Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bensch, Wolfgang' 'Stahler, Ralph' _publ_contact_author_name 'Prof D Wolfgang Bensch' _publ_contact_author_address ; Prof D Wolfgang Bensch Institut fur Anorganische Chemie Universitat Kiel Olshausenstr. 40 D-24098 Kiel GERMANY ; _publ_contact_author_email 'WBENSCH@AC.UNI-KIEL.DE' data_rs201 _database_code_CSD 161743 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 Co2 N8 S5 Sb2' _chemical_formula_weight 814.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 30.157(6) _cell_length_b 7.7196(15) _cell_length_c 22.875(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.68(3) _cell_angle_gamma 90.00 _cell_volume 5307.6(18) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.038 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3200 _exptl_absorpt_coefficient_mu 3.653 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24623 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.01 _reflns_number_total 6230 _reflns_number_gt 5248 _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^)+(0.0367P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00049(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6230 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0586 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 S1 S 0.199573(19) 0.58767(8) 0.27006(2) 0.02751(12) Uani 1 1 d . . . S2 S 0.17133(2) 0.24887(11) 0.37595(3) 0.03846(16) Uani 1 1 d . . . Sb1 Sb 0.164366(5) 0.30535(2) 0.274124(6) 0.02547(6) Uani 1 1 d . . . S3 S 0.085494(18) 0.40455(8) 0.26389(2) 0.02534(12) Uani 1 1 d . . . Sb2 Sb 0.051788(5) 0.18723(2) 0.194112(7) 0.02864(6) Uani 1 1 d . . . S4 S 0.09394(4) 0.21077(11) 0.11339(3) 0.0589(3) Uani 1 1 d . . . S5 S 0.08239(3) -0.07614(9) 0.23524(3) 0.04124(17) Uani 1 1 d . . . Co1 Co 0.187179(10) 0.65667(4) 0.169824(13) 0.02217(8) Uani 1 1 d . . . Co2 Co 0.072135(10) -0.11702(4) 0.334317(13) 0.02400(8) Uani 1 1 d . . . N1 N 0.18191(6) 0.7174(3) 0.07026(8) 0.0240(4) Uani 1 1 d . . . C1 C 0.21801(8) 0.6230(4) 0.04485(10) 0.0314(5) Uani 1 1 d . . . H1A H 0.2449 0.6922 0.0485 0.038 Uiso 1 1 calc R . . H1B H 0.2101 0.6026 0.0035 0.038 Uiso 1 1 calc R . . C2 C 0.22631(9) 0.4527(4) 0.07573(11) 0.0362(6) Uani 1 1 d . . . H2A H 0.2005 0.3782 0.0692 0.043 Uiso 1 1 calc R . . H2B H 0.2516 0.3947 0.0609 0.043 Uiso 1 1 calc R . . N2 N 0.19969(7) 0.9208(3) 0.16997(10) 0.0342(5) Uani 1 1 d . . . H1N2 H 0.1746 0.9784 0.1764 0.041 Uiso 1 1 calc R . . H2N2 H 0.2203 0.9463 0.1994 0.041 Uiso 1 1 calc R . . C5 C 0.18585(9) 0.9053(4) 