# Copyright The Royal Society of Chemistry, 1998 data_global _publ_contact_author 'G. P. Shields' _publ_contact_author_email shields@ccdc.cam.ac.uk loop_ _publ_author_name Davies,J.E. Mays,M.J Raithby,P.R. Sarveswaran,V. Shields,G.P. _journal_name_full 'J. Chem. Soc., Dalton Trans.' _journal_volume '' _journal_page_first '' _journal_page_last '' _journal_year '' data_mm9610 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Co3(m3-S)(CO)7(M-BuNCPh)]' _chemical_formula_analytical ? _chemical_formula_sum 'C18 H14 Co3 N O7 S' _chemical_formula_weight 565.15 _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' '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.797(2) _cell_length_b 15.793(3) _cell_length_c 8.5066(11) _cell_angle_alpha 104.259(13) _cell_angle_beta 101.344(13) _cell_angle_gamma 83.24(2) _cell_volume 1120.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 40 _cell_measurement_theta_max 45 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method ? _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 2.326 _exptl_absorpt_correction_type 'empirical (10 psi scans)' _exptl_absorpt_correction_T_min 0.888 _exptl_absorpt_correction_T_max 0.997 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC5-R' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7 _diffrn_reflns_number 3157 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2931 _reflns_number_observed 1986 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _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 0 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^)+(0.1000P)^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 2931 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_obs 0.0529 _refine_ls_wR_factor_all 0.2068 _refine_ls_wR_factor_obs 0.1474 _refine_ls_goodness_of_fit_all 1.296 _refine_ls_goodness_of_fit_obs 1.148 _refine_ls_restrained_S_all 1.296 _refine_ls_restrained_S_obs 1.148 _refine_ls_shift/esd_max 0.000 _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 0.5347(2) 0.15356(9) 0.3106(2) 0.0439(5) Uani 1 d . . Co2 Co 0.4233(2) 0.29831(9) 0.4173(2) 0.0451(5) Uani 1 d . . Co3 Co 0.2552(2) 0.19834(10) 0.1838(2) 0.0515(5) Uani 1 d . . S1 S 0.3360(3) 0.1790(2) 0.4328(3) 0.0524(7) Uani 1 d . . O1 O 0.6943(11) 0.1907(7) 0.0647(12) 0.090(3) Uani 1 d . . N1 N 0.6865(9) 0.2031(5) 0.5132(9) 0.041(2) Uani 1 d . . C1 C 0.6346(14) 0.1766(8) 0.1595(14) 0.059(3) Uani 1 d . . O2 O 0.5596(13) -0.0378(6) 0.2184(14) 0.100(3) Uani 1 d . . C2 C 0.5561(14) 0.0348(8) 0.2589(15) 0.063(3) Uani 1 d . . O3 O 0.3450(13) 0.2653(7) -0.0776(12) 0.098(3) Uani 1 d . . C3 C 0.3130(14) 0.2402(8) 0.0250(16) 0.065(3) Uani 1 d . . O4 O 0.1620(13) 0.0236(7) -0.0063(13) 0.101(3) Uani 1 d . . C4 C 0.1953(14) 0.0911(9) 0.0694(15) 0.066(3) Uani 1 d . . O5 O -0.0288(12) 0.3147(7) 0.2343(14) 0.104(4) Uani 1 d . . C5 C 0.0769(17) 0.2709(9) 0.2145(15) 0.068(3) Uani 1 d . . C6 C 0.4985(14) 0.3661(8) 0.3133(14) 0.060(3) Uani 1 d . . O6 O 0.5498(12) 0.4063(7) 0.2464(13) 0.100(4) Uani 1 d . . O7 O 0.2446(12) 0.4262(7) 0.6390(13) 0.104(4) Uani 1 d . . C7 C 0.3144(14) 0.3793(8) 0.5558(15) 0.064(3) Uani 1 d . . C8 C 0.9280(19) 0.2188(10) 0.7343(21) 0.130(8) Uani 1 d . . H8A H 0.9644(19) 0.2637(10) 0.6960(21) 0.195 Uiso 1 calc R . H8B H 1.0153(19) 0.1854(10) 0.7822(21) 0.195 Uiso 1 calc R . H8C H 0.8643(19) 0.2451(10) 0.8156(21) 0.195 Uiso 1 calc R . C9 C 0.9251(15) 0.1179(10) 0.4538(19) 0.091(5) Uani 1 d . . H9A H 0.9587(15) 0.1633(10) 0.4144(19) 0.136 Uiso 1 calc R . H9B H 0.8605(15) 0.0812(10) 0.3652(19) 0.136 Uiso 1 calc R . H9C H 1.0141(15) 0.0833(10) 0.4954(19) 0.136 Uiso 1 calc R . C10 C 0.7782(17) 0.0891(9) 0.6559(17) 0.085(4) Uani 1 d . . H10A H 0.7178(17) 0.0502(9) 0.5671(17) 0.127 Uiso 1 calc R . H10B H 0.7155(17) 0.1163(9) 0.7377(17) 0.127 Uiso 1 calc R . H10C H 0.8665(17) 0.0566(9) 0.7043(17) 0.127 Uiso 1 calc R . C11 C 0.8332(12) 0.1588(7) 0.5907(14) 0.055(3) Uani 1 d . . C12 C 0.6270(11) 0.2820(7) 0.5547(11) 0.042(2) Uani 1 d . . C13 C 0.6903(11) 0.3586(6) 0.6791(12) 0.043(2) Uani 1 d . . C14 C 0.7888(12) 0.4085(7) 0.6386(14) 0.055(3) Uani 1 d . . H14 H 0.8151(12) 0.3935(7) 0.5340(14) 0.066 Uiso 1 calc R . C15 C 0.8484(14) 0.4804(8) 0.7519(17) 0.069(3) Uani 1 d . . H15 H 0.9168(14) 0.5131(8) 0.7251(17) 0.082 Uiso 1 calc R . C16 C 0.8057(16) 0.5038(8) 0.9067(18) 0.077(4) Uani 1 d . . H16 H 0.8433(16) 0.5531(8) 0.9832(18) 0.093 Uiso 1 calc R . C17 C 0.7094(15) 0.4548(9) 0.9452(14) 0.073(4) Uani 1 d . . H17 H 0.6846(15) 0.4696(9) 1.0504(14) 0.087 Uiso 1 calc R . C18 C 0.6475(13) 0.3842(8) 0.8347(12) 0.056(3) Uani 1 d . . H18 H 0.5773(13) 0.3531(8) 0.8625(12) 0.067 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 0.0441(9) 0.0434(9) 0.0416(9) 0.0029(6) 0.0069(6) -0.0087(6) Co2 0.0391(8) 0.0474(9) 0.0417(8) 0.0033(6) -0.0006(6) -0.0031(6) Co3 0.0455(9) 0.0604(10) 0.0453(9) 0.0086(7) -0.0023(7) -0.0159(7) S1 0.046(2) 0.066(2) 0.048(2) 0.0143(14) 0.0097(13) -0.0124(13) O1 0.096(7) 0.114(8) 0.074(6) 0.023(6) 0.042(6) -0.020(6) N1 0.040(5) 0.043(5) 0.037(5) 0.008(4) 0.001(4) -0.003(4) C1 0.065(8) 0.060(7) 0.047(7) 0.000(6) 0.014(6) -0.006(6) O2 0.126(9) 0.043(6) 0.131(9) 0.000(6) 0.044(7) -0.013(6) C2 0.062(8) 0.052(8) 0.069(8) -0.005(6) 0.015(6) -0.013(6) O3 0.111(8) 0.129(9) 0.065(6) 0.037(6) 0.003(6) -0.041(7) C3 0.056(8) 0.075(9) 0.055(8) 0.005(7) -0.007(6) -0.023(6) O4 0.115(9) 0.075(7) 0.101(8) -0.010(6) 0.008(6) -0.045(6) C4 0.068(9) 0.072(9) 0.057(8) 0.016(7) 0.003(6) -0.018(7) O5 0.060(7) 0.101(8) 0.143(10) 0.026(7) 0.017(7) 0.022(6) C5 0.073(10) 0.071(9) 0.055(8) 0.013(6) -0.011(7) -0.025(7) C6 0.060(8) 0.056(8) 0.056(7) 0.019(6) -0.015(6) 0.000(6) O6 0.095(8) 0.106(8) 