Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Hope-Weeks, Louisa J.' 'Mays, Martin J.' 'Woods, Anthony D.' _publ_contact_author_name 'Dr Martin J Mays' _publ_contact_author_address ; Chemistry University of Cambridge Lensfield Road Cambridge Cambridgeshire CB2 1EW UNITED KINGDOM ; _publ_contact_author_email 'MJM14@CUS.CAM.AC.UK' _publ_section_title ; Synthesis of thio and mixed donor atom macrocycles containing coordinate diyne ligands ; data_mm9931 #COMPLEX 7 _database_code_CSD 172436 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H24 Co8 O24 S4' _chemical_formula_weight 1536.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4440(10) _cell_length_b 10.9660(7) _cell_length_c 14.3500(9) _cell_angle_alpha 105.700(3) _cell_angle_beta 90.290(4) _cell_angle_gamma 101.800(4) _cell_volume 1397.57(19) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 37443 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.03 _exptl_crystal_description Block _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 2.541 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.6577 _exptl_absorpt_correction_T_max 0.7852 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _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 CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9804 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.11 _reflns_number_total 4943 _reflns_number_gt 3355 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1991)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0613P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4943 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Co1 Co 0.46981(7) 0.75306(7) 0.14889(5) 0.0337(2) Uani 1 1 d . . . S1 S 0.57316(15) 0.68717(14) 0.69094(12) 0.0480(4) Uani 1 1 d . . . O1 O 0.6991(4) 0.9698(4) 0.2556(3) 0.0617(12) Uani 1 1 d . . . C1 C 0.6116(6) 0.8865(6) 0.2134(4) 0.0413(13) Uani 1 1 d . . . Co2 Co 0.12543(7) 1.00628(7) 0.17205(5) 0.0376(2) Uani 1 1 d . . . S2 S 0.23004(17) 0.71535(15) 0.42802(11) 0.0505(4) Uani 1 1 d . . . O2 O 0.6255(4) 0.5386(4) 0.1152(3) 0.0553(11) Uani 1 1 d . . . C2 C 0.5665(6) 0.6221(5) 0.1280(4) 0.0405(13) Uani 1 1 d . . . Co3 Co 0.22093(7) 0.62463(6) 0.14345(5) 0.0339(2) Uani 1 1 d . . . C3 C 0.4626(6) 0.7846(5) 0.0303(5) 0.0431(14) Uani 1 1 d . . . O3 O 0.4547(5) 0.8044(5) -0.0427(3) 0.0635(12) Uani 1 1 d . . . Co4 Co 0.14713(7) 1.01668(7) 0.34568(5) 0.0361(2) Uani 1 1 d . . . O4 O 0.1104(5) 0.6588(4) -0.0381(3) 0.0634(12) Uani 1 1 d . . . C4 C 0.1509(6) 0.6419(5) 0.0301(4) 0.0430(14) Uani 1 1 d . . . O5 O 0.2873(4) 0.3631(4) 0.0881(3) 0.0574(11) Uani 1 1 d . . . C5 C 0.2611(5) 0.4632(6) 0.1104(4) 0.0401(13) Uani 1 1 d . . . O6 O -0.0527(4) 0.5604(4) 0.2336(3) 0.0646(13) Uani 1 1 d . . . C6 C 0.0545(6) 0.5869(5) 0.2013(4) 0.0439(14) Uani 1 1 d . . . O7 O -0.1228(4) 0.7850(4) 0.1101(3) 0.0618(12) Uani 1 1 d . . . C7 C -0.0312(6) 0.8722(6) 0.1328(4) 0.0441(14) Uani 1 1 d . . . O8 O 0.2525(5) 0.9983(5) -0.0148(3) 0.0683(13) Uani 1 1 d . . . C8 C 0.2055(6) 1.0016(6) 0.0570(5) 0.0469(14) Uani 1 1 d . . . C9 C 0.0581(7) 1.1547(6) 0.1868(4) 0.0521(15) Uani 1 1 d . . . O9 O 0.0155(5) 1.2466(5) 0.1993(4) 0.0782(14) Uani 1 1 d . . . O10 O 0.3439(5) 1.0394(4) 0.5108(3) 0.0688(13) Uani 1 1 d . . . C10 C 0.2663(6) 1.0276(5) 0.4485(4) 0.0455(14) Uani 1 1 d . . . O11 O -0.1071(4) 0.8153(4) 0.3612(3) 0.0578(11) Uani 1 1 d . . . C11 C -0.0093(6) 0.8916(6) 0.3559(4) 0.0415(13) Uani 1 1 d . . . C12 C 0.0826(6) 1.1659(6) 0.3960(4) 0.0480(15) Uani 1 1 d . . . O12 O 0.0423(5) 1.2578(4) 0.4261(3) 0.0671(13) Uani 1 1 d . . . C20 C 0.2986(5) 1.0551(5) 0.2592(4) 0.0337(12) Uani 1 1 d . . . C21 C 0.2488(5) 0.9251(5) 0.2374(4) 0.0338(12) Uani 1 1 d . . . C22 C 0.2991(5) 0.8068(5) 0.2139(3) 0.0291(11) Uani 1 1 d . . . C23 C 0.3512(5) 0.7266(5) 0.2555(3) 0.0305(11) Uani 1 1 d . . . C24 C 0.3859(6) 0.7155(6) 0.3543(4) 0.0455(14) Uani 1 1 d . . . H24A H 0.4653 0.7891 0.3874 0.055 Uiso 1 1 calc R . . H24B H 0.4203 0.6344 0.3477 0.055 Uiso 1 1 calc R . . C25 C 0.2012(6) 0.5543(5) 0.4430(4) 0.0466(14) Uani 1 1 d . . . H25A H 0.0998 0.5291 0.4597 0.056 Uiso 1 1 calc R . . H25B H 0.2137 0.4932 0.3803 0.056 Uiso 1 1 calc R . . C26 C 0.3020(6) 0.5403(5) 0.5203(4) 0.0454(14) Uani 1 1 d . . . H26A H 0.4035 0.5704 0.5058 0.054 Uiso 1 1 calc R . . H26B H 0.2882 0.4474 0.5175 0.054 Uiso 1 1 calc R . . C27 C 0.2781(6) 0.6160(5) 0.6225(4) 0.0430(13) Uani 1 1 d . . . H27A H 0.1785 0.5822 0.6386 0.052 Uiso 1 1 calc R . . H27B H 0.2860 0.7081 0.6244 0.052 Uiso 1 1 calc R . . C28 C 0.3856(6) 0.6084(6) 0.6994(4) 0.0484(15) Uani 1 1 d . . . H28A H 0.3818 0.5159 0.6945 0.058 Uiso 1 1 calc R . . H28B H 0.3544 0.6484 0.7643 0.058 Uiso 1 1 calc R . . C29 C 0.5581(5) 0.8548(5) 0.7295(4) 0.0358(12) Uani 1 1 d . . . H29A H 0.4951 0.8716 0.6811 0.054 Uiso 1 1 calc R . . H29B H 0.5118 0.8712 0.7921 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0300(4) 0.0362(4) 0.0338(4) 0.0083(3) 0.0062(3) 0.0065(3) S1 0.0432(8) 0.0332(8) 0.0644(10) 0.0083(7) -0.0065(7) 0.0086(6) O1 0.036(2) 0.049(3) 0.082(3) -0.008(2) -0.004(2) 0.005(2) C1 0.031(3) 0.039(3) 0.053(4) 0.008(3) 0.006(3) 0.012(3) Co2 0.0340(4) 0.0388(4) 0.0412(4) 0.0130(4) 0.0002(3) 0.0076(3) S2 0.0607(9) 0.0596(10) 0.0450(9) 0.0270(8) 0.0186(7) 0.0272(8) O2 0.056(2) 0.054(3) 0.063(3) 0.019(2) 0.015(2) 0.024(2) C2 0.042(3) 0.045(4) 0.036(3) 0.012(3) 0.013(3) 0.012(3) Co3 0.0327(4) 0.0314(4) 0.0341(4) 0.0056(3) 0.0037(3) 0.0038(3) C3 0.037(3) 0.042(3) 0.051(4) 0.015(3) 0.008(3) 0.005(3) O3 0.067(3) 0.086(3) 0.045(3) 0.030(3) 0.008(2) 0.016(2) Co4 0.0353(4) 0.0351(4) 0.0375(4) 0.0069(3) 0.0063(3) 0.0102(3) O4 0.074(3) 0.070(3) 0.044(3) 0.017(2) -0.017(2) 0.008(2) C4 0.035(3) 0.041(3) 0.045(4) 0.002(3) 0.003(3) 0.003(3) O5 0.071(3) 0.038(2) 0.062(3) 0.007(2) 0.007(2) 0.017(2) C5 0.036(3) 0.040(4) 0.038(3) 0.005(3) 0.004(2) 0.004(3) O6 0.044(2) 0.063(3) 0.073(3) 0.007(2) 0.019(2) -0.004(2) C6 0.040(3) 0.036(3) 0.044(3) -0.001(3) -0.003(3) -0.002(3) O7 0.037(2) 0.057(3) 0.079(3) 0.006(2) -0.002(2) -0.001(2) C7 0.035(3) 0.053(4) 0.047(4) 0.014(3) 0.002(3) 0.015(3) O8 0.071(3) 0.089(4) 0.052(3) 0.034(3) 0.013(2) 0.014(3) C8 0.041(3) 0.054(4) 0.050(4) 0.023(3) -0.005(3) 0.009(3) C9 0.058(4) 0.050(4) 0.051(4) 0.015(3) -0.004(3) 0.015(3) O9 0.099(4) 0.066(3) 0.087(4) 0.032(3) 0.003(3) 0.044(3) O10 0.069(3) 0.075(3) 0.053(3) 0.002(2) -0.021(3) 0.015(2) C10 0.043(3) 0.042(4) 0.046(4) 0.000(3) 0.004(3) 0.012(3) O11 0.045(2) 0.059(3) 0.070(3) 0.022(2) 0.018(2) 0.004(2) C11 0.045(3) 0.048(4) 0.036(3) 0.011(3) 0.011(3) 0.021(3) C12 0.051(4) 0.038(4) 0.053(4) 0.012(3) 0.015(3) 0.007(3) O12 0.076(3) 0.044(3) 0.088(3) 0.016(2) 0.033(3) 0.030(2) C20 0.033(3) 0.032(3) 0.034(3) 0.007(2) 0.001(2) 0.004(2) C21 0.030(3) 0.039(3) 0.032(3) 0.010(2) 0.001(2) 0.006(2) C22 0.026(3) 0.029(3) 0.029(3) 0.005(2) 0.006(2) 0.003(2) C23 0.027(3) 0.033(3) 0.027(3) 0.005(2) 0.002(2) 0.001(2) C24 0.042(3) 0.061(4) 0.039(3) 0.021(3) 0.006(3) 0.013(3) C25 0.048(3) 0.048(4) 0.041(3) 0.011(3) 0.002(3) 0.005(3) C26 0.051(3) 0.038(3) 0.044(4) 0.009(3) -0.001(3) 0.005(3) C27 0.038(3) 0.045(3) 0.046(3) 0.019(3) 0.004(3) -0.001(3) C28 0.054(4) 0.044(4) 0.046(4) 0.021(3) -0.006(3) -0.006(3) C29 0.037(3) 0.030(3) 0.039(3) 0.007(2) 0.003(2) 0.006(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 Co1 C1 1.801(6) . ? Co1 C2 1.814(6) . ? Co1 C3 1.830(6) . ? Co1 C23 1.951(5) . ? Co1 C22 1.981(4) . ? Co1 Co3 2.4696(10) . ? S1 C29 1.806(5) . ? S1 C28 1.825(6) . ? O1 C1 1.127(6) . ? Co2 C8 1.812(7) . ? Co2 C7 1.823(6) . ? Co2 C9 1.827(6) . ? Co2 C20 1.946(5) . ? Co2 C21 1.973(5) . ? Co2 Co4 2.4686(10) . ? S2 C25 1.802(6) . ? S2 C24 1.818(5) . ? O2 C2 1.141(6) . ? Co3 C6 1.806(6) . ? Co3 C5 1.823(6) . ? Co3 C4 1.824(7) . ? Co3 C23 1.948(5) . ? Co3 C22 1.963(5) . ? C3 O3 1.131(6) . ? Co4 C10 1.814(7) . ? Co4 C12 1.828(6) . ? Co4 C11 1.834(6) . ? Co4 C20 1.954(5) . ? Co4 C21 1.977(5) . ? O4 C4 1.124(6) . ? O5 C5 1.136(6) . ? O6 C6 1.133(6) . ? O7 C7 1.122(6) . ? O8 C8 1.118(6) . ? C9 O9 1.130(7) . ? O10 C10 1.115(6) . ? O11 C11 1.132(6) . ? C12 O12 1.127(6) . ? C20 C21 1.353(7) . ? C20 C29 1.482(7) 2_676 ? C21 C22 1.428(7) . ? C22 C23 1.354(7) . ? C23 C24 1.494(7) . ? C25 C26 1.518(7) . ? C26 C27 1.521(7) . ? C27 C28 1.527(7) . ? C29 C20 1.482(7) 2_676 ? 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 C1 Co1 C2 99.8(2) . . ? C1 Co1 C3 101.1(3) . . ? C2 Co1 C3 103.2(2) . . ? C1 Co1 C23 100.4(2) . . ? C2 Co1 C23 102.7(2) . . ? C3 Co1 C23 142.7(2) . . ? C1 Co1 C22 100.2(2) . . ? C2 Co1 C22 140.7(2) . . ? C3 Co1 C22 105.7(2) . . ? C23 Co1 C22 40.28(19) . . ? C1 Co1 Co3 148.61(17) . . ? C2 Co1 Co3 98.68(17) . . ? C3 Co1 Co3 99.04(17) . . ? C23 Co1 Co3 50.66(14) . . ? C22 Co1 Co3 50.92(14) . . ? C29 S1 C28 99.7(2) . . ? O1 C1 Co1 178.5(5) . . ? C8 Co2 C7 100.1(3) . . ? C8 Co2 C9 97.8(3) . . ? C7 Co2 C9 106.4(3) . . ? C8 Co2 C20 100.7(2) . . ? C7 Co2 C20 138.7(2) . . ? C9 Co2 C20 105.7(2) . . ? C8 Co2 C21 103.7(2) . . ? C7 Co2 C21 99.8(2) . . ? C9 Co2 C21 142.4(2) . . ? C20 Co2 C21 40.4(2) . . ? C8 Co2 Co4 150.74(18) . . ? C7 Co2 Co4 99.59(18) . . ? C9 Co2 Co4 97.22(19) . . ? C20 Co2 Co4 50.88(14) . . ? C21 Co2 Co4 51.41(14) . . ? C25 S2 C24 100.7(3) . . ? O2 C2 Co1 178.9(5) . . ? C6 Co3 C5 98.0(2) . . ? C6 Co3 C4 100.8(2) . . ? C5 Co3 C4 104.3(2) . . ? C6 Co3 C23 100.8(2) . . ? C5 Co3 C23 106.4(2) . . ? C4 Co3 C23 139.2(2) . . ? C6 Co3 C22 102.6(2) . . ? C5 Co3 C22 143.7(2) . . ? C4 Co3 C22 100.9(2) . . ? C23 Co3 C22 40.50(19) . . ? C6 Co3 Co1 150.36(17) . . ? C5 Co3 Co1 98.59(16) . . ? C4 Co3 Co1 98.69(17) . . ? C23 Co3 Co1 50.74(14) . . ? C22 Co3 Co1 51.55(13) . . ? O3 C3 Co1 178.3(5) . . ? C10 Co4 C12 98.0(3) . . ? C10 Co4 C11 102.3(3) . . ? C12 Co4 C11 102.1(2) . . ? C10 Co4 C20 97.0(2) . . ? C12 Co4 C20 107.1(2) . . ? C11 Co4 C20 142.2(2) . . ? C10 Co4 C21 100.8(2) . . ? C12 Co4 C21 143.9(2) . . ? C11 Co4 C21 103.6(2) . . ? C20 Co4 C21 40.3(2) . . ? C10 Co4 Co2 146.80(17) . . ? C12 Co4 Co2 98.77(19) . . ? C11 Co4 Co2 101.93(17) . . ? C20 Co4 Co2 50.58(15) . . ? C21 Co4 Co2 51.24(14) . . ? O4 C4 Co3 176.6(5) . . ? O5 C5 Co3 178.6(5) . . ? O6 C6 Co3 177.0(5) . . ? O7 C7 Co2 175.8(5) . . ? O8 C8 Co2 178.7(5) . . ? O9 C9 Co2 177.5(6) . . ? O10 C10 Co4 176.6(6) . . ? O11 C11 Co4 178.8(5) . . ? O12 C12 Co4 179.3(6) . . ? C21 C20 C29 136.6(4) . 