0.06384(12) 0.0345(6) Uani 1 1 d . . . H5A H 0.1566 0.9580 0.0636 0.041 Uiso 1 1 calc R . . H5B H 0.1979 0.9317 0.0268 0.041 Uiso 1 1 calc R . . C6 C 0.21574(9) 0.9790(4) 0.11343(12) 0.0379(6) Uani 1 1 d . . . H6A H 0.2460 0.9397 0.1105 0.045 Uiso 1 1 calc R . . H6B H 0.2154 1.1045 0.1114 0.045 Uiso 1 1 calc R . . N3 N 0.23523(7) 0.4894(3) 0.13877(9) 0.0333(5) Uani 1 1 d . . . H1N3 H 0.2623 0.5381 0.1451 0.040 Uiso 1 1 calc R . . H2N3 H 0.2354 0.3893 0.1589 0.040 Uiso 1 1 calc R . . N4 N 0.12021(6) 0.6188(3) 0.14697(9) 0.0291(4) Uani 1 1 d . . . H1N4 H 0.1147 0.5042 0.1467 0.035 Uiso 1 1 calc R . . H2N4 H 0.1047 0.6667 0.1748 0.035 Uiso 1 1 calc R . . C3 C 0.13804(8) 0.6536(4) 0.04694(10) 0.0324(5) Uani 1 1 d . . . H3A H 0.1395 0.5298 0.0401 0.039 Uiso 1 1 calc R . . H3B H 0.1295 0.7096 0.0098 0.039 Uiso 1 1 calc R . . C4 C 0.10388(8) 0.6910(4) 0.08971(12) 0.0358(6) Uani 1 1 d . . . H4A H 0.0995 0.8150 0.0930 0.043 Uiso 1 1 calc R . . H4B H 0.0757 0.6383 0.0763 0.043 Uiso 1 1 calc R . . N6 N 0.06602(7) -0.1895(3) 0.42939(9) 0.0298(4) Uani 1 1 d . . . C7 C 0.02330(11) -0.2809(4) 0.43205(14) 0.0477(7) Uani 1 1 d . . . H7A H -0.0005 -0.1971 0.4338 0.057 Uiso 1 1 calc R . . H7B H 0.0243 -0.3510 0.4673 0.057 Uiso 1 1 calc R . . C8 C 0.01410(10) -0.3947(4) 0.37919(13) 0.0449(7) Uani 1 1 d . . . H8A H 0.0345 -0.4920 0.3813 0.054 Uiso 1 1 calc R . . H8B H -0.0160 -0.4397 0.3783 0.054 Uiso 1 1 calc R . . N7 N 0.13664(8) -0.1924(4) 0.35961(11) 0.0470(6) Uani 1 1 d . . . H1N7 H 0.1434 -0.2835 0.3375 0.056 Uiso 1 1 calc R . . H2N7 H 0.1550 -0.1052 0.3517 0.056 Uiso 1 1 calc R . . C9 C 0.10383(12) -0.3007(5) 0.44724(14) 0.0524(8) Uani 1 1 d . . . H9A H 0.0972 -0.4185 0.4346 0.063 Uiso 1 1 calc R . . H9B H 0.1087 -0.3007 0.4897 0.063 Uiso 1 1 calc R . . C10 C 0.14551(10) -0.2401(5) 0.42127(14) 0.0503(8) Uani 1 1 d . . . H10A H 0.1576 -0.1409 0.4432 0.060 Uiso 1 1 calc R . . H10B H 0.1676 -0.3317 0.4247 0.060 Uiso 1 1 calc R . . N5 N 0.01945(7) -0.2943(3) 0.32560(10) 0.0341(5) Uani 1 1 d . . . H1N5 H -0.0060 -0.2364 0.3157 0.041 Uiso 1 1 calc R . . H2N5 H 0.0240 -0.3680 0.2962 0.041 Uiso 1 1 calc R . . N8 N 0.06321(7) 0.1243(3) 0.37163(8) 0.0268(4) Uani 1 1 d . . . H1N8 H 0.0896 0.1796 0.3754 0.032 Uiso 1 1 calc R . . H2N8 H 0.0446 0.1870 0.3472 0.032 Uiso 1 1 calc R . . C11 C 0.06695(10) -0.0277(4) 0.46379(11) 0.0378(6) Uani 1 1 d . . . H11A H 0.0976 0.0031 0.4755 0.045 Uiso 1 1 calc R . . H11B H 0.0517 -0.0459 0.4991 0.045 Uiso 1 1 calc R . . C12 C 0.04517(9) 0.1168(4) 0.42921(10) 0.0326(5) Uani 