units_Z 1 _cell_measurement_temperature 193 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 402 _exptl_absorpt_coefficient_mu 9.550 _exptl_absorpt_correction_type 4th3D+4th2D _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method '3D method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'not applied' _diffrn_reflns_number 2632 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0075 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.60 _reflns_number_total 2632 _reflns_number_gt 2610 _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^)+(0.0928P)^2^+1.2221P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2632 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1159 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _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 W W 0.32092(2) 0.213694(15) 0.21938(3) 0.01791(14) Uani 1 1 d . . . S1 S 0.2059(3) 0.31664(15) 0.3998(3) 0.0361(4) Uani 1 1 d . . . S2 S 0.5468(3) 0.15270(18) 0.4265(3) 0.0383(4) Uani 1 1 d . . . N N 0.1225(8) 0.0809(5) 0.0898(8) 0.0304(12) Uani 1 1 d . . . C C 0.0000 0.0000 0.0000 0.0231(16) Uani 1 2 d S . . C1 C 0.4956(9) 0.2212(5) 0.0007(9) 0.0231(11) Uani 1 1 d . . . C2 C 0.5400(8) 0.3279(5) 0.1405(9) 0.0224(11) Uani 1 1 d . . . C3 C 0.3718(8) 0.3755(5) 0.0939(9) 0.0219(11) Uani 1 1 d . . . C4 C 0.2234(8) 0.2982(5) -0.0671(9) 0.0226(11) Uani 1 1 d . . . C5 C 0.3008(9) 0.2025(5) -0.1243(9) 0.0247(12) Uani 1 1 d . . . C6 C 0.6339(11) 0.1475(6) -0.0109(12) 0.0354(15) Uani 1 1 d . . . H6A H 0.6853 0.1648 -0.1064 0.053 Uiso 1 1 calc R . . H6B H 0.5714 0.0700 -0.0528 0.053 Uiso 1 1 calc R . . H6C H 0.7343 0.1599 0.1189 0.053 Uiso 1 1 calc R . . C7 C 0.7328(10) 0.3846(7) 0.2916(12) 0.0367(15) Uani 1 1 d . . . H7A H 0.7983 0.4265 0.2289 0.055 Uiso 1 1 calc R . . H7B H 0.8029 0.3287 0.3419 0.055 Uiso 1 1 calc R . . H7C H 0.7209 0.4348 0.4009 0.055 Uiso 1 1 calc R . . C8 C 0.3618(11) 0.4918(6) 0.1852(11) 0.0328(14) Uani 1 1 d . . . H8A H 0.3875 0.5427 0.1082 0.049 Uiso 1 1 calc R . . H8B H 0.4538 0.5144 0.3208 0.049 Uiso 1 1 calc R . . H8C H 0.2375 0.4933 0.1855 0.049 Uiso 1 1 calc R . . C9 C 0.0261(10) 0.3172(8) -0.1661(12) 0.0406(17) Uani 1 1 d . . . H9A H 0.0182 0.3519 -0.2761 0.061 Uiso 1 1 calc R . . H9B H -0.0064 0.3657 -0.0702 0.061 Uiso 1 1 calc R . . H9C H -0.0603 0.2464 -0.2155 0.061 Uiso 1 1 calc R . . C10 C 0.1952(12) 0.1034(7) -0.2957(10) 0.0379(16) Uani 1 1 d . . . H10A H 0.2070 0.1179 -0.4158 0.057 Uiso 1 1 calc R . . H10B H 0.0640 0.0910 -0.3149 0.057 Uiso 1 1 calc R . . H10C H 0.2469 0.0378 -0.2662 0.057 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 W 0.01355(18) 0.01846(19) 0.01867(19) 0.00281(12) 0.00423(12) -0.00019(11) S1 0.0407(9) 0.0288(8) 0.0439(10) 0.0013(7) 0.0268(8) 0.0028(7) S2 0.0268(8) 0.0559(11) 0.0331(9) 0.0225(8) 0.0058(7) 0.0120(8) N 0.029(3) 0.028(3) 0.027(3) 0.003(2) 0.008(2) -0.008(2) C 0.022(4) 0.024(4) 0.025(4) 0.005(3) 0.011(3) 0.005(3) C1 