2_676 ? C21 C20 Co2 70.9(3) . . ? C29 C20 Co2 136.7(4) 2_676 . ? C21 C20 Co4 70.8(3) . . ? C29 C20 Co4 135.5(4) 2_676 . ? Co2 C20 Co4 78.55(18) . . ? C20 C21 C22 141.1(4) . . ? C20 C21 Co2 68.7(3) . . ? C22 C21 Co2 136.2(4) . . ? C20 C21 Co4 68.9(3) . . ? C22 C21 Co4 135.2(4) . . ? Co2 C21 Co4 77.35(17) . . ? C23 C22 C21 141.8(5) . . ? C23 C22 Co3 69.2(3) . . ? C21 C22 Co3 136.8(4) . . ? C23 C22 Co1 68.7(3) . . ? C21 C22 Co1 133.7(4) . . ? Co3 C22 Co1 77.53(17) . . ? C22 C23 C24 139.5(5) . . ? C22 C23 Co3 70.3(3) . . ? C24 C23 Co3 136.6(4) . . ? C22 C23 Co1 71.1(3) . . ? C24 C23 Co1 133.2(3) . . ? Co3 C23 Co1 78.60(18) . . ? C23 C24 S2 112.2(4) . . ? C26 C25 S2 114.3(4) . . ? C25 C26 C27 113.6(5) . . ? C26 C27 C28 113.4(5) . . ? C27 C28 S1 114.9(4) . . ? C20 C29 S1 112.0(3) 2_676 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.678 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.227 #===END data_mm0023 #DATA FOR COMPLEX 10 _database_code_CSD 172437 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H8 Co4 O12 S2' _chemical_formula_weight 788.14 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' 'Co' 'Co' 0.3494 0.9721 '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 13.1458(2) _cell_length_b 16.0321(4) _cell_length_c 16.5151(4) _cell_angle_alpha 61.743(2) _cell_angle_beta 68.506(2) _cell_angle_gamma 88.404(2) _cell_volume 2807.26(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.865 _exptl_crystal_density_method ? _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 2.533 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 1.173 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device NoniusKappaCCD _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33397 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.46 _reflns_number_total 12637 _reflns_number_observed 9143 _reflns_observed_criterion >2sigma(I) _computing_data_collection maXus _computing_cell_refinement maXus _computing_data_reduction maXus _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 29 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0383P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12608 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_obs 0.0398 _refine_ls_wR_factor_all 0.1194 _refine_ls_wR_factor_obs 0.0835 _refine_ls_goodness_of_fit_all 1.011 _refine_ls_goodness_of_fit_obs 1.060 _refine_ls_restrained_S_all 1.276 _refine_ls_restrained_S_obs 1.060 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1_1 Co 1.00076(3) 0.79235(3) -0.37420(3) 0.02549(10) Uani 1 d . . Co2_1 Co 0.80641(3) 0.79390(3) -0.27755(3) 0.02557(10) Uani 1 d . . Co3_1 Co 0.71854(3) 0.48975(3) -0.15778(3) 0.02943(11) Uani 1 d . . Co4_1 Co 0.86838(3) 0.52350(3) -0.31717(3) 0.03591(12) Uani 1 d . . S1_1 S 0.85496(6) 0.71702(6) -0.03763(6) 0.0355(2) Uani 1 d . . S2_1 S 0.88408(8) 0.35857(6) -0.00727(7) 0.0471(2) Uani 1 d . . C1_1 C 1.1228(2) 0.7392(2) -0.3776(2) 0.0321(7) Uani 1 d . . O1_1 O 1.1996(2) 0.7047(2) -0.3788(2) 0.0522(7) Uani 1 d . . C2_1 C 1.0588(2) 0.9140(2) -0.4143(2) 0.0361(8) Uani 1 d . . O2_1 O 1.0933(2) 0.9881(2) -0.4337(2) 0.0537(7) Uani 1 d . . C3_1 C 0.9932(2) 0.7996(2) -0.4860(2) 0.0343(8) Uani 1 d . . O3_1 O 0.9909(2) 0.8023(2) -0.5550(2) 0.0530(7) Uani 1 d . . C4_1 C 0.8229(2) 0.9121(3) -0.2891(3) 0.0375(8) Uani 1 d . . O4_1 O 0.8350(2) 0.9834(2) -0.2931(2) 0.0663(8) Uani 1 d . . C5_1 C 0.7458(2) 0.8078(2) -0.3652(2) 0.0330(7) Uani 1 d . . O5_1 O 0.7074(2) 0.8168(2) -0.4192(2) 0.0524(7) Uani 1 d . . C6_1 C 0.6820(3) 0.7389(2) -0.1631(2) 0.0361(8) Uani 1 d . . O6_1 O 0.6029(2) 0.7061(2) -0.0921(2) 0.0577(7) Uani 1 d . . C7_1 C 0.6227(2) 0.5524(2) -0.2130(2) 0.0381(8) Uani 1 d . . O7_1 O 0.5678(2) 0.5949(2) -0.2509(2) 0.0560(7) Uani 1 d . . C8_1 C 0.6719(3) 0.3612(3) -0.1004(3) 0.0432(9) Uani 1 d . . O8_1 O 0.6462(2) 0.2807(2) -0.0629(2) 0.0654(8) Uani 1 d . . C9_1 C 0.6544(2) 0.4928(2) -0.0427(3) 0.0374(8) Uani 1 d . . O9_1 O 0.6065(2) 0.4921(2) 0.0308(2) 0.0543(7) Uani 1 d . . C10_1 C 1.0141(3) 0.5539(3) -0.3961(3) 0.0573(11) Uani 1 d . . O10_1 O 1.1058(2) 0.5714(3) -0.4447(3) 0.0949(12) Uani 1 d . . C11_1 C 0.8114(3) 0.5985(3) -0.4082(3) 0.0485(10) Uani 1 d . . O11_1 O 0.7747(3) 0.6427(2) -0.4650(2) 0.0738(9) Uani 1 d . . C12_1 C 0.8388(3) 0.4072(3) -0.3047(3) 0.0487(9) Uani 1 d . . O12_1 O 0.8181(3) 0.3353(2) -0.2970(2) 0.0765(9) Uani 1 d . . C13_1 C 0.9522(2) 0.4401(2) -0.1416(3) 0.0377(8) Uani 1 d . . H13A_1 H 1.0123(2) 0.4862(2) -0.1542(3) 0.045 Uiso 1 calc R . H13B_1 H 0.9873(2) 0.4023(2) -0.1741(3) 0.045 Uiso 1 calc R . C14_1 C 0.8784(2) 0.4962(2) -0.1910(2) 0.0282(7) Uani 1 d . . C15_1 C 0.8571(2) 0.5863(2) -0.2351(2) 0.0257(6) Uani 1 d . . C16_1 C 0.8849(2) 0.6826(2) -0.2577(2) 0.0241(6) Uani 1 d . . C17_1 C 0.9201(2) 0.7389(2) -0.2295(2) 0.0222(6) Uani 1 d . . C18_1 C 0.9604(2) 0.7454(2) -0.1584(2) 0.0274(7) Uani 1 d . . H18A_1 H 1.0008(2) 0.8116(2) -0.1910(2) 0.033 Uiso 1 calc R . H18B_1 H 1.0143(2) 0.7013(2) -0.1474(2) 0.033 Uiso 1 calc R . C19_1 C 0.8301(2) 0.5904(2) 0.0301(2) 0.0302(7) Uani 1 d . . C20_1 C 0.8709(2) 0.5344(2) -0.0137(2) 0.0294(7) Uani 1 d . . H20_1 H 0.9180(2) 0.5643(2) -0.0831(2) 0.035 Uiso 1 calc R . C21_1 C 0.8434(2) 0.4346(2) 0.0433(2) 0.0364(8) Uani 1 d . . C22_1 C 0.7771(3) 0.3913(3) 0.1462(3) 0.0485(10) Uani 1 d . . H22_1 H 0.7586(3) 0.3232(3) 0.1863(3) 0.058 Uiso 1 calc R . C23_1 C 0.7390(3) 0.4479(3) 0.1887(3) 0.0535(11) Uani 1 d . . H23_1 H 0.6943(3) 0.4179(3) 0.2586(3) 0.064 Uiso 1 calc R . C24_1 C 0.7640(2) 0.5470(3) 0.1326(2) 0.0425(9) Uani 1 d . . H24_1 H 0.7366(2) 0.5850(3) 0.1632(2) 0.051 Uiso 1 calc R . Co1_2 Co 0.54588(3) 0.79568(3) 0.18401(3) 0.02924(11) Uani 1 d . . Co2_2 Co 0.45703(3) 0.72736(3) 0.36685(3) 0.03512(12) Uani 1 d . . Co3_2 Co 0.65324(3) 0.97382(3) 0.33223(3) 0.02256(10) Uani 1 d . . Co4_2 Co 0.51882(3) 1.03672(3) 0.25645(3) 0.02472(10) Uani 1 d . . S1_2 S 0.83028(7) 0.72363(7) 0.19217(7) 0.0446(2) Uani 1 d . . S2_2 S 0.89570(6) 1.10647(6) 0.08315(6) 0.0388(2) Uani 1 d . . O1_2 O 0.7266(2) 0.9145(2) -0.0133(2) 0.0607(8) Uani 1 d . . C1_2 C 0.6580(3) 0.8683(3) 0.0635(3) 0.0400(8) Uani 1 d . . O2_2 O 0.5269(2) 0.6190(2) 0.1734(3) 0.0863(11) Uani 1 d . . C2_2 C 0.5330(3) 0.6869(3) 0.1771(3) 0.0515(10) Uani 1 d . . O3_2 O 0.3615(2) 0.8828(2) 0.1334(2) 0.0603(7) Uani 1 d . . C3_2 C 0.4331(3) 0.8506(3) 0.1528(3) 0.0396(8) Uani 1 d . . O4_2 O 0.3939(3) 0.5257(2) 0.4269(3) 0.123(2) Uani 1 d . . C4_2 C 0.4159(3) 0.6043(3) 0.4033(3) 0.0689(13) Uani 1 d . . O5_2 O 0.2498(2) 0.8064(2) 0.3782(2) 0.0668(8) Uani 1 d . . C5_2 C 0.3290(3) 0.7764(3) 0.3754(3) 0.0464(9) Uani 1 d . . O6_2 O 0.4757(3) 0.6854(2) 0.5531(2) 0.0750(9) Uani 1 d . . C6_2 C 0.4659(3) 0.7043(3) 0.4811(3) 0.0511(10) Uani 1 d . . O7_2 O 0.4910(2) 0.8799(2) 0.5426(2) 0.0501(6) Uani 1 d . . C7_2 C 0.5536(2) 0.9146(2) 0.4622(3) 0.0331(7) Uani 1 d . . O8_2 O 0.7645(2) 1.1482(2) 0.3049(2) 0.0463(6) Uani 1 d . . C8_2 C 0.7213(2) 1.0812(2) 0.3162(2) 0.0303(7) Uani 1 d . . O9_2 O 0.8148(2) 0.8464(2) 0.3726(2) 0.0499(6) Uani 1 d . . C9_2 C 0.7554(2) 0.8973(2) 0.3537(2) 0.0307(7) Uani 1 d . . O10_2 O 0.4476(2) 1.0801(2) 0.0948(2) 0.0641(8) Uani 1 d . . C10_2 C 0.4724(2) 1.0613(2) 0.1594(3) 0.0366(8) Uani 1 d . . O11_2 O 0.3133(2) 0.9452(2) 0.4411(2) 0.0607(8) Uani 1 d . . C11_2 C 0.3913(2) 0.9798(2) 0.3694(3) 0.0375(8) Uani 1 d . . O12_2 O 0.5593(2) 1.2361(2) 0.2147(2) 0.0632(8) Uani 1 d . . C12_2 C 0.5419(2) 1.1595(2) 0.2320(2) 0.0353(8) Uani 1 d . . C13_2 C 0.7569(2) 1.0837(2) 0.0907(2) 0.0309(7) Uani 1 d . . H13A_2 H 0.7323(2) 1.1461(2) 0.0613(2) 0.037 Uiso 1 calc R . H13B_2 H 0.7609(2) 1.0543(2) 0.0490(2) 0.037 Uiso 1 calc R . C14_2 C 0.6704(2) 1.0193(2) 0.1949(2) 0.0248(6) Uani 1 d . . C15_2 C 0.6034(2) 0.9318(2) 0.2559(2) 0.0212(6) Uani 1 d . . C16_2 C 0.5787(2) 0.8400(2) 0.2668(2) 0.0237(6) Uani 1 d . . C17_2 C 0.6154(2) 0.7570(2) 0.2797(2) 0.0288(7) Uani 1 d . . C18_2 C 0.7022(2) 0.6989(2) 0.3003(2) 0.0353(8) Uani 1 d . . H18A_2 H 0.6692(2) 0.6301(2) 0.3344(2) 0.042 Uiso 1 calc R . H18B_2 H 0.7220(2) 0.7086(2) 0.3479(2) 0.042 Uiso 1 calc R . C19_2 C 0.9066(2) 0.8248(3) 0.1750(2) 0.0341(8) Uani 1 d . . C20_2 C 0.8751(2) 0.9130(2) 0.1373(2) 0.0317(7) Uani 1 d . . H20_2 H 0.8133(2) 0.9201(2) 0.1192(2) 0.038 Uiso 1 calc R . C21_2 C 0.9331(2) 0.9922(2) 0.1254(2) 0.0333(8) Uani 1 d . . C22_2 C 1.0257(2) 0.9807(3) 0.1491(3) 0.0477(10) Uani 1 d . . H22_2 H 1.0661(2) 1.0341(3) 0.1412(3) 0.057 Uiso 1 calc R . C23_2 C 1.0593(3) 0.8934(3) 0.1834(3) 0.0566(11) Uani 1 d . . H23_2 H 1.1242(3) 0.8874(3) 0.1971(3) 0.068 Uiso 1 calc R . C24_2 C 0.9994(2) 0.8135(3) 0.1984(3) 0.0471(9) Uani 1 d . . H24_2 H 1.0213(2) 0.7525(3) 0.2241(3) 0.056 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1_1 0.0228(2) 0.0257(2) 0.0221(2) -0.0073(2) -0.0092(2) 0.0023(2) Co2_1 0.0244(2) 0.0248(2) 0.0260(2) -0.0101(2) -0.0122(2) 0.0066(2) Co3_1 0.0266(2) 0.0254(2) 0.0352(2) -0.0107(2) -0.0171(2) 0.0020(2) Co4_1 0.0422(2) 0.0351(3) 0.0389(3) -0.0233(2) -0.0181(2) 0.0053(2) S1_1 0.0441(4) 0.0371(5) 0.0291(4) -0.0190(4) -0.0155(4) 0.0120(4) S2_1 0.0632(5) 0.0237(4) 0.0638(6) -0.0134(4) -0.0464(5) 0.0119(4) C1_1 0.033(2) 0.035(2) 0.023(2) -0.0104(14) -0.0108(13) 0.0012(15) O1_1 0.0439(13) 0.071(2) 0.052(2) -0.0340(14) -0.0264(12) 0.0302(13) C2_1 0.031(2) 0.033(2) 0.030(2) -0.0052(15) -0.0128(14) 0.0033(14) O2_1 0.0459(13) 0.0322(15) 0.067(2) -0.0157(13) -0.0185(13) -0.0012(11) C3_1 0.0227(14) 