1 1 d . . . H12A H 0.0133 0.0981 0.4243 0.039 Uiso 1 1 calc R . . H12B H 0.0507 0.2255 0.4498 0.039 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 S1 0.0282(3) 0.0335(3) 0.0205(3) 0.0028(2) -0.0001(2) -0.0012(2) S2 0.0331(3) 0.0530(5) 0.0279(3) 0.0141(3) -0.0056(2) -0.0081(3) Sb1 0.02648(8) 0.02762(10) 0.02238(8) -0.00089(6) 0.00253(6) 0.00374(6) S3 0.0274(3) 0.0261(3) 0.0228(3) -0.0024(2) 0.0033(2) 0.0028(2) Sb2 0.02825(9) 0.03027(11) 0.02595(9) -0.00081(6) -0.00662(6) -0.00157(6) S4 0.1220(8) 0.0355(5) 0.0224(3) -0.0030(3) 0.0245(4) -0.0101(4) S5 0.0774(5) 0.0267(4) 0.0214(3) 0.0032(2) 0.0148(3) 0.0091(3) Co1 0.02522(14) 0.02196(17) 0.01935(14) 0.00142(11) 0.00183(11) -0.00154(11) Co2 0.02832(15) 0.02672(18) 0.01721(14) 0.00082(11) 0.00337(11) 0.00138(12) N1 0.0272(9) 0.0216(11) 0.0229(9) 0.0032(7) 0.0013(7) -0.0049(7) C1 0.0366(12) 0.0370(15) 0.0218(11) 0.0038(9) 0.0106(9) -0.0016(10) C2 0.0447(14) 0.0334(16) 0.0321(13) -0.0034(10) 0.0117(10) 0.0068(11) N2 0.0378(11) 0.0266(12) 0.0369(11) -0.0063(9) -0.0047(9) -0.0019(9) C5 0.0407(13) 0.0263(14) 0.0356(13) 0.0118(10) -0.0014(10) -0.0022(10) C6 0.0423(14) 0.0217(14) 0.0482(16) 0.0089(11) -0.0051(11) -0.0092(10) N3 0.0400(11) 0.0318(13) 0.0283(10) 0.0049(8) 0.0052(8) 0.0093(9) N4 0.0276(9) 0.0342(13) 0.0260(10) 0.0007(8) 0.0061(7) -0.0046(8) C3 0.0336(12) 0.0388(16) 0.0236(11) 0.0037(10) -0.0044(9) -0.0082(10) C4 0.0256(11) 0.0442(17) 0.0367(14) 0.0051(11) -0.0023(10) -0.0003(10) N6 0.0394(11) 0.0278(12) 0.0222(9) 0.0037(8) 0.0037(8) 0.0014(8) C7 0.0605(19) 0.0444(19) 0.0411(16) 0.0001(13) 0.0218(14) -0.0130(14) C8 0.0500(16) 0.0366(18) 0.0509(17) -0.0057(13) 0.0203(13) -0.0128(13) N7 0.0339(12) 0.066(2) 0.0411(14) -0.0047(12) 0.0058(10) 0.0135(11) C9 0.070(2) 0.049(2) 0.0367(16) 0.0132(13) -0.0033(14) 0.0227(16) C10 0.0398(15) 0.060(2) 0.0484(17) 0.0033(15) -0.0106(13) 0.0155(14) N5 0.0352(11) 0.0328(13) 0.0342(11) -0.0087(9) 0.0014(9) -0.0006(9) N8 0.0302(9) 0.0264(11) 0.0241(9) 0.0037(8) 0.0033(7) 0.0033(8) C11 0.0547(16) 0.0370(16) 0.0216(11) -0.0008(10) 0.0018(10) 0.0052(12) C12 0.0428(13) 0.0324(15) 0.0234(11) -0.0044(9) 0.0065(10) 0.0047(11) _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 S1 Co1 2.3540(8) . ? S1 Sb1 2.4294(8) . ? S2 Sb1 2.3621(8) . ? Sb1 S3 2.4916(7) . ? S3 Sb2 2.4761(8) . ? Sb2 S4 2.3327(10) . ? Sb2 S5 2.3935(8) . ? S5 Co2 2.3337(8) . ? Co1 N4 2.065(2) . ? Co1 N2 2.073(2) . ? Co1 N3 2.107(2) . ? Co1 N1 2.3181(19) . ? Co2 N7 2.067(2) . ? Co2 N8 2.076(2) . ? Co2 N5 2.094(2) . ? Co2 N6 2.268(2) . ? N1 