0.025(3) 0.025(3) 0.025(3) 0.009(2) 0.014(2) 0.006(2) C2 0.019(3) 0.017(3) 0.028(3) 0.006(2) 0.006(2) 0.002(2) C3 0.015(2) 0.021(3) 0.027(3) 0.008(2) 0.005(2) 0.002(2) C4 0.016(3) 0.028(3) 0.021(3) 0.008(2) 0.004(2) 0.002(2) C5 0.024(3) 0.026(3) 0.025(3) 0.009(2) 0.011(2) 0.001(2) C6 0.035(4) 0.038(4) 0.046(4) 0.016(3) 0.026(3) 0.017(3) C7 0.018(3) 0.041(4) 0.042(4) 0.008(3) 0.002(3) -0.001(3) C8 0.037(4) 0.024(3) 0.039(4) 0.009(3) 0.013(3) 0.011(3) C9 0.019(3) 0.059(5) 0.035(4) 0.016(3) -0.002(3) 0.006(3) C10 0.047(4) 0.036(4) 0.025(3) 0.002(3) 0.013(3) -0.004(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 W N 1.942(5) . ? W S1 2.1513(17) . ? W S2 2.1610(17) . ? W C2 2.369(6) . ? W C3 2.379(6) . ? W C4 2.414(6) . ? W C1 2.440(6) . ? W C5 2.443(6) . ? N C 1.197(5) . ? C N 1.197(5) 2 ? C1 C5 1.418(9) . ? C1 C2 1.437(8) . ? C1 C6 1.486(9) . ? C2 C3 1.433(8) . ? C2 C7 1.498(8) . ? C3 C4 1.417(8) . ? C3 C8 1.489(8) . ? C4 C5 1.438(9) . ? C4 C9 1.495(9) . ? C5 C10 1.496(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 N W S1 102.42(18) . . ? N W S2 103.35(19) . . ? S1 W S2 106.20(8) . . ? N W C2 138.7(2) . . ? S1 W C2 110.23(15) . . ? S2 W C2 91.28(15) . . ? N W C3 128.3(2) . . ? S1 W C3 86.06(16) . . ? S2 W C3 123.25(15) . . ? C2 W C3 35.1(2) . . ? N W C4 94.1(2) . . ? S1 W C4 97.54(16) . . ? S2 W C4 146.41(15) . . ? C2 W C4 57.8(2) . . ? C3 W C4 34.4(2) . . ? N W C1 105.8(2) . . ? S1 W C1 142.84(15) . . ? S2 W C1 90.29(15) . . ? C2 W C1 34.7(2) . . ? C3 W C1 57.5(2) . . ? C4 W C1 57.10(19) . . ? N W C5 82.3(2) . . ? S1 W C5 131.67(16) . . ? S2 W C5 119.56(16) . . ? C2 W C5 57.2(2) . . ? C3 W C5 57.0(2) . . ? C4 W C5 34.4(2) . . ? C1 W C5 33.8(2) . . ? C N W 176.4(4) . . ? N C N 180.0(7) 2 . ? C5 C1 C2 107.6(5) . . ? C5 C1 C6 127.3(6) . . ? C2 C1 C6 125.0(6) . . ? C5 C1 W 73.2(3) . . ? C2 C1 W 69.9(3) . . ? C6 C1 W 123.7(4) . . ? C3 C2 C1 107.7(5) . . ? C3 C2 C7 126.2(6) . . ? C1 C2 C7 125.7(6) . . ? C3 C2 W 72.8(3) . . ? C1 C2 W 75.3(3) . . ? C7 C2 W 122.9(5) . . ? C4 C3 C2 108.5(5) . . ? C4 C3 C8 126.0(6) . . ? C2 C3 C8 125.2(6) . . ? C4 C3 W 74.2(3) . . ? C2 C3 W 72.0(3) . . ? C8 C3 W 124.8(4) . . ? C3 C4 C5 107.5(5) . . ? C3 C4 C9 125.5(6) . . ? C5 C4 C9 126.9(6) . . ? C3 C4 W 71.5(3) . . ? C5 C4 W 73.9(3) . . ? C9 C4 W 123.1(5) . . ? C1 C5 C4 108.6(5) . . ? C1 C5 C10 125.9(6) . . ? C4 C5 C10 125.4(6) . . ? C1 C5 W 73.0(3) . . ? C4 C5 W 71.7(3) . . ? C10 C5 W 124.2(4) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 2.893 _refine_diff_density_min -3.847 _refine_diff_density_rms 0.305 data_[Cp*WS2(NCN)]K _database_code_CSD 183860 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H15 K N2 S2 W' _chemical_formula_weight 462.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2 1/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2146(11) _cell_length_b 9.3644(13) _cell_length_c 12.9428(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.4420(10) _cell_angle_gamma 90.00 _cell_volume 1471.