0.039(2) 0.032(2) -0.011(2) -0.0104(13) 0.0081(13) O3_1 0.0456(13) 0.083(2) 0.0358(14) -0.0300(14) -0.0212(12) 0.0096(13) C4_1 0.033(2) 0.036(2) 0.045(2) -0.019(2) -0.0196(15) 0.0131(15) O4_1 0.068(2) 0.042(2) 0.103(2) -0.044(2) -0.039(2) 0.0155(14) C5_1 0.0283(15) 0.034(2) 0.029(2) -0.0100(15) -0.0110(14) 0.0079(13) O5_1 0.0484(14) 0.074(2) 0.0429(15) -0.0264(14) -0.0301(12) 0.0149(13) C6_1 0.035(2) 0.038(2) 0.038(2) -0.018(2) -0.020(2) 0.0159(15) O6_1 0.0360(13) 0.067(2) 0.0420(15) -0.0173(13) -0.0005(12) 0.0103(12) C7_1 0.030(2) 0.038(2) 0.037(2) -0.011(2) -0.0144(15) -0.0017(15) O7_1 0.0455(13) 0.058(2) 0.057(2) -0.0132(14) -0.0332(13) 0.0119(12) C8_1 0.043(2) 0.035(2) 0.054(2) -0.016(2) -0.030(2) 0.002(2) O8_1 0.077(2) 0.030(2) 0.082(2) -0.0142(14) -0.042(2) -0.0041(13) C9_1 0.0249(15) 0.041(2) 0.038(2) -0.012(2) -0.0152(15) 0.0011(14) O9_1 0.0334(12) 0.082(2) 0.043(2) -0.0265(15) -0.0162(12) 0.0086(12) C10_1 0.059(2) 0.066(3) 0.057(3) -0.043(2) -0.015(2) 0.008(2) O10_1 0.051(2) 0.132(3) 0.099(3) -0.081(2) 0.005(2) -0.001(2) C11_1 0.064(2) 0.042(2) 0.041(2) -0.019(2) -0.025(2) -0.001(2) O11_1 0.105(2) 0.055(2) 0.063(2) -0.014(2) -0.055(2) 0.005(2) C12_1 0.063(2) 0.042(2) 0.060(2) -0.032(2) -0.035(2) 0.014(2) O12_1 0.109(2) 0.055(2) 0.099(2) -0.052(2) -0.057(2) 0.021(2) C13_1 0.036(2) 0.036(2) 0.058(2) -0.029(2) -0.030(2) 0.0173(14) C14_1 0.0288(14) 0.027(2) 0.038(2) -0.0191(14) -0.0186(13) 0.0071(13) C15_1 0.0228(13) 0.027(2) 0.028(2) -0.0131(13) -0.0114(12) 0.0019(12) C16_1 0.0197(13) 0.026(2) 0.0223(15) -0.0094(13) -0.0084(11) 0.0048(12) C17_1 0.0198(13) 0.0191(15) 0.0222(15) -0.0074(12) -0.0067(11) 0.0041(11) C18_1 0.0300(14) 0.027(2) 0.025(2) -0.0102(13) -0.0140(13) 0.0023(12) C19_1 0.0258(14) 0.035(2) 0.028(2) -0.0113(14) -0.0154(13) 0.0027(13) C20_1 0.0300(15) 0.028(2) 0.025(2) -0.0057(14) -0.0161(13) 0.0024(13) C21_1 0.037(2) 0.030(2) 0.041(2) -0.007(2) -0.028(2) 0.0030(14) C22_1 0.046(2) 0.035(2) 0.043(2) 0.003(2) -0.026(2) -0.008(2) C23_1 0.043(2) 0.060(3) 0.031(2) -0.006(2) -0.009(2) -0.006(2) C24_1 0.034(2) 0.057(2) 0.028(2) -0.015(2) -0.0116(14) 0.001(2) Co1_2 0.0262(2) 0.0349(2) 0.0384(2) -0.0243(2) -0.0168(2) 0.0074(2) Co2_2 0.0325(2) 0.0287(2) 0.0362(3) -0.0146(2) -0.0074(2) -0.0023(2) Co3_2 0.0228(2) 0.0264(2) 0.0225(2) -0.0135(2) -0.0115(2) 0.0059(2) Co4_2 0.0236(2) 0.0263(2) 0.0284(2) -0.0146(2) -0.0137(2) 0.0080(2) S1_2 0.0426(4) 0.0542(6) 0.0645(6) -0.0455(5) -0.0284(4) 0.0256(4) S2_2 0.0272(4) 0.0416(5) 0.0366(5) -0.0171(4) -0.0040(3) -0.0037(4) O1_2 0.0390(13) 0.094(2) 0.039(2) -0.027(2) -0.0125(12) -0.0023(14) C1_2 0.036(2) 0.060(2) 0.043(2) -0.033(2) -0.025(2) 0.011(2) O2_2 0.080(2) 0.079(2) 0.172(4) -0.098(3) -0.077(2) 0.035(2) C2_2 0.041(2) 0.061(3) 0.088(3) -0.053(2) -0.041(2) 0.017(2) O3_2 0.0476(14) 0.067(2) 0.087(2) -0.042(2) -0.0436(15) 0.0280(13) C3_2 0.033(2) 0.043(2) 0.051(2) -0.029(2) -0.019(2) 0.010(2) O4_2 0.143(3) 0.048(2) 0.147(4) -0.046(2) -0.026(3) -0.022(2) C4_2 0.068(3) 0.042(3) 0.080(3) -0.029(2) -0.012(2) -0.009(2) O5_2 0.0350(13) 0.091(2) 0.079(2) -0.050(2) -0.0168(14) 0.0153(14) C5_2 0.034(2) 0.053(2) 0.045(2) -0.026(2) -0.005(2) -0.005(2) O6_2 0.093(2) 0.079(2) 0.039(2) -0.020(2) -0.025(2) 0.006(2) C6_2 0.051(2) 0.044(2) 0.040(2) -0.015(2) -0.006(2) -0.003(2) O7_2 0.0483(13) 0.062(2) 0.0267(13) -0.0196(12) -0.0053(11) 0.0121(12) C7_2 0.035(2) 0.038(2) 0.037(2) -0.023(2) -0.019(2) 0.0136(14) O8_2 0.0504(13) 0.0375(14) 0.058(2) -0.0243(12) -0.0276(12) 0.0010(11) C8_2 0.034(2) 0.032(2) 0.029(2) -0.0155(14) -0.0172(14) 0.0084(14) O9_2 0.0533(14) 0.068(2) 0.0372(14) -0.0280(13) -0.0264(12) 0.0373(13) C9_2 0.031(2) 0.042(2) 0.022(2) -0.0175(15) -0.0125(13) 0.0070(15) O10_2 0.083(2) 0.069(2) 0.064(2) -0.031(2) -0.058(2) 0.020(2) C10_2 0.038(2) 0.034(2) 0.044(2) -0.019(2) -0.025(2) 0.0108(14) O11_2 0.0330(12) 0.081(2) 0.046(2) -0.0256(15) -0.0013(12) 0.0063(13) C11_2 0.030(2) 0.042(2) 0.043(2) -0.021(2) -0.019(2) 0.0121(15) O12_2 0.066(2) 0.042(2) 0.105(2) -0.042(2) -0.051(2) 0.0172(13) C12_2 0.033(2) 0.038(2) 0.045(2) -0.021(2) -0.0243(15) 0.0121(15) C13_2 0.0300(15) 0.033(2) 0.025(2) -0.0117(14) -0.0088(13) 0.0045(13) C14_2 0.0251(14) 0.027(2) 0.026(2) -0.0157(13) -0.0119(12) 0.0065(12) C15_2 0.0205(13) 0.024(2) 0.0218(15) -0.0123(12) -0.0108(11) 0.0074(11) C16_2 0.0229(13) 0.026(2) 0.024(2) -0.0137(13) -0.0094(12) 0.0026(12) C17_2 0.0306(15) 0.026(2) 0.033(2) -0.0152(14) -0.0151(13) 0.0029(13) C18_2 0.037(2) 0.030(2) 0.046(2) -0.020(2) -0.023(2) 0.0101(14) C19_2 0.0259(15) 0.054(2) 0.034(2) -0.030(2) -0.0133(13) 0.0147(14) C20_2 0.0254(14) 0.049(2) 0.029(2) -0.025(2) -0.0129(13) 0.0143(14) C21_2 0.0205(14) 0.047(2) 0.024(2) -0.0154(15) -0.0033(12) 0.0018(14) C22_2 0.025(2) 0.062(3) 0.052(2) -0.028(2) -0.012(2) 0.001(2) C23_2 0.027(2) 0.087(3) 0.063(3) -0.040(2) -0.022(2) 0.012(2) C24_2 0.034(2) 0.062(3) 0.053(2) -0.033(2) -0.021(2) 0.024(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 Co1_1 C1_1 1.790(3) . ? Co1_1 C2_1 1.820(3) . ? Co1_1 C3_1 1.834(4) . ? Co1_1 C17_1 1.956(3) . ? Co1_1 C16_1 1.979(3) . ? Co1_1 Co2_1 2.4742(5) . ? Co2_1 C6_1 1.806(3) . ? Co2_1 C5_1 1.820(3) . ? Co2_1 C4_1 1.823(4) . ? Co2_1 C17_1 1.943(3) . ? Co2_1 C16_1 1.987(3) . ? Co3_1 C9_1 1.800(4) . ? Co3_1 C8_1 1.822(3) . ? Co3_1 C7_1 1.825(4) . ? Co3_1 C14_1 1.960(3) . ? Co3_1 C15_1 1.981(2) . ? Co3_1 Co4_1 2.4521(6) . ? Co4_1 C10_1 1.796(4) . ? Co4_1 C12_1 1.813(4) . ? Co4_1 C11_1 1.825(4) . ? Co4_1 C14_1 1.970(3) . ? Co4_1 C15_1 2.002(3) . ? S1_1 C19_1 1.760(3) . ? S1_1 C18_1 1.804(3) . ? S2_1 C21_1 1.753(4) . ? S2_1 C13_1 1.815(3) . ? C1_1 O1_1 1.136(4) . ? C2_1 O2_1 1.133(4) . ? C3_1 O3_1 1.130(4) . ? C4_1 O4_1 1.127(4) . ? C5_1 O5_1 1.129(4) . ? C6_1 O6_1 1.133(4) . ? C7_1 O7_1 1.130(4) . ? C8_1 O8_1 1.130(4) . ? C9_1 O9_1 1.139(4) . ? C10_1 O10_1 1.128(4) . ? C11_1 O11_1 1.139(4) . ? C12_1 O12_1 1.128(4) . ? C13_1 C14_1 1.501(4) . ? C14_1 C15_1 1.352(4) . ? C15_1 C16_1 1.429(4) . ? C16_1 C17_1 1.351(4) . ? C17_1 C18_1 1.497(4) . ? C19_1 C20_1 1.386(4) . ? C19_1 C24_1 1.395(4) . ? C20_1 C21_1 1.390(4) . ? C21_1 C22_1 1.399(5) . ? C22_1 C23_1 1.374(5) . ? C23_1 C24_1 1.380(5) . ? Co1_2 C1_2 1.801(4) . ? Co1_2 C3_2 1.816(4) . ? Co1_2 C2_2 1.816(4) . ? Co1_2 C17_2 1.954(3) . ? Co1_2 C16_2 1.982(3) . ? Co1_2 Co2_2 2.4571(6) . ? Co2_2 C6_2 1.792(4) . ? Co2_2 C4_2 1.801(4) . ? Co2_2 C5_2 1.824(4) . ? Co2_2 C17_2 1.961(3) . ? Co2_2 C16_2 1.986(3) . ? Co3_2 C9_2 1.810(3) . ? Co3_2 C7_2 1.818(3) . ? Co3_2 C8_2 1.820(3) . ? Co3_2 C14_2 1.949(3) . ? Co3_2 C15_2 1.977(3) . ? Co3_2 Co4_2 2.4560(5) . ? Co4_2 C10_2 1.789(3) . ? Co4_2 C11_2 1.818(3) . ? Co4_2 C12_2 1.823(3) . ? Co4_2 C14_2 1.958(3) . ? Co4_2 C15_2 1.993(3) . ? S1_2 C19_2 1.779(3) . ? S1_2 C18_2 1.829(3) . ? S2_2 C21_2 1.753(4) . ? S2_2 C13_2 1.818(3) . ? O1_2 C1_2 1.131(4) . ? O2_2 C2_2 1.126(4) . ? O3_2 C3_2 1.137(4) . ? O4_2 C4_2 1.138(5) . ? O5_2 C5_2 1.130(4) . ? O6_2 C6_2 1.137(4) . ? O7_2 C7_2 1.129(4) . ? O8_2 C8_2 1.131(3) . ? O9_2 C9_2 1.130(4) . ? O10_2 C10_2 1.132(4) . ? O11_2 C11_2 1.131(4) . ? O12_2 C12_2 1.130(4) . ? C13_2 C14_2 1.506(4) . ? C14_2 C15_2 1.356(4) . ? C15_2 C16_2 1.427(4) . ? C16_2 C17_2 1.349(4) . ? C17_2 C18_2 1.486(4) . ? C19_2 C20_2 1.371(4) . ? C19_2 C24_2 1.392(4) . ? C20_2 C21_2 1.394(4) . ? C21_2 C22_2 1.391(4) . ? C22_2 C23_2 1.368(5) . ? C23_2 C24_2 1.392(5) . ? 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 C1_1 Co1_1 C2_1 99.20(13) . . ? C1_1 Co1_1 C3_1 98.56(14) . . ? C2_1 Co1_1 C3_1 104.97(14) . . ? C1_1 Co1_1 C17_1 100.40(12) . . ? C2_1 Co1_1 C17_1 101.98(13) . . ? C3_1 Co1_1 C17_1 143.88(11) . . ? C1_1 Co1_1 C16_1 100.77(12) . . ? C2_1 Co1_1 C16_1 139.84(13) . . ? C3_1 Co1_1 C16_1 106.03(12) . . ? C17_1 Co1_1 C16_1 40.15(11) . . ? C1_1 Co1_1 Co2_1 149.10(9) . . ? C2_1 Co1_1 Co2_1 97.19(10) . . ? C3_1 Co1_1 Co2_1 102.27(9) . . ? C17_1 Co1_1 Co2_1 50.38(8) . . ? C16_1 Co1_1 Co2_1 51.54(8) . . ? C6_1 Co2_1 C5_1 98.79(13) . . ? C6_1 Co2_1 C4_1 97.64(15) . . ? C5_1 Co2_1 C4_1 105.58(15) . . ? C6_1 Co2_1 C17_1 101.88(12) . . ? C5_1 Co2_1 C17_1 143.59(13) . . ? C4_1 Co2_1 C17_1 101.00(13) . . ? C6_1 Co2_1 C16_1 100.48(13) . . ? C5_1 Co2_1 C16_1 106.64(13) . . ? C4_1 Co2_1 C16_1 139.82(12) . . ? C17_1 Co2_1 C16_1 40.20(11) . . ? C6_1 Co2_1 Co1_1 149.87(10) . . ? C5_1 Co2_1 Co1_1 99.66(9) . . ? C4_1 Co2_1 Co1_1 100.07(10) . . ? C17_1 Co2_1 Co1_1 50.85(8) . . ? C16_1 Co2_1 Co1_1 51.26(7) . . ? C9_1 Co3_1 C8_1 95.1(2) . . ? C9_1 Co3_1 C7_1 96.27(15) . . ? C8_1 Co3_1 C7_1 107.49(14) . . ? C9_1 Co3_1 C14_1 108.12(13) . . ? C8_1 Co3_1 C14_1 101.46(14) . . ? C7_1 Co3_1 C14_1 140.05(13) . . ? C9_1 Co3_1 C15_1 104.52(12) . . ? C8_1 Co3_1 C15_1 140.61(14) . . ? C7_1 Co3_1 C15_1 103.96(13) . . ? C14_1 Co3_1 C15_1 40.11(12) . . ? C9_1 Co3_1 Co4_1 156.18(9) . . ? C8_1 Co3_1 Co4_1 101.00(12) . . ? C7_1 Co3_1 Co4_1 95.53(10) . . ? C14_1 Co3_1 Co4_1 51.59(9) . . ? C15_1 Co3_1 Co4_1 52.40(9) . . ? C10_1 Co4_1 C12_1 98.8(2) . . ? C10_1 Co4_1 C11_1 100.9(2) . . ? C12_1 Co4_1 C11_1 101.0(2) . . ? C10_1 Co4_1 C14_1 98.9(2) . . ? C12_1 Co4_1 C14_1 105.86(15) . . ? C11_1 Co4_1 C14_1 143.5(2) . . ? C10_1 Co4_1 C15_1 102.76(14) . . ? C12_1 Co4_1 C15_1 141.63(15) . . ? C11_1 Co4_1 C15_1 105.48(15) . . ? C14_1 Co4_1 C15_1 39.77(12) . . ? C10_1 Co4_1 Co3_1 149.47(13) . . ? C12_1 Co4_1 Co3_1 96.14(12) . . ? C11_1 Co4_1 Co3_1 102.12(12) . . ? C14_1 Co4_1 Co3_1 51.20(8) . . ? C15_1 Co4_1 Co3_1 51.62(7) . . ? C19_1 S1_1 C18_1 103.18(14) . . ? C21_1 S2_1 C13_1 104.3(2) . . ? O1_1 C1_1 Co1_1 179.3(3) . . ? O2_1 C2_1 Co1_1 176.1(3) . . ? O3_1 C3_1 Co1_1 177.9(3) . . ? O4_1 C4_1 Co2_1 176.9(3) . . ? O5_1 C5_1 Co2_1 179.4(3) . . ? O6_1 C6_1 Co2_1 178.5(3) . . ? O7_1 C7_1 Co3_1 176.5(3) . . ? O8_1 C8_1 Co3_1 177.0(3) . . ? O9_1 C9_1 Co3_1 174.9(3) . . ? O10_1 C10_1 Co4_1 178.8(4) . . ? O11_1 C11_1 Co4_1 177.7(3) . . ? O12_1 C12_1 Co4_1 