C5 1.463(3) . ? N1 C1 1.469(3) . ? N1 C3 1.471(3) . ? C1 C2 1.503(4) . ? C2 N3 1.473(3) . ? N2 C6 1.487(4) . ? C5 C6 1.502(4) . ? N4 C4 1.471(3) . ? C3 C4 1.505(4) . ? N6 C9 1.459(4) . ? N6 C7 1.475(4) . ? N6 C11 1.475(3) . ? C7 C8 1.502(4) . ? C8 N5 1.470(4) . ? N7 C10 1.461(4) . ? C9 C10 1.507(5) . ? N8 C12 1.467(3) . ? C11 C12 1.489(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 Co1 S1 Sb1 101.84(3) . . ? S2 Sb1 S1 101.50(3) . . ? S2 Sb1 S3 99.02(4) . . ? S1 Sb1 S3 97.91(2) . . ? Sb2 S3 Sb1 101.00(3) . . ? S4 Sb2 S5 99.20(3) . . ? S4 Sb2 S3 103.65(3) . . ? S5 Sb2 S3 101.38(3) . . ? Co2 S5 Sb2 114.78(3) . . ? N4 Co1 N2 108.28(9) . . ? N4 Co1 N3 120.87(9) . . ? N2 Co1 N3 118.23(9) . . ? N4 Co1 N1 78.03(8) . . ? N2 Co1 N1 78.49(8) . . ? N3 Co1 N1 77.68(8) . . ? N4 Co1 S1 106.79(6) . . ? N2 Co1 S1 101.92(6) . . ? N3 Co1 S1 97.52(6) . . ? N1 Co1 S1 174.59(5) . . ? N7 Co2 N8 106.76(10) . . ? N7 Co2 N5 122.13(11) . . ? N8 Co2 N5 120.19(9) . . ? N7 Co2 N6 79.07(10) . . ? N8 Co2 N6 78.67(8) . . ? N5 Co2 N6 79.03(9) . . ? N7 Co2 S5 96.52(8) . . ? N8 Co2 S5 108.06(6) . . ? N5 Co2 S5 98.95(7) . . ? N6 Co2 S5 172.91(6) . . ? C5 N1 C1 112.54(19) . . ? C5 N1 C3 111.9(2) . . ? C1 N1 C3 111.3(2) . . ? C5 N1 Co1 107.43(14) . . ? C1 N1 Co1 107.14(14) . . ? C3 N1 Co1 106.03(14) . . ? N1 C1 C2 110.39(19) . . ? N3 C2 C1 107.6(2) . . ? C6 N2 Co1 111.58(16) . . ? N1 C5 C6 110.4(2) . . ? N2 C6 C5 108.9(2) . . ? C2 N3 Co1 111.87(16) . . ? C4 N4 Co1 114.93(15) . . ? N1 C3 C4 110.1(2) . . ? N4 C4 C3 108.0(2) . . ? C9 N6 C7 111.9(3) . . ? C9 N6 C11 111.6(2) . . ? C7 N6 C11 111.2(2) . . ? C9 N6 Co2 106.89(17) . . ? C7 N6 Co2 107.30(17) . . ? C11 N6 Co2 107.67(15) . . ? N6 C7 C8 110.6(2) . . ? N5 C8 C7 109.7(2) . . ? C10 N7 Co2 115.79(19) . . ? N6 C9 C10 111.4(3) . . ? N7 C10 C9 111.4(2) . . ? C8 N5 Co2 113.53(17) . . ? C12 N8 Co2 113.82(16) . . ? N6 C11 C12 111.2(2) . . ? N8 C12 C11 109.1(2) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.586 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.092 data_rs162 _database_code_CSD 161744 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 Co2 N8 S8 Sb4' _chemical_formula_weight 1153.83 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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.936(4) _cell_length_b 13.442(3) _cell_length_c 14.000(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.73(3) _cell_angle_gamma 90.00 _cell_volume 3305.