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 193 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 8.399 _exptl_absorpt_correction_type 4th3D+4th2D _exptl_absorpt_correction_T_min 0.796 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method '3D method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'not applied' _diffrn_reflns_number 3280 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0072 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 27.55 _reflns_number_total 3280 _reflns_number_gt 3216 _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^)+(0.0466P)^2^+3.4894P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3280 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.200 _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 W W 0.266634(13) 0.003869(14) 0.329670(12) 0.02053(9) Uani 1 1 d . . . K K 0.44528(8) -0.42766(11) 0.63535(8) 0.0347(2) Uani 1 1 d . . . S1 S 0.17655(11) 0.00394(12) 0.17347(10) 0.0327(3) Uani 1 1 d . . . S2 S 0.40573(10) 0.15085(14) 0.31901(9) 0.0360(3) Uani 1 1 d . . . N1 N 0.3330(3) -0.1749(4) 0.3379(3) 0.0345(8) Uani 1 1 d . . . N2 N 0.3897(4) -0.4017(4) 0.4203(3) 0.0412(10) Uani 1 1 d . . . C C 0.3615(4) -0.2925(5) 0.3815(3) 0.0295(9) Uani 1 1 d . . . C1 C 0.2285(4) -0.0282(5) 0.5073(3) 0.0258(8) Uani 1 1 d . . . C2 C 0.1322(3) -0.0664(4) 0.4407(3) 0.0245(8) Uani 1 1 d . . . C3 C 0.0911(3) 0.0598(5) 0.3883(3) 0.0287(9) Uani 1 1 d . . . C4 C 0.1651(3) 0.1733(5) 0.4191(3) 0.0282(9) Uani 1 1 d . . . C5 C 0.2495(3) 0.1182(5) 0.4943(3) 0.0269(8) Uani 1 1 d . . . C6 C 0.2927(4) -0.1256(6) 0.5834(3) 0.0374(10) Uani 1 1 d . . . H6A H 0.2630 -0.1214 0.6489 0.056 Uiso 1 1 calc R . . H6B H 0.3685 -0.0962 0.5926 0.056 Uiso 1 1 calc R . . H6C H 0.2879 -0.2217 0.5574 0.056 Uiso 1 1 calc R . . C7 C 0.0793(4) -0.2129(6) 0.4309(4) 0.0432(12) Uani 1 1 d . . . H7A H 0.0278 -0.2225 0.4812 0.065 Uiso 1 1 calc R . . H7B H 0.1352 -0.2849 0.4429 0.065 Uiso 1 1 calc R . . H7C H 0.0415 -0.2241 0.3622 0.065 Uiso 1 1 calc R . . C8 C -0.0168(4) 0.0745(7) 0.3205(4) 0.0442(13) Uani 1 1 d . . . H8A H -0.0741 0.0967 0.3630 0.066 Uiso 1 1 calc R . . H8B H -0.0339 -0.0137 0.2844 0.066 Uiso 1 1 calc R . . H8C H -0.0113 0.1497 0.2710 0.066 Uiso 1 1 calc R . . C9 C 0.1522(5) 0.3260(5) 0.3853(5) 0.0474(13) Uani 1 1 d . . . H9A H 0.1089 0.3761 0.4312 0.071 Uiso 1 1 calc R . . H9B H 0.1158 0.3299 0.3157 0.071 Uiso 1 1 calc R . . H9C H 0.2234 0.3698 0.3875 0.071 Uiso 1 1 calc R . . C10 C 0.3375(4) 0.2042(6) 0.5547(4) 0.0410(11) Uani 1 1 d . . . H10A H 0.3112 0.2384 0.6173 0.062 Uiso 1 1 calc R . . H10B H 0.3564 0.2839 0.5136 0.062 Uiso 1 1 calc R . . H10C H 0.4014 0.1456 0.5720 0.062 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 W 0.02219(13) 0.02280(13) 0.01721(13) -0.00079(5) 0.00490(8) 0.00179(5) K 0.0384(5) 0.0310(5) 0.0372(5) 0.0050(4) 0.0160(4) 0.0036(4) S1 0.0319(6) 0.0463(7) 0.0199(6) -0.0031(4) 0.0022(5) -0.0012(4) S2 