178.4(4) . . ? C14_1 C13_1 S2_1 115.6(2) . . ? C15_1 C14_1 C13_1 141.7(3) . . ? C15_1 C14_1 Co3_1 70.8(2) . . ? C13_1 C14_1 Co3_1 137.1(2) . . ? C15_1 C14_1 Co4_1 71.4(2) . . ? C13_1 C14_1 Co4_1 130.7(2) . . ? Co3_1 C14_1 Co4_1 77.21(10) . . ? C14_1 C15_1 C16_1 143.7(3) . . ? C14_1 C15_1 Co3_1 69.1(2) . . ? C16_1 C15_1 Co3_1 134.9(2) . . ? C14_1 C15_1 Co4_1 68.8(2) . . ? C16_1 C15_1 Co4_1 134.7(2) . . ? Co3_1 C15_1 Co4_1 75.98(10) . . ? C17_1 C16_1 C15_1 145.9(3) . . ? C17_1 C16_1 Co1_1 69.0(2) . . ? C15_1 C16_1 Co1_1 132.0(2) . . ? C17_1 C16_1 Co2_1 68.2(2) . . ? C15_1 C16_1 Co2_1 135.3(2) . . ? Co1_1 C16_1 Co2_1 77.20(10) . . ? C16_1 C17_1 C18_1 147.9(3) . . ? C16_1 C17_1 Co2_1 71.7(2) . . ? C18_1 C17_1 Co2_1 132.6(2) . . ? C16_1 C17_1 Co1_1 70.8(2) . . ? C18_1 C17_1 Co1_1 127.6(2) . . ? Co2_1 C17_1 Co1_1 78.78(11) . . ? C17_1 C18_1 S1_1 116.0(2) . . ? C20_1 C19_1 C24_1 120.2(3) . . ? C20_1 C19_1 S1_1 123.4(2) . . ? C24_1 C19_1 S1_1 116.4(3) . . ? C19_1 C20_1 C21_1 120.4(3) . . ? C20_1 C21_1 C22_1 119.2(3) . . ? C20_1 C21_1 S2_1 123.4(3) . . ? C22_1 C21_1 S2_1 117.3(3) . . ? C23_1 C22_1 C21_1 119.6(3) . . ? C22_1 C23_1 C24_1 121.7(3) . . ? C23_1 C24_1 C19_1 118.8(3) . . ? C1_2 Co1_2 C3_2 98.0(2) . . ? C1_2 Co1_2 C2_2 98.6(2) . . ? C3_2 Co1_2 C2_2 101.98(15) . . ? C1_2 Co1_2 C17_2 104.38(13) . . ? C3_2 Co1_2 C17_2 144.54(14) . . ? C2_2 Co1_2 C17_2 101.4(2) . . ? C1_2 Co1_2 C16_2 101.45(12) . . ? C3_2 Co1_2 C16_2 108.91(14) . . ? C2_2 Co1_2 C16_2 140.1(2) . . ? C17_2 Co1_2 C16_2 40.06(12) . . ? C1_2 Co1_2 Co2_2 152.14(10) . . ? C3_2 Co1_2 Co2_2 98.61(11) . . ? C2_2 Co1_2 Co2_2 99.62(14) . . ? C17_2 Co1_2 Co2_2 51.25(8) . . ? C16_2 Co1_2 Co2_2 51.82(7) . . ? C6_2 Co2_2 C4_2 97.4(2) . . ? C6_2 Co2_2 C5_2 102.0(2) . . ? C4_2 Co2_2 C5_2 103.8(2) . . ? C6_2 Co2_2 C17_2 100.05(14) . . ? C4_2 Co2_2 C17_2 103.6(2) . . ? C5_2 Co2_2 C17_2 142.02(15) . . ? C6_2 Co2_2 C16_2 100.88(13) . . ? C4_2 Co2_2 C16_2 141.5(2) . . ? C5_2 Co2_2 C16_2 105.16(14) . . ? C17_2 Co2_2 C16_2 39.95(12) . . ? C6_2 Co2_2 Co1_2 149.42(11) . . ? C4_2 Co2_2 Co1_2 99.14(15) . . ? C5_2 Co2_2 Co1_2 98.78(12) . . ? C17_2 Co2_2 Co1_2 51.01(9) . . ? C16_2 Co2_2 Co1_2 51.67(8) . . ? C9_2 Co3_2 C7_2 96.01(14) . . ? C9_2 Co3_2 C8_2 99.46(13) . . ? C7_2 Co3_2 C8_2 103.35(13) . . ? C9_2 Co3_2 C14_2 106.84(12) . . ? C7_2 Co3_2 C14_2 143.90(12) . . ? C8_2 Co3_2 C14_2 100.07(12) . . ? C9_2 Co3_2 C15_2 99.44(12) . . ? C7_2 Co3_2 C15_2 109.41(12) . . ? C8_2 Co3_2 C15_2 139.91(12) . . ? C14_2 Co3_2 C15_2 40.40(11) . . ? C9_2 Co3_2 Co4_2 151.38(10) . . ? C7_2 Co3_2 Co4_2 96.70(10) . . ? C8_2 Co3_2 Co4_2 102.39(10) . . ? C14_2 Co3_2 Co4_2 51.23(8) . . ? C15_2 Co3_2 Co4_2 52.08(8) . . ? C10_2 Co4_2 C11_2 102.78(14) . . ? C10_2 Co4_2 C12_2 97.94(15) . . ? C11_2 Co4_2 C12_2 103.78(15) . . ? C10_2 Co4_2 C14_2 99.69(13) . . ? C11_2 Co4_2 C14_2 142.93(14) . . ? C12_2 Co4_2 C14_2 101.84(13) . . ? C10_2 Co4_2 C15_2 100.69(13) . . ? C11_2 Co4_2 C15_2 106.22(13) . . ? C12_2 Co4_2 C15_2 139.89(12) . . ? C14_2 Co4_2 C15_2 40.12(11) . . ? C10_2 Co4_2 Co3_2 148.93(11) . . ? C11_2 Co4_2 Co3_2 99.00(10) . . ? C12_2 Co4_2 Co3_2 98.08(10) . . ? C14_2 Co4_2 Co3_2 50.88(8) . . ? C15_2 Co4_2 Co3_2 51.49(8) . . ? C19_2 S1_2 C18_2 101.90(14) . . ? C21_2 S2_2 C13_2 103.15(14) . . ? O1_2 C1_2 Co1_2 178.3(3) . . ? O2_2 C2_2 Co1_2 178.5(3) . . ? O3_2 C3_2 Co1_2 178.2(3) . . ? O4_2 C4_2 Co2_2 177.1(5) . . ? O5_2 C5_2 Co2_2 177.8(3) . . ? O6_2 C6_2 Co2_2 175.6(4) . . ? O7_2 C7_2 Co3_2 178.3(3) . . ? O8_2 C8_2 Co3_2 179.1(3) . . ? O9_2 C9_2 Co3_2 176.0(3) . . ? O10_2 C10_2 Co4_2 176.6(3) . . ? O11_2 C11_2 Co4_2 177.9(3) . . ? O12_2 C12_2 Co4_2 177.9(3) . . ? C14_2 C13_2 S2_2 115.3(2) . . ? C15_2 C14_2 C13_2 143.6(3) . . ? C15_2 C14_2 Co3_2 70.9(2) . . ? C13_2 C14_2 Co3_2 137.1(2) . . ? C15_2 C14_2 Co4_2 71.3(2) . . ? C13_2 C14_2 Co4_2 128.3(2) . . ? Co3_2 C14_2 Co4_2 77.89(10) . . ? C14_2 C15_2 C16_2 144.8(3) . . ? C14_2 C15_2 Co3_2 68.7(2) . . ? C16_2 C15_2 Co3_2 133.4(2) . . ? C14_2 C15_2 Co4_2 68.6(2) . . ? C16_2 C15_2 Co4_2 135.3(2) . . ? Co3_2 C15_2 Co4_2 76.43(10) . . ? C17_2 C16_2 C15_2 144.9(3) . . ? C17_2 C16_2 Co1_2 68.8(2) . . ? C15_2 C16_2 Co1_2 134.7(2) . . ? C17_2 C16_2 Co2_2 69.0(2) . . ? C15_2 C16_2 Co2_2 133.5(2) . . ? Co1_2 C16_2 Co2_2 76.50(9) . . ? C16_2 C17_2 C18_2 145.4(3) . . ? C16_2 C17_2 Co1_2 71.1(2) . . ? C18_2 C17_2 Co1_2 136.0(2) . . ? C16_2 C17_2 Co2_2 71.0(2) . . ? C18_2 C17_2 Co2_2 127.5(2) . . ? Co1_2 C17_2 Co2_2 77.75(11) . . ? C17_2 C18_2 S1_2 116.9(2) . . ? C20_2 C19_2 C24_2 120.8(3) . . ? C20_2 C19_2 S1_2 120.1(2) . . ? C24_2 C19_2 S1_2 119.2(3) . . ? C19_2 C20_2 C21_2 120.5(3) . . ? C22_2 C21_2 C20_2 118.6(3) . . ? C22_2 C21_2 S2_2 117.5(3) . . ? C20_2 C21_2 S2_2 123.9(2) . . ? C23_2 C22_2 C21_2 120.9(3) . . ? C22_2 C23_2 C24_2 120.5(3) . . ? C19_2 C24_2 C23_2 118.7(4) . . ? _refine_diff_density_max 0.598 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.100 #===END data_mm0025 #COMPLEX 11 _database_code_CSD 172438 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H16 Co8 O24 S4' _chemical_formula_weight 1576.29 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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' 'Co' 'Co' 0.3494 0.9721 '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 9.0208(11) _cell_length_b 10.5638(13) _cell_length_c 15.0520(13) _cell_angle_alpha 97.803(6) _cell_angle_beta 96.594(7) _cell_angle_gamma 91.095(5) _cell_volume 1410.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method ? _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 2.520 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 1.046 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device NoniusKappaCCD _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13816 _diffrn_reflns_av_R_equivalents 0.0805 _diffrn_reflns_av_sigmaI/netI 0.1308 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _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 1.38 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6351 _reflns_number_observed 3765 _reflns_observed_criterion >2sigma(I) _computing_data_collection maXus _computing_cell_refinement maXus _computing_data_reduction maXus _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 15 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0184P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6336 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1130 _refine_ls_R_factor_obs 0.0496 _refine_ls_wR_factor_all 0.1725 _refine_ls_wR_factor_obs 0.0767 _refine_ls_goodness_of_fit_all 0.989 _refine_ls_goodness_of_fit_obs 1.042 _refine_ls_restrained_S_all 1.769 _refine_ls_restrained_S_obs 1.042 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.38183(6) 0.51721(5) 0.72013(3) 0.0285(2) Uani 1 d . . Co2 Co 0.27233(6) 0.37145(5) 0.58495(3) 0.0288(2) Uani 1 d . . Co3 Co 0.50901(7) 0.07911(5) 0.69927(3) 0.0308(2) Uani 1 d . . Co4 Co 0.33726(7) 0.09669(5) 0.81736(3) 0.0342(2) Uani 1 d . . S1 S 0.76526(14) 0.14743(11) 0.90859(7) 0.0441(4) Uani 1 d . . S2 S 0.96132(13) 0.57396(10) 1.14844(6) 0.0367(3) Uani 1 d . . O1 O 0.6841(4) 0.5271(3) 0.6656(2) 0.0567(10) Uani 1 d . . C1 C 0.5678(6) 0.5262(4) 0.6873(3) 0.0365(12) Uani 1 d . . O2 O 0.2428(4) 0.7596(3) 0.6852(2) 0.0578(10) Uani 1 d . . C2 C 0.2986(5) 0.6680(4) 0.6986(3) 0.0344(11) Uani 1 d . . O3 O 0.4646(4) 0.5616(3) 0.9163(2) 0.0548(10) Uani 1 d . . C3 C 0.4295(5) 0.5466(4) 0.8409(3) 0.0340(11) Uani 1 d . . O4 O 0.0470(4) 0.1704(3) 0.5072(2) 0.0632(11) Uani 1 d . . C4 C 0.1360(5) 0.2465(4) 0.5365(3) 0.0373(12) Uani 1 d . . O5 O 0.5216(4) 0.2877(3) 0.4830(2) 0.0533(10) Uani 1 d . . C5 C 0.4270(6) 0.3201(4) 0.5230(3) 0.0361(12) Uani 1 d . . O6 O 0.1463(3) 0.5808(3) 0.4919(2) 0.0484(9) Uani 1 d . . C6 C 0.1946(5) 0.4984(4) 0.5266(2) 0.0352(11) Uani 1 d . . O7 O 0.6558(4) -0.1598(3) 0.7336(2) 0.0689(12) Uani 1 d . . C7 C 0.6002(5) -0.0663(5) 0.7229(3) 0.0434(13) Uani 1 d . . O8 O 0.3043(4) -0.0135(3) 0.5349(2) 0.0603(11) Uani 1 d . . C8 C 0.3847(5) 0.0198(4) 0.5981(3) 0.0371(12) Uani 1 d . . O9 O 0.7588(4) 0.2093(3) 0.6366(2) 0.0544(10) Uani 1 d . . C9 C 0.6612(6) 0.1559(4) 0.6573(3) 0.0385(12) Uani 1 d . . O10 O 0.4459(4) -0.1282(3) 0.8988(2) 0.0655(11) Uani 1 d . . C10 C 0.4027(5) -0.0418(5) 0.8681(3) 0.0452(13) Uani 1 d . . O11 O 0.0472(4) 0.0290(3) 0.7067(2) 0.0656(11) Uani 1 d . . C11 C 0.1583(6) 0.0502(4) 0.7509(3) 0.0448(13) Uani 1 d . . O12 O 0.2610(4) 0.2408(3) 0.9855(2) 0.0697(12) Uani 1 d . . C12 C 0.2856(5) 0.1856(4) 0.9188(3) 0.0433(13) Uani 1 d . . C13 C 0.3301(5) 0.3320(4) 0.7086(2) 0.0239(10) Uani 1 d . . C14 C 0.4000(5) 0.2293(4) 0.7484(2) 0.0259(10) Uani 1 d . . C15 C 0.5136(5) 0.2008(3) 0.8091(2) 0.0281(10) Uani 1 d . . C16 C 0.6376(5) 0.2662(4) 0.8748(2) 0.0324(11) Uani 1 d . . H16A H 0.5968(5) 0.3112(4) 0.9283(2) 0.039 Uiso 1 calc R . H16B H 0.6905(5) 0.3301(4) 0.8463(2) 0.039 Uiso 1 calc R . C17 C 0.8614(5) 0.2240(4) 1.0122(2) 0.0297(11) Uani 1 d . . C18 C 0.8698(5) 0.3540(4) 1.0394(2) 0.0306(11) Uani 1 d . . H18 H 0.8208(5) 0.4096(4) 1.0019(2) 0.037 Uiso 1 calc R . C19 C 0.9497(5) 0.4045(4) 1.1216(2) 0.0292(10) Uani 1 d . . C20 C 1.0239(5) 0.3229(4) 1.1747(2) 0.0377(12) Uani 1 d . . H20 H 1.0817(5) 0.3569(4) 1.2299(2) 0.045 Uiso 1 calc R . C21 C 1.0144(5) 0.1930(4) 1.1483(3) 0.0403(12) Uani 1 d . . H21 H 1.0646(5) 0.1379(4) 1.1858(3) 0.048 Uiso 1 calc R . C22 C 0.9329(5) 0.1419(4) 1.0681(3) 0.0340(11) Uani 1 d . . H22 H 0.9250(5) 0.0519(4) 1.0507(3) 0.041 Uiso 1 calc R . C23 C 0.9469(5) 0.6013(4) 1.2693(2) 0.0343(11) Uani 1 d . . H23A H 1.0035(5) 0.5352(4) 1.2981(2) 0.041 Uiso 1 calc R . H23B H 0.9954(5) 0.6853(4) 1.2945(2) 0.041 Uiso 1 calc R . C24 C 0.7923(5) 0.5991(4) 1.2944(2) 0.0260(10) Uani 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 0.0317(4) 0.0247(3) 0.0282(3) 0.0018(2) 0.0018(3) -0.0029(3) Co2 0.0326(4) 0.0286(4) 0.0244(3) 0.0027(2) 0.0004(3) 