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 4.729 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17807 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 30.03 _reflns_number_total 9659 _reflns_number_gt 7923 _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^)+(0.0235P)^2^+2.0734P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00076(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9659 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0550 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.060075(18) 0.36624(3) 0.88681(2) 0.02776(7) Uani 1 1 d . . . N1 N 1.09827(12) 0.36454(17) 1.03613(15) 0.0331(4) Uani 1 1 d . . . H2N1 H 1.0958 0.4269 1.0588 0.040 Uiso 1 1 calc R . . H1N1 H 1.0664 0.3266 1.0627 0.040 Uiso 1 1 calc R . . C1 C 1.17647(15) 0.3271(2) 1.06975(19) 0.0376(6) Uani 1 1 d . . . H1C H 1.1754 0.2554 1.0777 0.045 Uiso 1 1 calc R . . H1D H 1.1984 0.3562 1.1326 0.045 Uiso 1 1 calc R . . C2 C 1.22495(15) 0.3531(2) 0.9969(2) 0.0410(6) Uani 1 1 d . . . H2A H 1.2361 0.4237 1.0002 0.049 Uiso 1 1 calc R . . H2B H 1.2728 0.3172 1.0127 0.049 Uiso 1 1 calc R . . N2 N 1.18470(12) 0.32672(17) 0.89755(16) 0.0335(4) Uani 1 1 d . . . C3 C 1.21225(17) 0.3868(3) 0.8238(2) 0.0491(7) Uani 1 1 d . . . H3A H 1.1985 0.3544 0.7608 0.059 Uiso 1 1 calc R . . H3B H 1.2673 0.3913 0.8408 0.059 Uiso 1 1 calc R . . C4 C 1.17876(18) 0.4895(3) 0.8173(2) 0.0498(7) Uani 1 1 d . . . H4A H 1.1989 0.5263 0.8765 0.060 Uiso 1 1 calc R . . H4B H 1.1919 0.5249 0.7626 0.060 Uiso 1 1 calc R . . N3 N 1.09495(14) 0.48067(18) 0.80386(18) 0.0402(5) Uani 1 1 d . . . H2N3 H 1.0752 0.4696 0.7404 0.048 Uiso 1 1 calc R . . H1N3 H 1.0760 0.5388 0.8204 0.048 Uiso 1 1 calc R . . N4 N 1.05058(13) 0.22127(18) 0.83447(16) 0.0367(5) Uani 1 1 d . . . H2N4 H 1.0410 0.1805 0.8816 0.044 Uiso 1 1 calc R . . H1N4 H 1.0108 0.2175 0.7837 0.044 Uiso 1 1 calc R . . C5 C 1.11942(18) 0.1872(2) 0.8031(2) 0.0489(7) Uani 1 1 d . . . H5A H 1.1216 0.2157 0.7401 0.059 Uiso 1 1 calc R . . H5B H 1.1186 0.1153 0.7968 0.059 Uiso 1 1 calc R . . C6 C 1.18801(17) 0.2189(2) 0.8777(2) 0.0474(7) Uani 1 1 d . . . H6A H 1.1898 0.1820 0.9377 0.057 Uiso 1 1 calc R . . H6B H 1.2339 0.2041 0.8539 0.057 Uiso 1 1 calc R . . S1 S 0.93189(4) 0.41654(5) 0.85970(5) 0.03648(14) Uani 1 1 d . . . Sb1 Sb 0.858433(9) 0.320186(14) 0.950096(13) 0.03522(5) Uani 1 1 d . . . S2 S 0.87534(4) 0.15170(5) 0.88938(5) 0.03951(15) Uani 1 1 d . . . Sb2 Sb 0.935178(10) 0.085145(15) 1.049183(14) 0.03708(5) Uani 1 1 d . . . S4 S 0.93070(4) -0.08873(5) 0.94761(5) 0.03776(14) Uani 1 1 d . . . S3 S 0.93873(4) 0.28053(6) 1.10417(5) 0.04090(15) Uani 1 1 d . . . Co2 Co 0.569998(18) 0.36970(2) 0.61094(2) 0.02785(7) Uani 1 1 d . . . N5 N 0.57843(12) 0.48283(18) 0.71510(17) 0.0375(5) Uani 1 1 d . . . H2N5 H 0.5409 0.5273 0.6955 0.045 Uiso 1 1 calc R . . H1N5 H 0.5718 0.4565 0.7719 0.045 Uiso 1 1 calc R . . C11 C 0.65193(16) 0.5344(2) 0.7312(2) 0.0446(7) Uani 1 1 d . . . H11A H 0.6594 0.5719 0.7916 0.054 Uiso 1 1 calc R . . H11B H 0.6529 0.5806 0.6782 0.054 Uiso 1 1 calc R . . C12 C 0.71453(15) 0.4587(2) 0.7363(2) 0.0430(6) Uani 1 1 d . . . H12A H 0.7627 0.4925 0.7388 0.052 Uiso 1 1 calc R . . H12B H 0.7186 0.4195 0.7953 0.052 Uiso 1 1 calc R . . N7 N 0.69865(11) 0.39301(17) 0.65077(16) 0.0326(4) Uani 1 1 d . . . C7 C 0.73328(16) 0.2937(2) 0.6732(2) 0.0450(7) Uani 1 1 d . . . H7A H 0.7833 0.3007 0.7148 0.054 Uiso 1 1 calc R . . H7B H 0.7392 0.2613 0.6133 0.054 Uiso 1 1 calc R . . C8 C 0.68353(17) 0.2313(2) 0.7238(2) 0.0484(7) Uani 1 1 d . . . H8A H 0.7031 0.1639 0.7319 0.058 Uiso 1 1 calc R . . H8B H 0.6832 0.2586 0.7878 0.058 Uiso 1 1 calc R . . N8 N 0.60577(13) 0.23077(18) 0.66440(19) 0.0423(5) Uani 1 1 d . . . H2N8 H 0.5735 0.2080 0.7009 0.051 Uiso 1 1 calc R . . H1N8 H 0.6039 0.1886 0.6140 0.051 Uiso 1 1 calc R . . N6 N 0.59391(13) 0.40230(19) 0.47480(16) 0.0388(5) Uani 1 1 d . . . H2N6 H 0.5674 0.3605 0.4303 0.047 Uiso 1 1 calc R . . H1N6 H 0.5781 0.4646 0.4579 0.047 Uiso 1 1 calc R . . C10 C 0.72027(16) 0.4385(3) 0.5641(2) 0.0500(8) Uani 1 1 d . . . H10A H 0.7742 0.4280 0.5668 0.060 Uiso 1 1 calc R . . H10B H 0.7111 0.5096 0.5642 0.060 Uiso 1 1 calc R . . C9 C 0.67541(18) 0.3940(3) 0.4725(2) 0.0529(8) Uani 1 1 d . . . H9A H 0.6861 0.4291 0.4162 0.064 Uiso 1 1 calc R . . H9B H 0.6892 0.3247 0.4677 0.064 Uiso 1 1 calc R . . S5 S 0.43804(4) 0.34952(5) 0.55137(4) 0.03374(13) Uani 1 1 d . . . Sb3 Sb 0.380935(10) 0.321888(14) 0.688174(13) 0.03498(5) Uani 1 1 d . . . S7 S 0.40026(4) 0.48226(5) 0.77553(4) 0.03157(12) Uani 1 1 d . . . Sb4 Sb 0.448360(11) 0.394322(15) 0.932360(12) 0.03627(5) Uani 1 1 d . . . S6 S 0.47873(6) 0.24699(6) 0.80837(6) 0.0527(2) Uani 1 1 d . . . S8 S 0.58056(4) 0.43741(6) 0.97049(5) 0.04391(16) 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 Co1 0.02770(15) 0.03074(16) 0.02437(14) 0.00043(12) 0.00420(12) 0.00285(12) N1 0.0336(10) 0.0387(12) 0.0274(10) -0.0035(9) 0.0070(8) -0.0005(9) C1 0.0315(12) 0.0491(16) 0.0299(12) 0.0038(11) 0.0006(10) -0.0020(11) C2 0.0286(12) 0.0537(17) 0.0386(14) 0.0069(12) 0.0018(10) -0.0038(11) N2 0.0306(10) 0.0411(12) 0.0299(10) 0.0045(9) 0.0091(8) 0.0040(9) C3 0.0381(14) 0.071(2) 0.0427(15) 