0.0324(6) 0.0418(6) 0.0350(6) -0.0074(5) 0.0091(4) -0.0107(5) N1 0.043(2) 0.0295(19) 0.034(2) 0.0012(16) 0.0151(16) 0.0121(16) N2 0.048(2) 0.030(2) 0.047(2) 0.0049(18) 0.0133(19) 0.0119(18) C 0.030(2) 0.031(2) 0.029(2) -0.0050(17) 0.0101(17) 0.0023(17) C1 0.031(2) 0.033(2) 0.0148(19) 0.0001(16) 0.0056(16) 0.0047(18) C2 0.0273(19) 0.028(2) 0.0195(18) -0.0036(15) 0.0075(15) -0.0029(16) C3 0.023(2) 0.041(3) 0.023(2) -0.0036(18) 0.0051(15) 0.0052(18) C4 0.028(2) 0.029(2) 0.029(2) 0.0006(16) 0.0074(16) 0.0075(16) C5 0.027(2) 0.031(2) 0.0243(19) -0.0098(16) 0.0069(15) 0.0006(16) C6 0.039(2) 0.046(3) 0.027(2) 0.0053(19) 0.0031(18) 0.015(2) C7 0.054(3) 0.039(3) 0.040(3) -0.010(2) 0.018(2) -0.017(2) C8 0.026(2) 0.076(4) 0.029(2) 0.003(2) 0.0008(18) 0.006(2) C9 0.056(3) 0.032(2) 0.057(3) 0.010(2) 0.019(3) 0.014(2) C10 0.042(3) 0.046(3) 0.036(2) -0.017(2) 0.005(2) -0.007(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 W N1 1.858(4) . ? W S1 2.1906(13) . ? W S2 2.2029(11) . ? W C4 2.391(4) . ? W C2 2.392(4) . ? W C3 2.411(4) . ? W C5 2.415(4) . ? W C1 2.415(4) . ? W K 3.5816(9) 4 ? K N2 2.732(4) 3_646 ? K N2 2.800(5) . ? K S2 3.1841(16) 3_656 ? K N1 3.238(4) 4_556 ? K S2 3.2419(15) 4_556 ? K C6 3.412(5) . ? K S1 3.4484(17) 4_556 ? K W 3.5816(9) 4_556 ? K K 4.1169(19) 3_646 ? S1 K 3.4484(17) 4 ? S2 K 3.1841(16) 3_656 ? S2 K 3.2419(15) 4 ? N1 C 1.268(6) . ? N1 K 3.238(4) 4 ? N2 C 1.174(6) . ? N2 K 2.732(4) 3_646 ? C1 C5 1.409(6) . ? C1 C2 1.424(6) . ? C1 C6 1.498(6) . ? C2 C3 1.426(7) . ? C2 C7 1.516(6) . ? C3 C4 1.423(6) . ? C3 C8 1.506(6) . ? C4 C5 1.431(6) . ? C4 C9 1.499(6) . ? C5 C10 1.491(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 W S1 102.95(13) . . ? N1 W S2 103.42(13) . . ? S1 W S2 104.66(5) . . ? N1 W C4 144.74(15) . . ? S1 W C4 102.28(11) . . ? S2 W C4 93.51(11) . . ? N1 W C2 92.41(16) . . ? S1 W C2 104.29(10) . . ? S2 W C2 142.71(10) . . ? C4 W C2 57.55(14) . . ? N1 W C3 125.13(17) . . ? S1 W C3 85.29(11) . . ? S2 W C3 127.11(12) . . ? C4 W C3 34.48(15) . . ? C2 W C3 34.53(16) . . ? N1 W C5 115.43(16) . . ? S1 W C5 136.88(11) . . ? S2 W C5 85.52(10) . . ? C4 W C5 34.65(14) . . ? C2 W C5 57.23(14) . . ? C3 W C5 57.17(14) . . ? N1 W C1 87.86(16) . . ? S1 W C1 138.42(12) . . ? S2 W C1 111.70(12) . . ? C4 W C1 57.02(15) . . ? C2 W C1 34.46(15) . . ? C3 W C1 56.93(15) . . ? C5 W C1 33.92(14) . . ? N1 W K 64.19(12) . 4 ? S1 W K 68.56(4) . 4 ? S2 W K 62.97(3) . 4 ? C4 W K 149.56(11) . 4 ? C2 W K 151.68(10) . 4 ? C3 W K 153.85(10) . 4 ? C5 W K 145.88(10) . 4 ? C1 W K 147.29(11) . 4 ? N2 K N2 83.83(13) 3_646 . ? N2 K S2 95.85(10) 3_646 3_656 ? N2 K S2 100.57(10) . 3_656 ? N2 K N1 141.19(12) 3_646 4_556 ? N2 K N1 134.54(12) . 4_556 ? S2 K N1 83.88(7) 3_656 4_556 ? N2 K S2 89.50(10) 3_646 4_556 ? N2 K S2 138.19(10) . 4_556 ? S2 K S2 121.19(4) 3_656 4_556 ? N1 K S2 59.07(7) 4_556 4_556 ? N2 K C6 146.69(13) 3_646 . ? N2 K C6 70.48(11) . . ? S2 K C6 69.50(10) 3_656 . ? N1 K C6 69.03(11) 4_556 . ? S2 K C6 123.77(9) 4_556 . ? N2 K S1 131.22(10) 3_646 4_556 ? N2 K S1 91.81(10) . 