0.0009(3) Co3 0.0345(4) 0.0257(3) 0.0295(3) -0.0009(2) -0.0017(3) 0.0008(3) Co4 0.0390(4) 0.0299(4) 0.0343(3) 0.0089(3) 0.0028(3) -0.0018(3) S1 0.0516(9) 0.0354(7) 0.0376(6) -0.0082(5) -0.0140(6) 0.0117(6) S2 0.0461(8) 0.0331(7) 0.0308(5) 0.0004(5) 0.0101(5) -0.0048(6) O1 0.039(2) 0.072(3) 0.055(2) -0.008(2) 0.010(2) -0.010(2) C1 0.038(3) 0.035(3) 0.034(2) 0.001(2) -0.001(2) -0.007(3) O2 0.071(3) 0.032(2) 0.072(2) 0.011(2) 0.004(2) 0.013(2) C2 0.040(3) 0.026(3) 0.037(2) 0.004(2) 0.003(2) -0.004(2) O3 0.072(3) 0.058(2) 0.031(2) -0.0017(15) -0.002(2) 0.006(2) C3 0.032(3) 0.023(3) 0.047(3) 0.005(2) 0.003(2) -0.001(2) O4 0.054(3) 0.045(2) 0.079(2) -0.008(2) -0.017(2) -0.007(2) C4 0.036(3) 0.043(3) 0.032(2) 0.003(2) -0.001(2) 0.005(2) O5 0.050(2) 0.067(3) 0.046(2) 0.009(2) 0.016(2) 0.011(2) C5 0.042(3) 0.039(3) 0.026(2) 0.004(2) 0.001(2) -0.002(3) O6 0.049(2) 0.048(2) 0.050(2) 0.020(2) -0.001(2) 0.008(2) C6 0.030(3) 0.048(3) 0.027(2) 0.004(2) 0.001(2) -0.001(2) O7 0.070(3) 0.042(2) 0.087(3) 0.004(2) -0.019(2) 0.017(2) C7 0.045(3) 0.035(3) 0.046(3) 0.002(2) -0.007(2) -0.002(3) O8 0.059(2) 0.057(2) 0.052(2) -0.014(2) -0.021(2) 0.006(2) C8 0.041(3) 0.028(3) 0.041(2) -0.001(2) 0.004(2) 0.003(2) O9 0.047(2) 0.060(3) 0.052(2) -0.003(2) 0.005(2) -0.015(2) C9 0.040(3) 0.032(3) 0.039(3) -0.006(2) -0.005(2) 0.001(2) O10 0.072(3) 0.053(2) 0.078(2) 0.037(2) 0.007(2) 0.009(2) C10 0.045(3) 0.046(3) 0.045(3) 0.012(2) 0.003(2) 0.002(3) O11 0.045(2) 0.072(3) 0.077(2) 0.019(2) -0.012(2) -0.012(2) C11 0.050(4) 0.031(3) 0.056(3) 0.012(2) 0.011(3) -0.005(3) O12 0.088(3) 0.081(3) 0.042(2) 0.007(2) 0.016(2) 0.017(2) C12 0.044(3) 0.044(3) 0.045(3) 0.016(2) 0.005(3) 0.003(3) C13 0.028(3) 0.020(2) 0.022(2) 0.002(2) 0.001(2) -0.004(2) C14 0.032(3) 0.024(2) 0.021(2) -0.002(2) 0.003(2) -0.002(2) C15 0.032(3) 0.026(2) 0.025(2) -0.001(2) 0.002(2) -0.002(2) C16 0.036(3) 0.030(3) 0.029(2) -0.001(2) -0.002(2) 0.001(2) C17 0.028(3) 0.032(3) 0.026(2) 0.000(2) -0.003(2) 0.003(2) C18 0.034(3) 0.032(3) 0.025(2) 0.002(2) -0.001(2) 0.001(2) C19 0.029(3) 0.029(3) 0.029(2) -0.001(2) 0.005(2) -0.003(2) C20 0.038(3) 0.043(3) 0.029(2) 0.005(2) -0.007(2) -0.002(2) C21 0.039(3) 0.042(3) 0.038(2) 0.005(2) -0.004(2) 0.006(2) C22 0.032(3) 0.026(3) 0.043(2) 0.001(2) 0.002(2) 0.002(2) C23 0.032(3) 0.037(3) 0.031(2) -0.006(2) 0.001(2) -0.002(2) C24 0.032(3) 0.024(2) 0.021(2) 0.000(2) 0.001(2) -0.003(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 Co1 C3 1.803(4) . ? Co1 C1 1.807(5) . ? Co1 C2 1.826(5) . ? Co1 C24 1.949(4) 2_667 ? Co1 C13 1.982(4) . ? Co1 Co2 2.4730(7) . ? Co2 C4 1.804(5) . ? Co2 C6 1.810(5) . ? Co2 C5 1.817(5) . ? Co2 C24 1.957(4) 2_667 ? Co2 C13 1.976(3) . ? Co3 C9 1.799(5) . ? Co3 C8 1.814(4) . ? Co3 C7 1.814(5) . ? Co3 C15 1.947(4) . ? Co3 C14 1.984(4) . ? Co3 Co4 2.4795(9) . ? Co4 C12 1.795(5) . ? Co4 C10 1.819(5) . ? Co4 C11 1.820(5) . ? Co4 C15 1.941(4) . ? Co4 C14 1.965(4) . ? S1 C17 1.777(3) . ? S1 C16 1.804(4) . ? S2 C19 1.779(4) . ? S2 C23 1.822(4) . ? O1 C1 1.135(5) . ? O2 C2 1.131(5) . ? O3 C3 1.131(4) . ? O4 C4 1.133(5) . ? O5 C5 1.132(5) . ? O6 C6 1.143(4) . ? O7 C7 1.139(5) . ? O8 C8 1.138(4) . ? O9 C9 1.133(5) . ? O10 C10 1.133(5) . ? O11 C11 1.138(5) . ? O12 C12 1.138(5) . ? C13 C24 1.334(5) 2_667 ? C13 C14 1.432(5) . ? C14 C15 1.359(5) . ? C15 C16 1.496(5) . ? C17 C18 1.377(5) . ? C17 C22 1.404(5) . ? C18 C19 1.391(4) . ? C19 C20 1.385(5) . ? C20 C21 1.374(5) . ? C21 C22 1.377(5) . ? C23 C24 1.486(6) . ? C24 C13 1.334(5) 2_667 ? C24 Co1 1.949(4) 2_667 ? C24 Co2 1.957(4) 2_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 C3 Co1 C1 98.6(2) . . ? C3 Co1 C2 101.1(2) . . ? C1 Co1 C2 105.3(2) . . ? C3 Co1 C24 102.9(2) . 2_667 ? C1 Co1 C24 140.8(2) . 2_667 ? C2 Co1 C24 102.3(2) . 2_667 ? C3 Co1 C13 98.2(2) . . ? C1 Co1 C13 105.2(2) . . ? C2 Co1 C13 140.8(2) . . ? C24 Co1 C13 39.7(2) 2_667 . ? C3 Co1 Co2 148.75(13) . . ? C1 Co1 Co2 96.28(13) . . ? C2 Co1 Co2 101.27(12) . . ? C24 Co1 Co2 50.87(11) 2_667 . ? C13 Co1 Co2 51.23(9) . . ? C4 Co2 C6 98.1(2) . . ? C4 Co2 C5 99.4(2) . . ? C6 Co2 C5 103.3(2) . . ? C4 Co2 C24 97.5(2) . 2_667 ? C6 Co2 C24 105.6(2) . 2_667 ? C5 Co2 C24 143.8(2) . 2_667 ? C4 Co2 C13 103.7(2) . . ? C6 Co2 C13 140.6(2) . . ? C5 Co2 C13 104.9(2) . . ? C24 Co2 C13 39.6(2) 2_667 . ? C4 Co2 Co1 147.96(14) . . ? C6 Co2 Co1 94.40(12) . . ? C5 Co2 Co1 106.29(12) . . ? C24 Co2 Co1 50.58(11) 2_667 . ? C13 Co2 Co1 51.44(11) . . ? C9 Co3 C8 103.8(2) . . ? C9 Co3 C7 98.5(2) . . ? C8 Co3 C7 100.9(2) . . ? C9 Co3 C15 95.1(2) . . ? C8 Co3 C15 140.2(2) . . ? C7 Co3 C15 110.6(2) . . ? C9 Co3 C14 101.1(2) . . ? C8 Co3 C14 100.9(2) . . ? C7 Co3 C14 146.1(2) . . ? C15 Co3 C14 40.43(14) . . ? C9 Co3 Co4 144.94(13) . . ? C8 Co3 Co4 102.24(15) . . ? C7 Co3 Co4 99.2(2) . . ? C15 Co3 Co4 50.28(12) . . ? C14 Co3 Co4 50.76(11) . . ? C12 Co4 C10 96.4(2) . . ? C12 Co4 C11 103.3(2) . . ? C10 Co4 C11 107.2(2) . . ? C12 Co4 C15 96.8(2) . . ? C10 Co4 C15 106.5(2) . . ? C11 Co4 C15 138.2(2) . . ? C12 Co4 C14 103.9(2) . . ? C10 Co4 C14 142.6(2) . . ? C11 Co4 C14 98.4(2) . . ? C15 Co4 C14 40.71(14) . . ? C12 Co4 Co3 147.22(15) . . ? C10 Co4 Co3 96.1(2) . . ? C11 Co4 Co3 101.7(2) . . ? C15 Co4 Co3 50.49(11) . . ? C14 Co4 Co3 51.45(12) . . ? C17 S1 C16 103.2(2) . . ? C19 S2 C23 103.7(2) . . ? O1 C1 Co1 177.4(4) . . ? O2 C2 Co1 177.9(4) . . ? O3 C3 Co1 176.9(4) . . ? O4 C4 Co2 177.8(4) . . ? O5 C5 Co2 178.7(4) . . ? O6 C6 Co2 178.1(4) . . ? O7 C7 Co3 176.8(4) . . ? O8 C8 Co3 177.6(4) . . ? O9 C9 Co3 175.3(4) . . ? O10 C10 Co4 178.6(5) . . ? O11 C11 Co4 175.1(4) . . ? O12 C12 Co4 175.9(4) . . ? C24 C13 C14 143.3(4) 2_667 . ? C24 C13 Co2 69.4(2) 2_667 . ? C14 C13 Co2 136.4(3) . . ? C24 C13 Co1 68.9(2) 2_667 . ? C14 C13 Co1 132.5(3) . . ? Co2 C13 Co1 77.33(13) . . ? C15 C14 C13 143.7(3) . . ? C15 C14 Co4 68.7(2) . . ? C13 C14 Co4 135.9(3) . . ? C15 C14 Co3 68.3(2) . . ? C13 C14 Co3 133.2(3) . . ? Co4 C14 Co3 77.79(14) . . ? C14 C15 C16 139.9(4) . . ? C14 C15 Co4 70.6(2) . . ? C16 C15 Co4 135.5(3) . . ? C14 C15 Co3 71.2(2) . . ? C16 C15 Co3 133.2(3) . . ? Co4 C15 Co3 79.23(13) . . ? C15 C16 S1 108.6(3) . . ? C18 C17 C22 119.7(3) . . ? C18 C17 S1 125.0(3) . . ? C22 C17 S1 115.3(3) . . ? C17 C18 C19 120.4(3) . . ? C20 C19 C18 119.3(4) . . ? C20 C19 S2 123.5(3) . . ? C18 C19 S2 117.1(3) . . ? C21 C20 C19 120.5(3) . . ? C20 C21 C22 120.7(4) . . ? C21 C22 C17 119.3(4) . . ? C24 C23 S2 115.3(2) . . ? C13 C24 C23 140.4(4) 2_667 . ? C13 C24 Co1 71.5(2) 2_667 2_667 ? C23 C24 Co1 139.3(3) . 2_667 ? C13 C24 Co2 70.9(2) 2_667 2_667 ? C23 C24 Co2 128.4(2) . 2_667 ? Co1 C24 Co2 78.5(2) 2_667 2_667 ? _refine_diff_density_max 0.509 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.122 #===END data_mm0131 #DATA FOR COMPLEX 12 _database_code_CSD 172439 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H8 Co4 O12 S2' _chemical_formula_weight 788.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 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 32.9896(9) _cell_length_b 11.5540(3) _cell_length_c 16.1586(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.071(14) _cell_angle_gamma 90.00 _cell_volume 5666.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 16217 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 2.510 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.590 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'fine slice omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26919 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6457 _reflns_number_gt 5107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; TEXSAN: Molecular Structure Corporation (1995). Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA' ; _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _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^)+(0.0511P)^2^+0.2791P] 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 6457 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Co1 Co 0.138781(11) -0.26541(3) -0.16904(2) 0.02547(9) Uani 1 1 d . . . Co2 Co 0.156932(11) -0.07998(3) -0.22142(2) 0.02532(9) Uani 1 1 d . . . Co3 Co 0.038143(11) -0.25051(3) -0.43788(2) 0.02645(10) Uani 1 1 d . . . Co4 Co 0.093572(11) -0.20944(3) -0.50073(2) 0.02785(10) Uani 1 1 d . . . S1 S 0.21732(2) -0.38111(5) -0.31485(4) 0.03155(15) Uani 1 1 d . . . S2 S 0.13868(2) -0.53485(6) -0.45108(4) 0.04101(18) Uani 1 1 d . . . O1 O 0.11363(8) -0.50968(17) -0.19485(16) 0.0572(6) Uani 1 1 d . . . C1 C 0.12504(9) -0.4166(2) -0.18360(17) 0.0338(6) Uani 1 1 d . . . O2 O 0.20489(9) -0.2600(2) 0.01741(14) 0.0750(8) Uani 1 1 d . . . C2 C 0.17868(10) -0.2631(3) -0.05320(18) 0.0439(7) Uani 1 1 d . . . O3 O 0.05319(8) -0.1935(2) -0.16793(16) 0.0664(7) Uani 1 1 d . . . C3 C 0.08656(10) -0.2210(2) -0.16615(18) 0.0391(7) Uani 1 1 d . . . O4 O 0.23045(8) -0.00883(19) -0.05407(13) 0.0585(6) Uani 1 1 d . . . C4 C 0.20218(10) -0.0333(2) -0.11853(18) 0.0380(6) Uani 1 1 d . . . O5 O 0.08371(8) 0.0642(2) -0.21879(16) 0.0654(7) Uani 1 1 d . . . C5 C 0.11113(10) 0.0076(2) -0.22179(18) 0.0390(6) Uani 1 1 d . . . O6 O 0.17783(7) 0.04084(16) -0.35924(13) 0.0440(5) Uani 1 1 d . . . C6 C 0.16994(8) -0.0045(2) -0.30490(16) 0.0299(5) Uani 1 1 d . . . O7 O 0.01015(8) -0.4133(2) -0.33209(15) 0.0604(6) Uani 1 1 d . . . C7 C 0.02068(9) -0.3472(2) -0.37131(17) 0.0372(6) Uani 1 1 d . . . O8 O 0.01736(8) -0.02011(19) -0.38508(16) 0.0620(6) Uani 1 1 d . . . C8 C 0.02544(9) -0.1084(3) -0.40443(18) 0.0394(6) Uani 1 1 d . . . O9 O -0.03658(8) -0.2849(2) -0.61122(14) 0.0631(7) Uani 1 1 d . . . C9 C -0.00797(9) -0.2723(2) -0.54473(19) 0.0397(6) Uani 1 1 d . . . O10 O 0.08215(8) 0.04358(19) -0.49989(16) 0.0657(7) Uani 1 1 d . . . C10 C 0.08638(9) -0.0536(3) -0.50265(17) 0.0409(7) Uani 1 1 d . . . O11 O 0.04696(8) -0.3053(2) -0.68336(13) 0.0660(7) Uani 1 1 d . . . C11 C 0.06435(10) -0.2642(3) -0.61529(18) 0.0426(7) Uani 1 1 d . . . O12 O 