0.0143(15) 0.0191(12) 0.0016(14) C4 0.0483(16) 0.0561(19) 0.0455(16) 0.0178(14) 0.0105(13) -0.0092(14) N3 0.0455(12) 0.0378(12) 0.0371(12) 0.0087(10) 0.0080(10) 0.0027(10) N4 0.0387(11) 0.0392(12) 0.0313(10) -0.0051(9) 0.0049(9) -0.0007(10) C5 0.0582(19) 0.0448(17) 0.0473(17) -0.0135(13) 0.0192(15) 0.0037(14) C6 0.0428(15) 0.0479(17) 0.0546(18) -0.0009(14) 0.0171(14) 0.0153(13) S1 0.0313(3) 0.0342(3) 0.0415(3) 0.0035(3) 0.0017(3) 0.0069(2) Sb1 0.02568(8) 0.03907(10) 0.03940(9) -0.00028(7) 0.00304(6) 0.00606(6) S2 0.0412(3) 0.0362(3) 0.0356(3) -0.0021(3) -0.0052(3) 0.0005(3) Sb2 0.02981(8) 0.04263(10) 0.03824(9) 0.01135(7) 0.00560(7) -0.00272(7) S4 0.0281(3) 0.0355(3) 0.0467(4) 0.0064(3) 0.0006(3) -0.0039(2) S3 0.0437(4) 0.0466(4) 0.0302(3) -0.0040(3) 0.0025(3) 0.0012(3) Co2 0.02633(14) 0.02835(16) 0.02743(15) -0.00010(12) 0.00204(12) 0.00192(12) N5 0.0310(10) 0.0431(13) 0.0375(11) -0.0085(10) 0.0050(9) 0.0035(9) C11 0.0400(14) 0.0354(14) 0.0551(18) -0.0099(13) 0.0014(13) -0.0042(11) C12 0.0295(12) 0.0439(16) 0.0491(16) -0.0076(13) -0.0074(11) -0.0026(11) N7 0.0260(9) 0.0356(11) 0.0347(11) 0.0011(9) 0.0027(8) 0.0021(8) C7 0.0336(13) 0.0474(16) 0.0508(16) -0.0043(13) 0.0008(12) 0.0152(12) C8 0.0498(16) 0.0362(15) 0.0518(17) 0.0090(13) -0.0069(14) 0.0094(13) N8 0.0398(12) 0.0335(12) 0.0502(14) 0.0054(10) 0.0012(10) 0.0006(10) N6 0.0411(12) 0.0440(13) 0.0291(11) 0.0013(9) 0.0019(9) -0.0022(10) C10 0.0316(13) 0.068(2) 0.0530(18) 0.0110(16) 0.0151(13) -0.0031(14) C9 0.0487(17) 0.075(2) 0.0391(15) 0.0079(15) 0.0180(13) 0.0119(16) S5 0.0304(3) 0.0427(3) 0.0263(3) -0.0046(2) 0.0015(2) 0.0007(2) Sb3 0.03385(8) 0.03616(9) 0.03561(9) -0.00798(7) 0.00865(7) -0.01124(7) S7 0.0359(3) 0.0283(3) 0.0292(3) -0.0002(2) 0.0034(2) 0.0034(2) Sb4 0.03987(9) 0.04195(10) 0.02741(8) 0.00500(7) 0.00782(7) 0.00339(7) S6 0.0832(6) 0.0367(4) 0.0375(4) 0.0044(3) 0.0104(4) 0.0186(4) S8 0.0365(3) 0.0588(5) 0.0343(3) -0.0066(3) 0.0023(3) 0.0110(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 Co1 N1 2.063(2) . ? Co1 N4 2.077(2) . ? Co1 N3 2.098(2) . ? Co1 N2 2.273(2) . ? Co1 S1 2.3521(9) . ? N1 C1 1.475(3) . ? C1 C2 1.509(4) . ? C2 N2 1.474(4) . ? N2 C3 1.473(3) . ? N2 C6 1.479(4) . ? C3 C4 1.501(5) . ? C4 N3 1.481(4) . ? N4 C5 1.465(4) . ? C5 C6 1.505(5) . ? S1 Sb1 2.3860(9) . ? Sb1 S3 2.3976(10) . ? Sb1 S2 2.4595(9) . ? S2 Sb2 2.4457(10) . ? Sb2 S4 2.3973(8) 3_757 ? Sb2 S4 2.7285(9) . ? Sb2 S3 2.7340(9) . ? S4 Sb2 2.3973(8) 3_757 ? Co2 N8 2.065(2) . ? Co2 N6 2.083(2) . ? Co2 N5 2.091(2) . ? Co2 N7 2.283(2) . ? Co2 S5 2.3598(9) . ? N5 C11 1.466(4) . ? C11 C12 1.506(4) . ? C12 N7 1.469(4) . ? N7 C10 1.479(4) . ? N7 C7 1.479(4) . ? C7 C8 1.502(5) . ? C8 N8 1.471(4) . ? N6 C9 1.473(4) . ? C10 C9 1.494(5) . ? S5 Sb3 2.3775(9) . ? Sb3 S6 2.3921(11) . ? Sb3 S7 2.4680(8) . ? S7 Sb4 2.4885(8) . ? Sb4 S8 2.3934(9) . ? Sb4 S8 2.7427(9) 3_667 ? Sb4 S6 2.7599(9) . ? S8 Sb4 2.7427(9) 3_667 ? 