4_556 ? S2 K S1 132.49(4) 3_656 4_556 ? N1 K S1 56.58(7) 4_556 4_556 ? S2 K S1 62.55(3) 4_556 4_556 ? C6 K S1 72.09(9) . 4_556 ? N2 K W 126.47(9) 3_646 4_556 ? N2 K W 128.05(10) . 4_556 ? S2 K W 114.36(4) 3_656 4_556 ? N1 K W 31.10(6) 4_556 4_556 ? S2 K W 37.25(2) 4_556 4_556 ? C6 K W 86.63(8) . 4_556 ? S1 K W 36.25(2) 4_556 4_556 ? N2 K K 42.55(9) 3_646 3_646 ? N2 K K 41.28(8) . 3_646 ? S2 K K 101.09(4) 3_656 3_646 ? N1 K K 173.82(9) 4_556 3_646 ? S2 K K 120.08(5) 4_556 3_646 ? C6 K K 109.11(8) . 3_646 ? S1 K K 117.31(5) 4_556 3_646 ? W K K 144.45(4) 4_556 3_646 ? W S1 K 75.19(4) . 4 ? W S2 K 157.79(5) . 3_656 ? W S2 K 79.78(4) . 4 ? K S2 K 122.13(4) 3_656 4 ? C N1 W 154.8(3) . . ? C N1 K 119.8(3) . 4 ? W N1 K 84.71(13) . 4 ? C N2 K 125.9(3) . 3_646 ? C N2 K 121.9(3) . . ? K N2 K 96.17(13) 3_646 . ? N2 C N1 178.5(5) . . ? C5 C1 C2 108.7(4) . . ? C5 C1 C6 125.6(4) . . ? C2 C1 C6 125.5(4) . . ? C5 C1 W 73.0(2) . . ? C2 C1 W 71.9(2) . . ? C6 C1 W 124.0(3) . . ? C1 C2 C3 107.6(4) . . ? C1 C2 C7 126.4(4) . . ? C3 C2 C7 125.9(4) . . ? C1 C2 W 73.6(2) . . ? C3 C2 W 73.4(2) . . ? C7 C2 W 120.9(3) . . ? C4 C3 C2 107.9(4) . . ? C4 C3 C8 125.7(4) . . ? C2 C3 C8 126.2(5) . . ? C4 C3 W 72.0(2) . . ? C2 C3 W 72.0(2) . . ? C8 C3 W 126.0(3) . . ? C3 C4 C5 108.0(4) . . ? C3 C4 C9 126.0(4) . . ? C5 C4 C9 125.9(4) . . ? C3 C4 W 73.5(2) . . ? C5 C4 W 73.6(2) . . ? C9 C4 W 122.4(3) . . ? C1 C5 C4 107.7(4) . . ? C1 C5 C10 126.4(4) . . ? C4 C5 C10 125.7(4) . . ? C1 C5 W 73.1(2) . . ? C4 C5 W 71.8(2) . . ? C10 C5 W 125.0(3) . . ? C1 C6 K 150.3(3) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.790 _refine_diff_density_min -1.268 _refine_diff_density_rms 0.140 data_[Co2(2_2'-bipy)4(NCN)2].CH3CN _database_code_CSD 183861 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H35 Cl2 Co2 N13 O8' _chemical_formula_weight 1062.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Co' 'Co' 0.3494 0.9721 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.096(2) _cell_length_b 15.189(4) _cell_length_c 13.9472(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.9350(10) _cell_angle_gamma 90.00 _cell_volume 4767.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 193 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'polyhedra' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 0.874 _exptl_absorpt_correction_type 4th3D+4th2D _exptl_absorpt_correction_T_min 0.576 _exptl_absorpt_correction_T_max 1.003 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _diffrn_measurement_method '3D method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'not applied' _diffrn_reflns_number 5444 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.55 _reflns_number_total 5444 _reflns_number_gt 5398 _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^)+(0.0715P)^2^+22.7199P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5444 