0.18303(7) -0.2062(2) -0.49723(14) 0.0577(6) Uani 1 1 d . . . C12 C 0.14846(10) -0.2112(2) -0.49740(16) 0.0381(6) Uani 1 1 d . . . C13 C 0.22084(8) -0.2747(2) -0.22988(16) 0.0267(5) Uani 1 1 d . . . H13A H 0.2376 -0.3082 -0.1697 0.032 Uiso 1 1 calc R . . H13B H 0.2375 -0.2067 -0.2371 0.032 Uiso 1 1 calc R . . C14 C 0.17750(8) -0.23546(18) -0.23393(14) 0.0221(5) Uani 1 1 d . . . C15 C 0.13466(8) -0.22545(18) -0.29040(14) 0.0213(5) Uani 1 1 d . . . C16 C 0.10313(7) -0.25801(19) -0.37730(14) 0.0203(5) Uani 1 1 d . . . C17 C 0.08782(7) -0.3461(2) -0.43610(14) 0.0229(5) Uani 1 1 d . . . C18 C 0.08784(8) -0.4738(2) -0.44999(17) 0.0331(6) Uani 1 1 d . . . H18A H 0.0635 -0.4929 -0.5079 0.040 Uiso 1 1 calc R . . H18B H 0.0814 -0.5124 -0.4017 0.040 Uiso 1 1 calc R . . C19 C 0.16642(9) -0.5756(2) -0.33626(16) 0.0321(6) Uani 1 1 d . . . C20 C 0.15502(9) -0.6791(2) -0.30670(19) 0.0420(7) Uani 1 1 d . . . H20 H 0.1330 -0.7272 -0.3482 0.050 Uiso 1 1 calc R . . C21 C 0.17526(10) -0.7128(2) -0.2179(2) 0.0442(7) Uani 1 1 d . . . H21 H 0.1672 -0.7835 -0.1985 0.053 Uiso 1 1 calc R . . C22 C 0.20723(9) -0.6435(2) -0.15748(18) 0.0390(6) Uani 1 1 d . . . H22 H 0.2208 -0.6658 -0.0961 0.047 Uiso 1 1 calc R . . C23 C 0.21959(9) -0.5418(2) -0.18585(17) 0.0333(6) Uani 1 1 d . . . H23 H 0.2420 -0.4952 -0.1440 0.040 Uiso 1 1 calc R . . C24 C 0.19948(8) -0.5065(2) -0.27549(15) 0.0277(5) 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 0.0308(2) 0.02781(18) 0.01934(17) -0.00164(12) 0.01145(14) -0.00581(14) Co2 0.0309(2) 0.01908(17) 0.02609(17) -0.00446(12) 0.01125(14) -0.00252(13) Co3 0.02205(19) 0.02873(18) 0.02618(18) 0.00160(13) 0.00686(14) 0.00050(14) Co4 0.0284(2) 0.0334(2) 0.01976(17) 0.00512(13) 0.00720(14) -0.00172(14) S1 0.0395(4) 0.0286(3) 0.0317(3) 0.0014(3) 0.0195(3) 0.0055(3) S2 0.0457(4) 0.0427(4) 0.0292(3) -0.0125(3) 0.0089(3) 0.0128(3) O1 0.0642(16) 0.0327(12) 0.0878(16) -0.0052(11) 0.0440(13) -0.0101(11) C1 0.0364(16) 0.0345(15) 0.0346(13) 0.0024(11) 0.0184(12) -0.0039(12) O2 0.0719(18) 0.107(2) 0.0264(11) 0.0110(11) -0.0019(11) -0.0420(15) C2 0.0467(19) 0.0557(18) 0.0280(15) 0.0045(12) 0.0131(14) -0.0199(14) O3 0.0542(15) 0.0728(16) 0.0915(18) -0.0271(14) 0.0493(14) -0.0098(13) C3 0.0457(19) 0.0401(16) 0.0391(15) -0.0155(12) 0.0247(14) -0.0137(13) O4 0.0619(15) 0.0589(14) 0.0383(11) -0.0102(10) 0.0018(11) -0.0218(12) C4 0.0504(18) 0.0268(14) 0.0369(15) -0.0057(11) 0.0173(14) -0.0085(12) O5 0.0569(15) 0.0630(15) 0.0760(16) -0.0241(12) 0.0258(13) 0.0188(12) C5 0.0416(17) 0.0340(15) 0.0402(15) -0.0125(12) 0.0149(13) -0.0021(13) O6 0.0466(13) 0.0430(11) 0.0427(11) 0.0091(9) 0.0179(9) -0.0042(9) C6 0.0281(14) 0.0240(12) 0.0343(13) -0.0045(10) 0.0085(11) -0.0002(10) O7 0.0706(17) 0.0620(15) 0.0635(14) 0.0098(11) 0.0424(13) -0.0129(12) C7 0.0333(15) 0.0431(16) 0.0365(14) -0.0029(12) 0.0151(12) 0.0006(13) O8 0.0574(15) 0.0439(13) 0.0725(15) -0.0124(11) 0.0123(12) 0.0172(11) C8 0.0264(15) 0.0432(17) 0.0415(15) -0.0012(13) 0.0057(12) 0.0022(12) O9 0.0383(14) 0.0903(18) 0.0425(12) 0.0015(11) -0.0037(10) -0.0163(12) C9 0.0267(16) 0.0469(17) 0.0403(16) 0.0041(12) 0.0075(13) -0.0041(12) O10 0.0558(16) 0.0349(13) 0.0881(17) 0.0197(11) 0.0085(13) 0.0030(11) C10 0.0354(17) 0.0428(18) 0.0350(14) 0.0150(12) 0.0037(12) -0.0015(13) O11 0.0604(16) 0.0950(19) 0.0315(11) -0.0121(12) 0.0061(11) -0.0177(14) C11 0.0383(17) 0.0602(19) 0.0258(14) 0.0055(13) 0.0089(12) -0.0074(14) O12 0.0436(14) 0.0822(17) 0.0552(13) 0.0132(12) 0.0278(11) -0.0012(12) C12 0.0401(18) 0.0493(17) 0.0247(13) 0.0066(12) 0.0126(12) -0.0006(13) C13 0.0253(14) 0.0245(12) 0.0274(12) -0.0008(9) 0.0073(10) -0.0005(10) C14 0.0304(14) 0.0170(11) 0.0208(11) -0.0011(8) 0.0120(10) -0.0031(9) C15 0.0289(14) 0.0163(11) 0.0201(11) -0.0001(8) 0.0113(10) -0.0005(9) C16 0.0203(12) 0.0232(11) 0.0176(11) 0.0014(8) 0.0077(9) 0.0005(9) C17 0.0216(12) 0.0264(12) 0.0180(10) 0.0014(9) 0.0051(9) 0.0001(9) C18 0.0304(15) 0.0276(13) 0.0333(13) -0.0076(10) 0.0039(11) -0.0014(11) C19 0.0327(15) 0.0260(13) 0.0338(13) -0.0081(10) 0.0090(11) 0.0079(11) C20 0.0414(18) 0.0267(14) 0.0523(17) -0.0111(12) 0.0124(14) -0.0001(12) C21 0.0473(19) 0.0238(14) 0.0599(19) 0.0052(13) 0.0195(15) 0.0025(13) C22 0.0402(17) 0.0328(15) 0.0416(15) 0.0057(12) 0.0134(13) 0.0042(12) C23 0.0312(15) 0.0311(14) 0.0342(13) 0.0026(11) 0.0093(11) 0.0035(11) C24 0.0304(14) 0.0225(12) 0.0315(12) -0.0007(10) 0.0134(11) 0.0070(10) _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 C1 1.797(3) . ? Co1 C3 1.816(3) . ? Co1 C2 1.818(3) . ? Co1 C15 1.967(2) . ? Co1 C14 1.975(2) . ? Co1 Co2 2.4621(4) . ? Co2 C6 1.794(3) . ? Co2 C5 1.816(3) . ? Co2 C4 1.827(3) . ? Co2 C14 1.959(2) . ? Co2 C15 1.991(2) . ? Co3 C7 1.795(3) . ? Co3 C9 1.817(3) . ? Co3 C8 1.828(3) . ? Co3 C17 1.967(2) . ? Co3 C16 1.979(2) . ? Co3 Co4 2.4609(5) . ? Co4 C12 1.790(3) . ? Co4 C10 1.815(3) . ? Co4 C11 1.832(3) . ? Co4 C17 1.943(2) . ? Co4 C16 1.975(2) . ? S1 C24 1.773(2) . ? S1 C13 1.813(2) . ? S2 C19 1.781(3) . ? S2 C18 1.826(3) . ? O1 C1 1.131(3) . ? O2 C2 1.130(3) . ? O3 C3 1.135(3) . ? O4 C4 1.128(3) . ? O5 C5 1.132(3) . ? O6 C6 1.137(3) . ? O7 C7 1.131(3) . ? O8 C8 1.129(3) . ? O9 C9 1.128(3) . ? O10 C10 1.135(3) . ? O11 C11 1.127(3) . ? O12 C12 1.141(3) . ? C13 C14 1.477(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.354(3) . ? C15 C16 1.432(3) . ? C16 C17 1.349(3) . ? C17 C18 1.492(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.393(4) . ? C19 C24 1.397(3) . ? C20 C21 1.380(4) . ? C20 H20 0.9500 . ? C21 C22 1.378(4) . ? C21 H21 0.9500 . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 C24 1.397(3) . ? C23 H23 0.9500 . ? 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 C1 Co1 C3 94.88(12) . . ? C1 Co1 C2 101.12(12) . . ? C3 Co1 C2 106.31(13) . . ? C1 Co1 C15 100.50(10) . . ? C3 Co1 C15 105.29(11) . . ? C2 Co1 C15 139.66(11) . . ? C1 Co1 C14 106.45(10) . . ? C3 Co1 C14 141.42(11) . . ? C2 Co1 C14 100.72(12) . . ? C15 Co1 C14 40.17(9) . . ? C1 Co1 Co2 152.10(8) . . ? C3 Co1 Co2 97.12(9) . . ? C2 Co1 Co2 99.53(9) . . ? C15 Co1 Co2 51.98(6) . . ? C14 Co1 Co2 50.95(6) . . ? C6 Co2 C5 99.82(12) . . ? C6 Co2 C4 100.94(11) . . ? C5 Co2 C4 102.72(12) . . ? C6 Co2 C14 100.00(10) . . ? C5 Co2 C14 146.30(11) . . ? C4 Co2 C14 99.92(11) . . ? C6 Co2 C15 97.70(10) . . ? C5 Co2 C15 110.14(11) . . ? C4 Co2 C15 138.53(11) . . ? C14 Co2 C15 40.08(9) . . ? C6 Co2 Co1 147.52(8) . . ? C5 Co2 Co1 99.89(9) . . ? C4 Co2 Co1 99.57(8) . . ? C14 Co2 Co1 51.55(6) . . ? C15 Co2 Co1 51.09(6) . . ? C7 Co3 C9 97.90(12) . . ? C7 Co3 C8 102.53(12) . . ? C9 Co3 C8 101.64(13) . . ? C7 Co3 C17 95.91(11) . . ? C9 Co3 C17 108.59(11) . . ? C8 Co3 C17 141.84(11) . . ? C7 Co3 C16 102.49(10) . . ? C9 Co3 C16 143.65(11) . . ? C8 Co3 C16 102.85(10) . . ? C17 Co3 C16 39.96(9) . . ? C7 Co3 Co4 146.33(9) . . ? C9 Co3 Co4 96.63(9) . . ? C8 Co3 Co4 104.03(9) . . ? C17 Co3 Co4 50.57(6) . . ? C16 Co3 Co4 51.43(6) . . ? C12 Co4 C10 97.80(13) . . ? C12 Co4 C11 98.74(13) . . ? C10 Co4 C11 108.17(13) . . ? C12 Co4 C17 106.57(11) . . ? C10 Co4 C17 140.88(11) . . ? C11 Co4 C17 97.98(11) . . ? C12 Co4 C16 101.95(10) . . ? C10 Co4 C16 105.50(11) . . ? C11 Co4 C16 137.29(11) . . ? C17 Co4 C16 40.26(9) . . ? C12 Co4 Co3 153.09(8) . . ? C10 Co4 Co3 94.87(9) . . ? C11 Co4 Co3 99.70(9) . . ? C17 Co4 Co3 51.44(7) . . ? C16 Co4 Co3 51.59(7) . . ? C24 S1 C13 102.40(11) . . ? C19 S2 C18 101.02(12) . . ? O1 C1 Co1 175.6(3) . . ? O2 C2 Co1 176.9(3) . . ? O3 C3 Co1 177.3(3) . . ? O4 C4 Co2 177.3(3) . . ? O5 C5 Co2 177.2(3) . . ? O6 C6 Co2 178.2(2) . . ? O7 C7 Co3 175.9(3) . . ? O8 C8 Co3 179.0(2) . . ? O9 C9 Co3 179.5(3) . . ? O10 C10 Co4 176.9(3) . . ? O11 C11 Co4 175.3(3) . . ? O12 C12 Co4 176.2(3) . . ? C14 C13 S1 113.64(17) . . ? C14 C13 H13A 108.8 . . ? S1 C13 H13A 108.8 . . ? C14 C13 H13B 108.8 . . ? S1 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C15 C14 C13 142.5(2) . . ? C15 C14 Co2 71.26(13) . . ? C13 C14 Co2 130.19(16) . . ? C15 C14 Co1 69.59(13) . . ? C13 C14 Co1 137.67(16) . . ? Co2 C14 Co1 77.50(8) . . ? C14 C15 C16 143.5(2) . . ? C14 C15 Co1 70.24(12) . . ? C16 C15 Co1 130.99(17) . . ? C14 C15 Co2 68.66(13) . . ? C16 C15 Co2 137.52(16) . . ? Co1 C15 Co2 76.93(8) . . ? C17 C16 C15 144.8(2) . . ? C17 C16 Co4 68.62(12) . . ? C15 C16 Co4 133.07(16) . . ? C17 C16 Co3 69.54(14) . . ? C15 C16 Co3 134.69(17) . . ? Co4 C16 Co3 76.98(8) . . ? C16 C17 C18 146.1(2) . . ? C16 C17 Co4 71.13(13) . . ? C18 C17 Co4 135.79(16) . . ? C16 C17 Co3 70.50(14) . . ? C18 C17 Co3 127.05(17) . . ? Co4 C17 Co3 77.99(9) . . ? C17 C18 S2 115.96(18) . . ? C17 C18 H18A 108.3 . . ? S2 C18 H18A 108.3 . . ? C17 C18 H18B 108.3 . . ? S2 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? C20 C19 C24 119.4(2) . . ? C20 C19 S2 119.1(2) . . ? C24 C19 S2 121.50(19) . . ? C21 C20 C19 120.8(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.2(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 120.7(2) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C19 C24 C23 119.0(2) . . ? C19 C24 S1 119.48(18) . . ? C23 C24 S1 121.38(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Co1 Co2 C6 -7.8(3) . . . . ? C3 Co1 Co2 C6 -122.51(18) . . . . ? C2 Co1 Co2 C6 129.56(19) . . . . ? C15 Co1 Co2 C6 -18.64(18) . . . . ? C14 Co1 Co2 C6 33.43(18) . . . . ? C1 Co1 Co2 C5 118.9(2) . . . . ? C3 Co1 Co2 C5 4.10(12) . . . . ? C2 Co1 Co2 C5 -103.83(13) . . . . ? C15 Co1 Co2 C5 107.97(12) . . . . ? C14 Co1 Co2 C5 160.04(12) . . . . ? C1 Co1 Co2 C4 -136.3(2) . . . . ? C3 Co1 Co2 C4 108.93(12) . . . . ? C2 Co1 Co2 C4 1.00(13) . . . . ? C15 Co1 Co2 C4 -147.19(12) . . . . ? C14 Co1 Co2 C4 -95.12(12) . . . . ? C1 Co1 Co2 C14 -41.2(2) . . . . ? C3 Co1 Co2 C14 -155.94(12) . . . . ? C2 Co1 Co2 C14 96.13(14) . . . . ? C15 Co1 Co2 C14 -52.07(12) . . . . ? C1 Co1 Co2 C15 10.9(2) . . . . ? C3 Co1 Co2 C15 -103.87(12) . . . . ? C2 Co1 Co2 C15 148.20(14) . . . . ? C14 Co1 Co2 C15 