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 Co1 N4 109.49(9) . . ? N1 Co1 N3 119.60(10) . . ? N4 Co1 N3 120.33(10) . . ? N1 Co1 N2 79.10(9) . . ? N4 Co1 N2 79.22(9) . . ? N3 Co1 N2 78.94(9) . . ? N1 Co1 S1 106.20(7) . . ? N4 Co1 S1 101.86(7) . . ? N3 Co1 S1 95.25(7) . . ? N2 Co1 S1 173.66(6) . . ? C1 N1 Co1 115.19(16) . . ? N1 C1 C2 110.3(2) . . ? N2 C2 C1 110.1(2) . . ? C3 N2 C2 111.1(2) . . ? C3 N2 C6 111.9(2) . . ? C2 N2 C6 112.4(2) . . ? C3 N2 Co1 106.93(17) . . ? C2 N2 Co1 107.02(16) . . ? C6 N2 Co1 107.05(17) . . ? N2 C3 C4 111.1(2) . . ? N3 C4 C3 108.5(3) . . ? C4 N3 Co1 113.42(18) . . ? C5 N4 Co1 112.68(18) . . ? N4 C5 C6 108.9(2) . . ? N2 C6 C5 110.5(2) . . ? Co1 S1 Sb1 112.66(3) . . ? S1 Sb1 S3 107.60(3) . . ? S1 Sb1 S2 101.33(3) . . ? S3 Sb1 S2 90.71(3) . . ? Sb2 S2 Sb1 94.74(3) . . ? S4 Sb2 S2 105.18(4) 3_757 . ? S4 Sb2 S4 87.14(3) 3_757 . ? S2 Sb2 S4 82.86(3) . . ? S4 Sb2 S3 90.55(3) 3_757 . ? S2 Sb2 S3 83.51(3) . . ? S4 Sb2 S3 165.05(2) . . ? Sb2 S4 Sb2 92.86(3) 3_757 . ? Sb1 S3 Sb2 89.14(2) . . ? N8 Co2 N6 114.53(10) . . ? N8 Co2 N5 115.59(10) . . ? N6 Co2 N5 119.07(10) . . ? N8 Co2 N7 79.13(9) . . ? N6 Co2 N7 78.98(9) . . ? N5 Co2 N7 78.67(8) . . ? N8 Co2 S5 103.86(7) . . ? N6 Co2 S5 94.53(7) . . ? N5 Co2 S5 104.79(7) . . ? N7 Co2 S5 173.51(6) . . ? C11 N5 Co2 112.73(18) . . ? N5 C11 C12 109.0(2) . . ? N7 C12 C11 110.4(2) . . ? C12 N7 C10 112.4(2) . . ? C12 N7 C7 111.5(2) . . ? C10 N7 C7 112.2(2) . . ? C12 N7 Co2 107.50(16) . . ? C10 N7 Co2 106.08(16) . . ? C7 N7 Co2 106.74(17) . . ? N7 C7 C8 109.9(2) . . ? N8 C8 C7 108.8(2) . . ? C8 N8 Co2 112.90(18) . . ? C9 N6 Co2 113.22(18) . . ? N7 C10 C9 110.7(3) . . ? N6 C9 C10 108.3(2) . . ? Co2 S5 Sb3 107.37(3) . . ? S5 Sb3 S6 104.96(3) . . ? S5 Sb3 S7 102.86(2) . . ? S6 Sb3 S7 90.57(3) . . ? Sb3 S7 Sb4 90.62(3) . . ? S8 Sb4 S7 103.41(4) . . ? S8 Sb4 S8 88.19(3) . 3_667 ? S7 Sb4 S8 88.81(3) . 3_667 ? S8 Sb4 S6 90.04(3) . . ? S7 Sb4 S6 82.14(3) . . ? S8 Sb4 S6 170.12(2) 3_667 . ? Sb3 S6 Sb4 86.00(3) . . ? Sb4 S8 Sb4 91.81(3) . 3_667 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.248 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.088