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0904 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2076 _refine_ls_wR_factor_gt 0.2069 _refine_ls_goodness_of_fit_ref 1.479 _refine_ls_restrained_S_all 1.479 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.46994(3) 0.23025(4) 0.39852(4) 0.01778(18) Uani 1 1 d . . . Cl Cl 0.24960(6) 0.07406(10) 0.11659(11) 0.0403(3) Uani 1 1 d . . . O1 O 0.1937(2) 0.1149(4) 0.0961(5) 0.070(2) Uani 0.981(19) 1 d P . . O2 O 0.28259(19) 0.1174(3) 0.0629(3) 0.0481(17) Uani 0.961(16) 1 d P . . O3 O 0.2826(3) 0.0715(6) 0.2222(5) 0.113(4) Uani 0.99(2) 1 d P . . O4 O 0.2385(4) -0.0150(4) 0.0808(7) 0.097(4) Uani 0.90(2) 1 d P . . N1 N 0.46882(18) 0.3276(3) 0.4920(3) 0.0239(8) Uani 1 1 d . . . N2 N 0.39738(17) 0.2869(2) 0.3107(3) 0.0223(8) Uani 1 1 d . . . N3 N 0.54180(17) 0.1800(2) 0.4956(3) 0.0215(7) Uani 1 1 d . . . N4 N 0.43185(17) 0.1480(2) 0.4660(3) 0.0230(8) Uani 1 1 d . . . N5 N 0.51334(17) 0.3113(2) 0.3434(3) 0.0213(7) Uani 1 1 d . . . N6 N 0.46477(16) 0.1403(2) 0.2955(3) 0.0197(7) Uani 1 1 d . . . N7 N 0.1646 0.2009 0.3527 0.104(6) Uiso 0.50 1 d P . . C1 C 0.5099(2) 0.3443(3) 0.5855(4) 0.0307(11) Uani 1 1 d . . . C2 C 0.5090(3) 0.4214(4) 0.6380(4) 0.0375(12) Uani 1 1 d . . . C3 C 0.4639(3) 0.4809(4) 0.5966(4) 0.0401(13) Uani 1 1 d . . . C4 C 0.4215(3) 0.4642(3) 0.5016(4) 0.0342(11) Uani 1 1 d . . . C5 C 0.4255(2) 0.3880(3) 0.4499(4) 0.0263(10) Uani 1 1 d . . . C6 C 0.3861(2) 0.3657(3) 0.3452(4) 0.0254(9) Uani 1 1 d . . . C7 C 0.3416(3) 0.4208(4) 0.2836(5) 0.0392(12) Uani 1 1 d . . . C8 C 0.3084(3) 0.3938(4) 0.1849(4) 0.0414(13) Uani 1 1 d . . . C9 C 0.3185(2) 0.3128(4) 0.1518(4) 0.0368(12) Uani 1 1 d . . . C10 C 0.3637(2) 0.2600(3) 0.2170(4) 0.0271(10) Uani 1 1 d . . . C11 C 0.5970(2) 0.2050(3) 0.5076(4) 0.0277(10) Uani 1 1 d . . . C12 C 0.6463(2) 0.1694(4) 0.5835(4) 0.0370(12) Uani 1 1 d . . . C13 C 0.6382(2) 0.1049(4) 0.6471(4) 0.0380(12) Uani 1 1 d . . . C14 C 0.5812(2) 0.0780(4) 0.6347(4) 0.0333(11) Uani 1 1 d . . . C15 C 0.5333(2) 0.1182(3) 0.5591(3) 0.0234(9) Uani 1 1 d . . . C16 C 0.4706(2) 0.0999(3) 0.5417(3) 0.0244(9) Uani 1 1 d . . . C17 C 0.4516(3) 0.0398(3) 0.5987(4) 0.0331(11) Uani 1 1 d . . . C18 C 0.3911(3) 0.0279(4) 0.5762(4) 0.0367(12) Uani 1 1 d . . . C19 C 0.3518(3) 0.0769(4) 0.4976(4) 0.0393(13) Uani 1 1 d . . . C20 C 0.3737(2) 0.1354(3) 0.4437(4) 0.0298(10) Uani 1 1 d . . . C21 C 0.5000 0.3099(4) 0.2500 0.0201(12) Uani 1 2 d S . . C22 C 0.5000 0.1433(4) 0.2500 0.0178(11) Uani 1 2 d S . . C25 C 0.2500 0.2500 0.5000 0.090(4) Uiso 1 2 d S . . C26 C 0.1999 0.1992 0.4657 0.058(7) Uiso 0.25 1 d P . . C26' C 0.2160 0.2461 0.3817 0.053(6) Uiso 0.25 1 d P . . H1 H 0.5447 0.2957 0.6202 0.030 Uiso 1 1 d . . . H2 H 0.5439 0.4235 0.7076 0.030 Uiso 1 1 d . . . H3 H 0.4623 0.5409 0.6299 0.030 Uiso 1 1 d . . . H4 H 0.3975 0.5070 0.4700 0.030 Uiso 1 1 d . . . H5 H 0.3363 0.4826 0.3127 0.030 Uiso 1 1 d . . . H6 H 0.2755 0.4351 0.1404 0.030 Uiso 1 1 d . . . H7 H 0.2933 0.2858 0.0873 0.030 Uiso 1 1 d . . . H8 H 0.3684 0.2034 0.1886 0.030 Uiso 1 1 d . . . H9 H 0.5978 0.2549 0.4604 0.030 Uiso 1 1 d . . . H10 H 0.6874 0.1939 0.5986 0.030 Uiso 1 1 d . . . H11 H 0.6697 0.0635 0.6949 0.030 Uiso 1 1 d . . . H12 H 0.5753 0.0388 0.6858 0.030 Uiso 1 1 d . . . H13 H 0.4771 -0.0026 0.6520 0.030 Uiso 1 1 d . . . H14 H 0.3804 -0.0103 0.6235 0.030 Uiso 1 1 d . . . H15 H 0.3105 0.0620 0.4644 0.030 Uiso 1 1 d . . . H16 H 0.3486 0.1721 0.3946 0.030 Uiso 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 0.0235(3) 0.0154(3) 0.0147(3) 0.0005(2) 0.0071(2) 0.0009(2) Cl 0.0332(7) 0.0422(8) 0.0440(7) 0.0098(6) 0.0118(6) -0.0031(5) O1 0.053(3) 0.071(4) 0.094(5) 0.017(3) 0.036(3) 0.020(3) O2 0.041(3) 0.056(3) 0.048(3) 0.011(2) 0.016(2) -0.013(2) O3 0.093(5) 0.173(9) 0.049(4) 0.049(4) -0.005(3) -0.023(5) O4 0.117(7) 0.040(4) 0.183(9) -0.025(4) 0.113(7) -0.019(3) N1 0.034(2) 0.0221(19) 0.0191(18) -0.0021(14) 0.0140(16) -0.0024(16) N2 0.0254(19) 0.0201(18) 0.0215(18) 0.0002(14) 0.0086(15) 0.0021(14) N3 0.0274(19) 0.0207(18) 0.0160(17) -0.0018(14) 0.0074(14) 0.0010(15) N4 0.032(2) 0.0194(18) 0.0193(18) -0.0004(14) 0.0111(15) 0.0003(15) N5 0.0267(19) 0.0189(18) 0.0188(18) 0.0003(14) 0.0086(15) -0.0001(15) N6 0.0268(19) 0.0137(16) 0.0180(16) 0.0007(13) 0.0071(15) -0.0015(14) C1 0.040(3) 0.032(3) 0.020(2) -0.0063(19) 0.011(2) -0.003(2) C2 0.050(3) 0.040(3) 0.025(2) -0.010(2) 0.017(2) -0.008(3) C3 0.065(4) 0.026(3) 0.041(3) -0.012(2) 0.033(3) -0.008(3) C4 0.049(3) 0.022(2) 0.039(3) -0.002(2) 0.025(2) 0.004(2) C5 0.037(3) 0.023(2) 0.026(2) -0.0023(18) 0.019(2) -0.0003(19) C6 0.028(2) 0.022(2) 0.029(2) 0.0025(18) 0.0136(19) 0.0052(18) C7 0.041(3) 0.033(3) 0.046(3) 0.005(2) 0.018(3) 0.015(2) C8 0.034(3) 0.045(3) 0.039(3) 0.009(2) 0.006(2) 0.018(2) C9 0.029(3) 0.046(3) 0.030(3) 0.001(2) 0.003(2) 0.005(2) C10 0.028(2) 0.027(2) 0.026(2) -0.0025(19) 0.0088(19) 0.0022(19) C11 0.028(2) 0.031(2) 0.024(2) 0.0006(19) 0.0081(19) -0.0007(19) C12 0.027(2) 0.048(3) 0.033(3) -0.002(2) 0.006(2) 0.005(2) C13 0.037(3) 0.043(3) 0.028(3) 0.004(2) 0.005(2) 0.017(2) C14 0.043(3) 0.032(3) 0.023(2) 0.005(2) 0.010(2) 0.012(2) C15 0.032(2) 0.021(2) 0.018(2) -0.0002(17) 0.0106(18) 0.0027(18) C16 0.038(3) 0.020(2) 0.016(2) 0.0002(16) 0.0120(18) 0.0030(19) C17 0.052(3) 0.025(2) 0.025(2) 0.0031(19) 0.017(2) -0.003(2) C18 0.054(3) 0.028(3) 0.035(3) 0.003(2) 0.025(3) -0.009(2) C19 0.040(3) 0.042(3) 0.041(3) -0.002(2) 0.021(2) -0.013(2) C20 0.032(2) 0.028(2) 0.032(2) 0.003(2) 0.014(2) -0.002(2) C21 0.028(3) 0.008(2) 0.026(3) 0.000 0.011(2) 0.000 C22 0.022(3) 0.009(2) 0.017(3) 0.000 0.001(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N3 1.934(4) . ? Co N2 1.941(4) . ? Co N5 1.942(4) . ? Co N6 1.954(4) . ? Co N4 1.976(4) . ? Co N1 1.978(4) . ? Cl O3 1.402(6) . ? Cl O1 1.416(5) . ? Cl O2 1.432(4) . ? Cl O4 1.434(6) . ? N1 C1 1.350(6) . ? N1 