52.07(12) . . . . ? C7 Co3 Co4 C12 -33.7(3) . . . . ? C9 Co3 Co4 C12 -148.8(2) . . . . ? C8 Co3 Co4 C12 107.4(2) . . . . ? C17 Co3 Co4 C12 -40.1(2) . . . . ? C16 Co3 Co4 C12 12.0(2) . . . . ? C7 Co3 Co4 C10 -151.66(18) . . . . ? C9 Co3 Co4 C10 93.25(13) . . . . ? C8 Co3 Co4 C10 -10.54(12) . . . . ? C17 Co3 Co4 C10 -158.10(12) . . . . ? C16 Co3 Co4 C10 -105.94(11) . . . . ? C7 Co3 Co4 C11 98.95(18) . . . . ? C9 Co3 Co4 C11 -16.14(14) . . . . ? C8 Co3 Co4 C11 -119.94(13) . . . . ? C17 Co3 Co4 C11 92.51(13) . . . . ? C16 Co3 Co4 C11 144.67(13) . . . . ? C7 Co3 Co4 C17 6.44(17) . . . . ? C9 Co3 Co4 C17 -108.65(12) . . . . ? C8 Co3 Co4 C17 147.55(12) . . . . ? C16 Co3 Co4 C17 52.16(11) . . . . ? C7 Co3 Co4 C16 -45.72(17) . . . . ? C9 Co3 Co4 C16 -160.81(12) . . . . ? C8 Co3 Co4 C16 95.40(12) . . . . ? C17 Co3 Co4 C16 -52.16(11) . . . . ? C3 Co1 C1 O1 22(3) . . . . ? C2 Co1 C1 O1 130(3) . . . . ? C15 Co1 C1 O1 -85(3) . . . . ? C14 Co1 C1 O1 -125(3) . . . . ? Co2 Co1 C1 O1 -93(3) . . . . ? C1 Co1 C2 O2 116(6) . . . . ? C3 Co1 C2 O2 -145(6) . . . . ? C15 Co1 C2 O2 -5(6) . . . . ? C14 Co1 C2 O2 7(6) . . . . ? Co2 Co1 C2 O2 -45(6) . . . . ? C1 Co1 C3 O3 -80(6) . . . . ? C2 Co1 C3 O3 177(100) . . . . ? C15 Co1 C3 O3 23(6) . . . . ? C14 Co1 C3 O3 44(6) . . . . ? Co2 Co1 C3 O3 75(6) . . . . ? C6 Co2 C4 O4 -127(6) . . . . ? C5 Co2 C4 O4 130(6) . . . . ? C14 Co2 C4 O4 -25(6) . . . . ? C15 Co2 C4 O4 -12(6) . . . . ? Co1 Co2 C4 O4 27(6) . . . . ? C6 Co2 C5 O5 -104(6) . . . . ? C4 Co2 C5 O5 0(6) . . . . ? C14 Co2 C5 O5 131(6) . . . . ? C15 Co2 C5 O5 154(6) . . . . ? Co1 Co2 C5 O5 102(6) . . . . ? C5 Co2 C6 O6 -113(7) . . . . ? C4 Co2 C6 O6 142(7) . . . . ? C14 Co2 C6 O6 40(7) . . . . ? C15 Co2 C6 O6 -1(7) . . . . ? Co1 Co2 C6 O6 14(8) . . . . ? C9 Co3 C7 O7 69(4) . . . . ? C8 Co3 C7 O7 173(4) . . . . ? C17 Co3 C7 O7 -40(4) . . . . ? C16 Co3 C7 O7 -80(4) . . . . ? Co4 Co3 C7 O7 -45(4) . . . . ? C7 Co3 C8 O8 -138(14) . . . . ? C9 Co3 C8 O8 -37(14) . . . . ? C17 Co3 C8 O8 105(14) . . . . ? C16 Co3 C8 O8 115(14) . . . . ? Co4 Co3 C8 O8 62(14) . . . . ? C7 Co3 C9 O9 145(100) . . . . ? C8 Co3 C9 O9 40(30) . . . . ? C17 Co3 C9 O9 -116(30) . . . . ? C16 Co3 C9 O9 -91(30) . . . . ? Co4 Co3 C9 O9 -65(30) . . . . ? C12 Co4 C10 O10 -104(5) . . . . ? C11 Co4 C10 O10 154(5) . . . . ? C17 Co4 C10 O10 25(5) . . . . ? C16 Co4 C10 O10 1(5) . . . . ? Co3 Co4 C10 O10 52(5) . . . . ? C12 Co4 C11 O11 86(3) . . . . ? C10 Co4 C11 O11 -172(100) . . . . ? C17 Co4 C11 O11 -22(3) . . . . ? C16 Co4 C11 O11 -32(4) . . . . ? Co3 Co4 C11 O11 -74(3) . . . . ? C10 Co4 C12 O12 -22(4) . . . . ? C11 Co4 C12 O12 88(4) . . . . ? C17 Co4 C12 O12 -171(4) . . . . ? C16 Co4 C12 O12 -129(4) . . . . ? Co3 Co4 C12 O12 -139(4) . . . . ? C24 S1 C13 C14 -72.36(19) . . . . ? S1 C13 C14 C15 -23.8(4) . . . . ? S1 C13 C14 Co2 -137.96(15) . . . . ? S1 C13 C14 Co1 101.6(2) . . . . ? C6 Co2 C14 C15 -90.10(14) . . . . ? C5 Co2 C14 C15 35.1(2) . . . . ? C4 Co2 C14 C15 166.81(14) . . . . ? Co1 Co2 C14 C15 72.42(12) . . . . ? C6 Co2 C14 C13 54.0(2) . . . . ? C5 Co2 C14 C13 179.2(2) . . . . ? C4 Co2 C14 C13 -49.1(2) . . . . ? C15 Co2 C14 C13 144.1(3) . . . . ? Co1 Co2 C14 C13 -143.5(2) . . . . ? C6 Co2 C14 Co1 -162.52(9) . . . . ? C5 Co2 C14 Co1 -37.3(2) . . . . ? C4 Co2 C14 Co1 94.39(10) . . . . ? C15 Co2 C14 Co1 -72.42(12) . . . . ? C1 Co1 C14 C15 86.84(15) . . . . ? C3 Co1 C14 C15 -34.0(2) . . . . ? C2 Co1 C14 C15 -168.05(15) . . . . ? Co2 Co1 C14 C15 -74.42(12) . . . . ? C1 Co1 C14 C13 -61.2(3) . . . . ? C3 Co1 C14 C13 178.0(2) . . . . ? C2 Co1 C14 C13 43.9(3) . . . . ? C15 Co1 C14 C13 -148.0(3) . . . . ? Co2 Co1 C14 C13 137.6(3) . . . . ? C1 Co1 C14 Co2 161.26(10) . . . . ? C3 Co1 C14 Co2 40.44(18) . . . . ? C2 Co1 C14 Co2 -93.63(12) . . . . ? C15 Co1 C14 Co2 74.42(12) . . . . ? C13 C14 C15 C16 10.8(6) . . . . ? Co2 C14 C15 C16 143.4(3) . . . . ? Co1 C14 C15 C16 -133.3(3) . . . . ? C13 C14 C15 Co1 144.1(3) . . . . ? Co2 C14 C15 Co1 -83.25(6) . . . . ? C13 C14 C15 Co2 -132.6(3) . . . . ? Co1 C14 C15 Co2 83.25(6) . . . . ? C1 Co1 C15 C14 -103.12(15) . . . . ? C3 Co1 C15 C14 158.82(14) . . . . ? C2 Co1 C15 C14 18.3(2) . . . . ? Co2 Co1 C15 C14 71.73(12) . . . . ? C1 Co1 C15 C16 41.9(2) . . . . ? C3 Co1 C15 C16 -56.2(2) . . . . ? C2 Co1 C15 C16 163.3(2) . . . . ? C14 Co1 C15 C16 145.0(3) . . . . ? Co2 Co1 C15 C16 -143.3(2) . . . . ? C1 Co1 C15 Co2 -174.84(10) . . . . ? C3 Co1 C15 Co2 87.09(10) . . . . ? C2 Co1 C15 Co2 -53.41(19) . . . . ? C14 Co1 C15 Co2 -71.73(12) . . . . ? C6 Co2 C15 C14 96.40(14) . . . . ? C5 Co2 C15 C14 -160.13(15) . . . . ? C4 Co2 C15 C14 -19.8(2) . . . . ? Co1 Co2 C15 C14 -73.62(12) . . . . ? C6 Co2 C15 C16 -51.9(3) . . . . ? C5 Co2 C15 C16 51.5(3) . . . . ? C4 Co2 C15 C16 -168.2(2) . . . . ? C14 Co2 C15 C16 -148.3(3) . . . . ? Co1 Co2 C15 C16 138.0(3) . . . . ? C6 Co2 C15 Co1 170.03(9) . . . . ? C5 Co2 C15 Co1 -86.50(11) . . . . ? C4 Co2 C15 Co1 53.78(17) . . . . ? C14 Co2 C15 Co1 73.62(12) . . . . ? C14 C15 C16 C17 45.1(6) . . . . ? Co1 C15 C16 C17 -69.8(4) . . . . ? Co2 C15 C16 C17 169.8(3) . . . . ? C14 C15 C16 Co4 -72.2(4) . . . . ? Co1 C15 C16 Co4 172.85(12) . . . . ? Co2 C15 C16 Co4 52.5(4) . . . . ? C14 C15 C16 Co3 168.4(2) . . . . ? Co1 C15 C16 Co3 53.4(3) . . . . ? Co2 C15 C16 Co3 -66.9(3) . . . . ? C12 Co4 C16 C17 -101.61(16) . . . . ? C10 Co4 C16 C17 156.70(15) . . . . ? C11 Co4 C16 C17 15.7(2) . . . . ? Co3 Co4 C16 C17 72.86(13) . . . . ? C12 Co4 C16 C15 45.0(2) . . . . ? C10 Co4 C16 C15 -56.7(2) . . . . ? C11 Co4 C16 C15 162.3(2) . . . . ? C17 Co4 C16 C15 146.6(3) . . . . ? Co3 Co4 C16 C15 -140.5(3) . . . . ? C12 Co4 C16 Co3 -174.47(10) . . . . ? C10 Co4 C16 Co3 83.84(11) . . . . ? C11 Co4 C16 Co3 -57.19(19) . . . . ? C17 Co4 C16 Co3 -72.86(13) . . . . ? C7 Co3 C16 C17 84.26(15) . . . . ? C9 Co3 C16 C17 -38.3(2) . . . . ? C8 Co3 C16 C17 -169.57(15) . . . . ? Co4 Co3 C16 C17 -71.75(12) . . . . ? C7 Co3 C16 C15 -64.8(2) . . . . ? C9 Co3 C16 C15 172.6(2) . . . . ? C8 Co3 C16 C15 41.4(2) . . . . ? C17 Co3 C16 C15 -149.0(3) . . . . ? Co4 Co3 C16 C15 139.2(3) . . . . ? C7 Co3 C16 Co4 156.01(9) . . . . ? C9 Co3 C16 Co4 33.4(2) . . . . ? C8 Co3 C16 Co4 -97.82(10) . . . . ? C17 Co3 C16 Co4 71.75(12) . . . . ? C15 C16 C17 C18 12.4(6) . . . . ? Co4 C16 C17 C18 148.2(4) . . . . ? Co3 C16 C17 C18 -128.2(4) . . . . ? C15 C16 C17 Co4 -135.8(4) . . . . ? Co3 C16 C17 Co4 83.56(7) . . . . ? C15 C16 C17 Co3 140.6(4) . . . . ? Co4 C16 C17 Co3 -83.56(7) . . . . ? C12 Co4 C17 C16 89.02(16) . . . . ? C10 Co4 C17 C16 -37.2(2) . . . . ? C11 Co4 C17 C16 -169.34(16) . . . . ? Co3 Co4 C17 C16 -73.26(13) . . . . ? C12 Co4 C17 C18 -66.1(3) . . . . ? C10 Co4 C17 C18 167.7(2) . . . . ? C11 Co4 C17 C18 35.6(3) . . . . ? C16 Co4 C17 C18 -155.1(3) . . . . ? Co3 Co4 C17 C18 131.7(3) . . . . ? C12 Co4 C17 Co3 162.28(9) . . . . ? C10 Co4 C17 Co3 36.09(19) . . . . ? C11 Co4 C17 Co3 -96.08(11) . . . . ? C16 Co4 C17 Co3 73.26(13) . . . . ? C7 Co3 C17 C16 -102.41(15) . . . . ? C9 Co3 C17 C16 157.18(14) . . . . ? C8 Co3 C17 C16 16.6(2) . . . . ? Co4 Co3 C17 C16 74.01(12) . . . . ? C7 Co3 C17 C18 44.3(2) . . . . ? C9 Co3 C17 C18 -56.1(2) . . . . ? C8 Co3 C17 C18 163.3(2) . . . . ? C16 Co3 C17 C18 146.7(3) . . . . ? Co4 Co3 C17 C18 -139.3(2) . . . . ? C7 Co3 C17 Co4 -176.41(10) . . . . ? C9 Co3 C17 Co4 83.18(11) . . . . ? C8 Co3 C17 Co4 -57.40(18) . . . . ? C16 Co3 C17 Co4 -74.01(12) . . . . ? C16 C17 C18 S2 -71.7(4) . . . . ? Co4 C17 C18 S2 62.6(3) . . . . ? Co3 C17 C18 S2 176.30(12) . . . . ? C19 S2 C18 C17 93.34(19) . . . . ? C18 S2 C19 C20 80.8(2) . . . . ? C18 S2 C19 C24 -99.6(2) . . . . ? C24 C19 C20 C21 1.5(4) . . . . ? S2 C19 C20 C21 -178.9(2) . . . . ? C19 C20 C21 C22 -0.1(4) . . . . ? C20 C21 C22 C23 -1.2(4) . . . . ? C21 C22 C23 C24 1.1(4) . . . . ? C20 C19 C24 C23 -1.5(4) . . . . ? S2 C19 C24 C23 178.89(19) . . . . ? C20 C19 C24 S1 174.68(19) . . . . ? S2 C19 C24 S1 -4.9(3) . . . . ? C22 C23 C24 C19 0.3(4) . . . . ? C22 C23 C24 S1 -175.9(2) . . . . ? C13 S1 C24 C19 136.33(19) . . . . ? C13 S1 C24 C23 -47.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.567 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.102 #===END data_mm9946 #DATA FOR COMPLEX 16 _database_code_CSD 172440 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44 H24 Co8 O26 S4' _chemical_formula_weight 1568.31 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 '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' _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 9.5307(3) _cell_length_b 10.9647(3) _cell_length_c 15.2542(5) _cell_angle_alpha 107.324(2) _cell_angle_beta 93.669(2) _cell_angle_gamma 104.731(2) _cell_volume 1454.80(8) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour dark _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method ? _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 2.445 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 1.119 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device NoniusKappaCCD _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8804 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5116 _reflns_number_observed 4265 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_structure_solution 'teXsan' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 15 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.1476P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5101 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_obs 0.0322 _refine_ls_wR_factor_all 0.1004 _refine_ls_wR_factor_obs 0.0748 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.065 _refine_ls_restrained_S_all 1.296 _refine_ls_restrained_S_obs 1.065 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.96704(4) 0.76004(4) 0.72756(3) 0.02598(12) Uani 1 d . . Co2 Co 0.70426(4) 0.63632(3) 0.68451(2) 0.02445(11) Uani 1 d . . Co3 Co 0.65013(4) 1.00610(3) 0.86005(2) 0.02586(12) Uani 1 d . . Co4 