C5 1.355(6) . ? N2 C10 1.332(6) . ? N2 C6 1.354(6) . ? N3 C11 1.335(6) . ? N3 C15 1.355(6) . ? N4 C20 1.336(6) . ? N4 C16 1.348(6) . ? N5 C21 1.226(4) . ? N6 C22 1.229(4) . ? N7 C26' 1.34607(12) . ? N7 C26 1.5003 . ? C1 C2 1.386(7) . ? C2 C3 1.371(9) . ? C3 C4 1.377(8) . ? C4 C5 1.386(7) . ? C5 C6 1.468(7) . ? C6 C7 1.388(7) . ? C7 C8 1.385(8) . ? C8 C9 1.367(8) . ? C9 C10 1.396(7) . ? C11 C12 1.388(7) . ? C12 C13 1.382(8) . ? C13 C14 1.384(8) . ? C14 C15 1.396(7) . ? C15 C16 1.469(7) . ? C16 C17 1.391(7) . ? C17 C18 1.389(8) . ? C18 C19 1.382(8) . ? C19 C20 1.386(7) . ? C21 N5 1.226(4) 2_655 ? C22 N6 1.229(4) 2_655 ? C25 C26 1.36712(13) 7_556 ? C25 C26 1.36712(13) . ? C25 C26' 1.5593 7_556 ? C25 C26' 1.5593 . ? C26 C26' 1.5354 . ? 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 N3 Co N2 175.10(15) . . ? N3 Co N5 93.03(16) . . ? N2 Co N5 87.73(16) . . ? N3 Co N6 92.54(15) . . ? N2 Co N6 92.26(15) . . ? N5 Co N6 93.10(15) . . ? N3 Co N4 82.48(16) . . ? N2 Co N4 96.54(16) . . ? N5 Co N4 174.96(16) . . ? N6 Co N4 89.40(15) . . ? N3 Co N1 93.07(16) . . ? N2 Co N1 82.15(16) . . ? N5 Co N1 85.59(15) . . ? N6 Co N1 174.30(16) . . ? N4 Co N1 92.34(15) . . ? O3 Cl O1 111.5(5) . . ? O3 Cl O2 110.5(4) . . ? O1 Cl O2 111.0(3) . . ? O3 Cl O4 107.7(5) . . ? O1 Cl O4 107.3(4) . . ? O2 Cl O4 108.7(3) . . ? C1 N1 C5 118.5(4) . . ? C1 N1 Co 126.8(3) . . ? C5 N1 Co 114.2(3) . . ? C10 N2 C6 119.4(4) . . ? C10 N2 Co 125.4(3) . . ? C6 N2 Co 114.7(3) . . ? C11 N3 C15 119.4(4) . . ? C11 N3 Co 125.3(3) . . ? C15 N3 Co 115.1(3) . . ? C20 N4 C16 118.6(4) . . ? C20 N4 Co 127.4(3) . . ? C16 N4 Co 114.0(3) . . ? C21 N5 Co 115.9(3) . . ? C22 N6 Co 118.6(3) . . ? C26' N7 C26 65.022(3) . . ? N1 C1 C2 121.6(5) . . ? C3 C2 C1 119.6(5) . . ? C2 C3 C4 119.2(5) . . ? C3 C4 C5 119.2(5) . . ? N1 C5 C4 121.7(5) . . ? N1 C5 C6 113.6(4) . . ? C4 C5 C6 124.7(5) . . ? N2 C6 C7 121.4(5) . . ? N2 C6 C5 114.6(4) . . ? C7 C6 C5 124.0(5) . . ? C8 C7 C6 118.7(5) . . ? C9 C8 C7 119.6(5) . . ? C8 C9 C10 119.2(5) . . ? N2 C10 C9 121.6(4) . . ? N3 C11 C12 121.9(5) . . ? C13 C12 C11 119.2(5) . . ? C12 C13 C14 119.4(5) . . ? C13 C14 C15 118.8(5) . . ? N3 C15 C14 121.3(4) . . ? N3 C15 C16 114.2(4) . . ? C14 C15 C16 124.5(4) . . ? N4 C16 C17 121.8(5) . . ? N4 C16 C15 114.2(4) . . ? C17 C16 C15 124.0(4) . . ? C18 C17 C16 119.3(5) . . ? C19 C18 C17 118.5(5) . . ? C18 C19 C20 119.2(5) . . ? N4 C20 C19 122.5(5) . . ? N5 C21 N5 178.1(6) . 2_655 ? N6 C22 N6 175.7(6) . 2_655 ? C26 C25 C26 180.0 7_556 . ? C26 C25 C26' 62.885(2) 7_556 7_556 ? C26 C25 C26' 117.115(2) . 7_556 ? C26 C25 C26' 117.115(2) 7_556 . ? C26 C25 C26' 62.885(2) . . ? C26' C25 C26' 180.0 7_556 . ? C25 C26 N7 117.134(3) . . ? C25 C26 C26' 64.689(5) . . ? N7 C26 C26' 52.629(4) . . ? N7 C26' C26 62.349(4) . . ? N7 C26' C25 114.598(2) . . ? C26 C26' C25 52.426(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.970 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.161