Co 0.66461(4) 1.06607(3) 0.71579(2) 0.02526(11) Uani 1 d . . S1 S 0.66750(8) 0.77068(7) 0.47831(5) 0.0314(2) Uani 1 d . . S2 S 1.03239(8) 0.65919(7) 0.11234(5) 0.0369(2) Uani 1 d . . C1 C 1.1144(3) 0.9061(3) 0.7423(2) 0.0352(7) Uani 1 d . . O1 O 1.2103(2) 0.9995(2) 0.7533(2) 0.0560(7) Uani 1 d . . C2 C 1.0448(3) 0.6346(3) 0.6579(2) 0.0428(8) Uani 1 d . . O2 O 1.0883(3) 0.5566(3) 0.6103(2) 0.0726(8) Uani 1 d . . C3 C 0.9913(3) 0.7528(3) 0.8440(2) 0.0433(8) Uani 1 d . . O3 O 1.0047(3) 0.7471(3) 0.9172(2) 0.0800(10) Uani 1 d . . C4 C 0.7263(3) 0.4723(3) 0.6258(2) 0.0365(7) Uani 1 d . . O4 O 0.7425(3) 0.3712(2) 0.5906(2) 0.0560(7) Uani 1 d . . C5 C 0.6609(3) 0.6313(3) 0.7991(2) 0.0314(7) Uani 1 d . . O5 O 0.6374(2) 0.6350(2) 0.87094(15) 0.0463(6) Uani 1 d . . C6 C 0.5240(3) 0.6133(3) 0.6268(2) 0.0316(7) Uani 1 d . . O6 O 0.4103(2) 0.5987(2) 0.5912(2) 0.0456(6) Uani 1 d . . C7 C 0.7394(3) 0.9655(3) 0.9500(2) 0.0364(7) Uani 1 d . . O7 O 0.7984(3) 0.9419(3) 1.0074(2) 0.0654(8) Uani 1 d . . C8 C 0.4775(3) 0.8722(3) 0.8262(2) 0.0337(7) Uani 1 d . . O8 O 0.3729(2) 0.7871(2) 0.8039(2) 0.0540(7) Uani 1 d . . C9 C 0.6060(4) 1.1526(3) 0.9331(2) 0.0433(8) Uani 1 d . . O9 O 0.5798(3) 1.2429(3) 0.9787(2) 0.0724(9) Uani 1 d . . C10 C 0.4934(3) 0.9546(3) 0.6416(2) 0.0335(7) Uani 1 d . . O10 O 0.3874(2) 0.8858(2) 0.5962(2) 0.0537(7) Uani 1 d . . C11 C 0.6289(3) 1.2277(3) 0.7592(2) 0.0361(7) Uani 1 d . . O11 O 0.6080(3) 1.3281(2) 0.7880(2) 0.0566(7) Uani 1 d . . C12 C 0.7785(3) 1.0974(3) 0.6306(2) 0.0367(7) Uani 1 d . . O12 O 0.8587(3) 1.1189(2) 0.5817(2) 0.0566(7) Uani 1 d . . C13 C 0.8242(3) 0.7579(2) 0.6293(2) 0.0227(6) Uani 1 d . . C14 C 0.8387(3) 0.7627(3) 0.5344(2) 0.0310(7) Uani 1 d . . H14A H 0.8636(3) 0.6823(3) 0.4973(2) 0.037 Uiso 1 calc R . H14B H 0.9193(3) 0.8420(3) 0.5374(2) 0.037 Uiso 1 calc R . C15 C 0.7233(3) 0.7836(3) 0.3698(2) 0.0293(7) Uani 1 d . . H15A H 0.6593(3) 0.8253(3) 0.3423(2) 0.035 Uiso 1 calc R . H15B H 0.8253(3) 0.8421(3) 0.3818(2) 0.035 Uiso 1 calc R . O16 O 0.7646(2) 0.6687(2) 0.21992(12) 0.0328(5) Uani 1 d . . C16 C 0.7147(3) 0.6487(3) 0.3013(2) 0.0314(7) Uani 1 d . . H16A H 0.7769(3) 0.6051(3) 0.3284(2) 0.038 Uiso 1 calc R . H16B H 0.6123(3) 0.5906(3) 0.2864(2) 0.038 Uiso 1 calc R . C17 C 0.7568(4) 0.5463(3) 0.1506(2) 0.0459(9) Uani 1 d . . H17A H 0.6530(4) 0.4959(3) 0.1250(2) 0.055 Uiso 1 calc R . H17B H 0.8018(4) 0.4912(3) 0.1778(2) 0.055 Uiso 1 calc R . C18 C 0.8382(3) 0.5773(3) 0.0744(2) 0.0403(8) Uani 1 d . . H18A H 0.7940(3) 0.6351(3) 0.0497(2) 0.048 Uiso 1 calc R . H18B H 0.8254(3) 0.4931(3) 0.0231(2) 0.048 Uiso 1 calc R . C21 C 0.7583(3) 0.9474(2) 0.7569(2) 0.0216(6) Uani 1 d . . C22 C 0.7947(3) 0.8280(2) 0.7115(2) 0.0218(6) Uani 1 d . . C19 C 1.0278(3) 0.8306(3) 0.1558(2) 0.0280(6) Uani 1 d . . H19A H 0.9828(3) 0.8540(3) 0.1051(2) 0.034 Uiso 1 calc R . H19B H 0.9663(3) 0.8405(3) 0.2059(2) 0.034 Uiso 1 calc R . C20 C 1.1779(3) 0.9234(3) 0.1923(2) 0.0237(6) Uani 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 0.0242(2) 0.0286(2) 0.0290(2) 0.0102(2) 0.0031(2) 0.0133(2) Co2 0.0269(2) 0.0209(2) 0.0260(2) 0.0072(2) 0.0029(2) 0.0085(2) Co3 0.0257(2) 0.0247(2) 0.0277(2) 0.0069(2) 0.0092(2) 0.0088(2) Co4 0.0248(2) 0.0245(2) 0.0304(2) 0.0099(2) 0.0050(2) 0.0124(2) S1 0.0304(4) 0.0458(5) 0.0243(4) 0.0128(3) 0.0084(3) 0.0190(3) S2 0.0327(4) 0.0242(4) 0.0477(5) 0.0023(3) 0.0129(4) 0.0072(3) C1 0.027(2) 0.040(2) 0.047(2) 0.0182(14) 0.0095(14) 0.0204(15) O1 0.0356(13) 0.0437(14) 0.095(2) 0.0284(13) 0.0231(13) 0.0117(12) C2 0.034(2) 0.043(2) 0.053(2) 0.009(2) 0.001(2) 0.023(2) O2 0.056(2) 0.066(2) 0.089(2) -0.0051(15) 0.0103(15) 0.0411(14) C3 0.035(2) 0.051(2) 0.043(2) 0.020(2) -0.0034(15) 0.008(2) O3 0.081(2) 0.109(2) 0.045(2) 0.042(2) -0.0091(14) 0.004(2) C4 0.039(2) 0.033(2) 0.036(2) 0.0104(14) -0.0006(14) 0.0104(14) O4 0.074(2) 0.0333(13) 0.057(2) 0.0021(11) 0.0003(13) 0.0268(12) C5 0.032(2) 0.0223(15) 0.038(2) 0.0079(13) 0.0060(14) 0.0064(12) O5 0.0559(15) 0.0465(14) 0.0339(13) 0.0149(10) 0.0134(11) 0.0066(11) C6 0.033(2) 0.027(2) 0.035(2) 0.0113(12) 0.0043(14) 0.0068(13) O6 0.0297(13) 0.0546(15) 0.0545(14) 0.0241(11) 0.0007(11) 0.0095(11) C7 0.038(2) 0.037(2) 0.031(2) 0.0083(14) 0.0079(14) 0.0076(14) O7 0.079(2) 0.074(2) 0.045(2) 0.0279(13) -0.0108(14) 0.021(2) C8 0.035(2) 0.039(2) 0.036(2) 0.0169(14) 0.0134(14) 0.018(2) O8 0.0297(13) 0.0506(15) 0.075(2) 0.0231(12) 0.0008(11) -0.0018(12) C9 0.054(2) 0.034(2) 0.044(2) 0.0111(15) 0.023(2) 0.014(2) O9 0.103(2) 0.046(2) 0.073(2) 0.0074(13) 0.051(2) 0.037(2) C10 0.038(2) 0.034(2) 0.032(2) 0.0073(13) 0.0072(14) 0.0206(15) O10 0.0356(14) 0.053(2) 0.055(2) -0.0060(12) -0.0059(12) 0.0153(12) C11 0.033(2) 0.033(2) 0.044(2) 0.0140(14) -0.0007(14) 0.0148(14) O11 0.063(2) 0.0351(14) 0.073(2) 0.0093(12) 0.0027(13) 0.0277(12) C12 0.037(2) 0.034(2) 0.045(2) 0.0175(14) 0.003(2) 0.0153(14) O12 0.056(2) 0.067(2) 0.066(2) 0.0418(14) 0.0302(14) 0.0220(13) C13 0.0241(14) 0.0245(14) 0.0239(14) 0.0087(11) 0.0035(11) 0.0139(11) C14 0.030(2) 0.046(2) 0.025(2) 0.0147(13) 0.0072(12) 0.0201(14) C15 0.036(2) 0.031(2) 0.0235(15) 0.0117(12) 0.0060(12) 0.0116(13) O16 0.0401(12) 0.0276(11) 0.0265(11) 0.0049(8) 0.0147(9) 0.0045(9) C16 0.038(2) 0.031(2) 0.026(2) 0.0095(12) 0.0086(13) 0.0083(13) C17 0.050(2) 0.031(2) 0.039(2) -0.0043(14) 0.019(2) -0.0039(15) C18 0.037(2) 0.033(2) 0.031(2) -0.0060(13) 0.0101(14) -0.0051(14) C21 0.0207(14) 0.0253(14) 0.0237(14) 0.0112(11) 0.0074(11) 0.0102(11) C22 0.0169(13) 0.0214(13) 0.0304(15) 0.0109(11) 0.0024(11) 0.0083(11) C19 0.0230(15) 0.0263(15) 0.034(2) 0.0071(12) 0.0050(12) 0.0083(12) C20 0.0233(14) 0.0247(14) 0.0264(15) 0.0101(11) 0.0057(11) 0.0100(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 Co1 C1 1.786(3) . ? Co1 C3 1.805(4) . ? Co1 C2 1.822(3) . ? Co1 C13 1.950(3) . ? Co1 C22 1.998(3) . ? Co1 Co2 2.4648(5) . ? Co2 C6 1.801(3) . ? Co2 C4 1.827(3) . ? Co2 C5 1.835(3) . ? Co2 C13 1.952(3) . ? Co2 C22 1.961(2) . ? Co3 C7 1.792(4) . ? Co3 C9 1.827(3) . ? Co3 C8 1.828(3) . ? Co3 C20 1.952(3) 2_776 ? Co3 C21 1.974(2) . ? Co3 Co4 2.4796(5) . ? Co4 C12 1.801(3) . ? Co4 C11 1.825(3) . ? Co4 C10 1.834(3) . ? Co4 C20 1.944(3) 2_776 ? Co4 C21 1.972(3) . ? S1 C15 1.805(3) . ? S1 C14 1.828(3) . ? S2 C18 1.810(3) . ? S2 C19 1.811(3) . ? C1 O1 1.147(3) . ? C2 O2 1.131(4) . ? C3 O3 1.137(4) . ? C4 O4 1.133(4) . ? C5 O5 1.124(3) . ? C6 O6 1.131(3) . ? C7 O7 1.138(4) . ? C8 O8 1.128(3) . ? C9 O9 1.124(4) . ? C10 O10 1.132(3) . ? C11 O11 1.131(4) . ? C12 O12 1.132(3) . ? C13 C22 1.350(4) . ? C13 C14 1.477(4) . ? C15 C16 1.514(4) . ? O16 C16 1.414(3) . ? O16 C17 1.421(3) . ? C17 C18 1.511(4) . ? C21 C20 1.351(3) 2_776 ? C21 C22 1.427(4) . ? C19 C20 1.487(4) . ? C20 C21 1.351(3) 2_776 ? C20 Co4 1.944(3) 2_776 ? C20 Co3 1.952(2) 2_776 ? 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 C1 Co1 C3 98.44(14) . . ? C1 Co1 C2 99.35(14) . . ? C3 Co1 C2 105.5(2) . . ? C1 Co1 C13 104.18(12) . . ? C3 Co1 C13 144.03(13) . . ? C2 Co1 C13 98.08(13) . . ? C1 Co1 C22 100.55(12) . . ? C3 Co1 C22 108.79(13) . . ? C2 Co1 C22 136.97(13) . . ? C13 Co1 C22 39.96(10) . . ? C1 Co1 Co2 150.59(10) . . ? C3 Co1 Co2 97.91(10) . . ? C2 Co1 Co2 99.62(10) . . ? C13 Co1 Co2 50.87(8) . . ? C22 Co1 Co2 50.84(7) . . ? C6 Co2 C4 99.03(13) . . ? C6 Co2 C5 100.11(13) . . ? C4 Co2 C5 104.97(13) . . ? C6 Co2 C13 100.56(12) . . ? C4 Co2 C13 105.77(12) . . ? C5 Co2 C13 139.41(11) . . ? C6 Co2 C22 101.83(12) . . ? C4 Co2 C22 142.93(12) . . ? C5 Co2 C22 101.11(11) . . ? C13 Co2 C22 40.34(10) . . ? C6 Co2 Co1 150.17(9) . . ? C4 Co2 Co1 97.40(10) . . ? C5 Co2 Co1 99.45(9) . . ? C13 Co2 Co1 50.79(8) . . ? C22 Co2 Co1 52.16(8) . . ? C7 Co3 C9 98.26(15) . . ? C7 Co3 C8 100.88(13) . . ? C9 Co3 C8 105.43(14) . . ? C7 Co3 C20 99.03(13) . 2_776 ? C9 Co3 C20 105.26(12) . 2_776 ? C8 Co3 C20 140.28(12) . 2_776 ? C7 Co3 C21 101.25(13) . . ? C9 Co3 C21 142.53(13) . . ? C8 Co3 C21 101.88(12) . . ? C20 Co3 C21 40.24(10) 2_776 . ? C7 Co3 Co4 148.14(10) . . ? C9 Co3 Co4 98.59(11) . . ? C8 Co3 Co4 100.42(9) . . ? C20 Co3 Co4 50.32(8) 2_776 . ? C21 Co3 Co4 51.04(8) . . ? C12 Co4 C11 99.38(14) . . ? C12 Co4 C10 101.45(13) . . ? C11 Co4 C10 104.65(13) . . ? C12 Co4 C20 96.37(12) . 2_776 ? C11 Co4 C20 103.71(12) . 2_776 ? C10 Co4 C20 143.31(12) . 2_776 ? C12 Co4 C21 98.89(12) . . ? C11 Co4 C21 141.30(12) . . ? C10 Co4 C21 104.73(12) . . ? C20 Co4 C21 40.35(10) 2_776 . ? C12 Co4 Co3 145.67(10) . . ? C11 Co4 Co3 98.06(10) . . ? C10 Co4 Co3 102.41(10) . . ? C20 Co4 Co3 50.63(7) 2_776 . ? C21 Co4 Co3 51.11(7) . . ? C15 S1 C14 99.50(13) . . ? C18 S2 C19 99.46(14) . . ? O1 C1 Co1 178.7(3) . . ? O2 C2 Co1 176.0(3) . . ? O3 C3 Co1 179.1(3) . . ? O4 C4 Co2 178.6(3) . . ? O5 C5 Co2 176.5(2) . . ? O6 C6 Co2 179.4(3) . . ? O7 C7 Co3 178.6(3) . . ? O8 C8 Co3 178.0(3) . . ? O9 C9 Co3 179.4(3) . . ? O10 C10 Co4 179.7(3) . . ? O11 C11 Co4 178.4(3) . . ? O12 C12 Co4 175.0(3) . . ? C22 C13 C14 141.5(3) . . ? C22 C13 Co1 71.9(2) . . ? C14 C13 Co1 131.2(2) . . ? C22 C13 Co2 70.18(15) . . ? C14 C13 Co2 136.3(2) . . ? Co1 C13 Co2 78.33(10) . . ? C13 C14 S1 110.5(2) . . ? C16 C15 S1 111.9(2) . . ? C16 O16 C17 111.9(2) . . ? O16 C16 C15 108.0(2) . . ? O16 C17 C18 108.3(2) . . ? C17 C18 S2 113.5(2) . . ? C20 C21 C22 141.1(2) 2_776 . ? C20 C21 Co4 68.7(2) 2_776 . ? C22 C21 Co4 135.1(2) . . ? C20 C21 Co3 69.0(2) 2_776 . ? C22 C21 Co3 136.0(2) . . ? Co4 C21 Co3 77.85(10) . . ? C13 C22 C21 142.4(3) . . ? C13 C22 Co2 69.5(2) . . ? C21 C22 Co2 136.0(2) . . ? C13 C22 Co1 68.1(2) . . ? C21 C22 Co1 134.5(2) . . ? Co2 C22 Co1 77.00(9) . . ? C20 C19 S2 111.2(2) . . ? C21 C20 C19 138.6(3) 2_776 . ? C21 C20 Co4 71.0(2) 2_776 2_776 ? C19 C20 Co4 133.5(2) . 2_776 ? C21 C20 Co3 70.75(15) 2_776 2_776 ? C19 C20 Co3 136.6(2) . 2_776 ? Co4 C20 Co3 79.05(10) 2_776 2_776 ? _refine_diff_density_max 0.506 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.080 #===END