0.115(9) 0.068(7) -0.005(6) -0.029(6) O7 0.082(7) 0.107(8) 0.093(7) -0.034(6) 0.030(6) 0.013(6) C7 0.056(8) 0.070(8) 0.052(7) -0.002(6) -0.003(6) -0.002(6) C8 0.109(14) 0.083(11) 0.141(15) 0.009(10) -0.081(12) 0.008(10) C9 0.049(8) 0.113(12) 0.127(13) 0.061(10) 0.029(8) 0.024(8) C10 0.086(10) 0.097(11) 0.080(9) 0.048(8) 0.015(8) 0.014(8) C11 0.036(6) 0.056(7) 0.068(7) 0.016(6) 0.006(5) 0.009(5) C12 0.036(6) 0.055(7) 0.035(6) 0.011(5) 0.001(4) -0.006(5) C13 0.035(6) 0.045(6) 0.041(6) 0.007(5) -0.008(5) -0.003(5) C14 0.051(7) 0.055(7) 0.057(7) 0.013(6) 0.002(6) -0.008(6) C15 0.059(8) 0.055(8) 0.083(10) 0.015(7) -0.011(7) -0.016(6) C16 0.065(9) 0.053(8) 0.085(10) -0.012(7) -0.016(8) 0.004(7) C17 0.066(8) 0.094(10) 0.043(7) -0.012(7) 0.006(6) -0.009(8) C18 0.061(7) 0.073(8) 0.031(6) 0.009(6) 0.001(5) -0.011(6) _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 C2 1.814(13) . ? Co1 C1 1.818(13) . ? Co1 N1 2.010(8) . ? Co1 S1 2.155(3) . ? Co1 Co2 2.411(2) . ? Co1 Co3 2.575(2) . ? Co2 C6 1.797(14) . ? Co2 C7 1.832(13) . ? Co2 C12 1.964(9) . ? Co2 S1 2.160(3) . ? Co2 Co3 2.545(2) . ? Co3 C4 1.814(13) . ? Co3 C3 1.818(14) . ? Co3 C5 1.85(2) . ? Co3 S1 2.183(3) . ? O1 C1 1.122(13) . ? N1 C12 1.285(12) . ? N1 C11 1.507(13) . ? O2 C2 1.111(13) . ? O3 C3 1.137(14) . ? O4 C4 1.139(14) . ? O5 C5 1.11(2) . ? C6 O6 1.131(14) . ? O7 C7 1.109(13) . ? C8 C11 1.52(2) . ? C9 C11 1.52(2) . ? C10 C11 1.51(2) . ? C12 C13 1.481(14) . ? C13 C14 1.379(14) . ? C13 C18 1.398(14) . ? C14 C15 1.38(2) . ? C15 C16 1.39(2) . ? C16 C17 1.35(2) . ? C17 C18 1.36(2) . ? 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 C2 Co1 C1 99.9(5) . . ? C2 Co1 N1 111.2(5) . . ? C1 Co1 N1 97.6(4) . . ? C2 Co1 S1 101.9(4) . . ? C1 Co1 S1 148.7(4) . . ? N1 Co1 S1 95.0(2) . . ? C2 Co1 Co2 158.1(4) . . ? C1 Co1 Co2 100.0(4) . . ? N1 Co1 Co2 74.9(2) . . ? S1 Co1 Co2 56.13(9) . . ? C2 Co1 Co3 106.8(4) . . ? C1 Co1 Co3 98.2(4) . . ? N1 Co1 Co3 135.3(2) . . ? S1 Co1 Co3 54.08(9) . . ? Co2 Co1 Co3 61.28(6) . . ? C6 Co2 C7 101.9(6) . . ? C6 Co2 C12 92.0(5) . . ? C7 Co2 C12 103.8(5) . . ? C6 Co2 S1 153.8(4) . . ? C7 Co2 S1 100.4(4) . . ? C12 Co2 S1 95.8(3) . . ? C6 Co2 Co1 103.6(4) . . ? C7 Co2 Co1 154.2(4) . . ? C12 Co2 Co1 71.9(3) . . ? S1 Co2 Co1 55.94(9) . . ? C6 Co2 Co3 103.1(4) . . ? C7 Co2 Co3 114.5(4) . . ? C12 Co2 Co3 134.2(3) . . ? S1 Co2 Co3 54.54(8) . . ? Co1 Co2 Co3 62.55(6) . . ? C4 Co3 C3 101.6(5) . . ? C4 Co3 C5 107.6(6) . . ? C3 Co3 C5 99.4(6) . . ? C4 Co3 S1 102.7(4) . . ? C3 Co3 S1 142.2(4) . . ? C5 Co3 S1 100.3(4) . . ? C4 Co3 Co2 152.2(4) . . ? C3 Co3 Co2 93.5(4) . . ? C5 Co3 Co2 92.5(4) . . ? S1 Co3 Co2 53.71(9) . . ? C4 Co3 Co1 99.0(4) . . ? C3 Co3 Co1 94.8(4) . . ? C5 Co3 Co1 146.4(4) . . ? S1 Co3 Co1 53.09(8) . . ? Co2 Co3 Co1 56.17(5) . . ? Co1 S1 Co2 67.93(9) . . ? Co1 S1 Co3 72.83(10) . . ? Co2 S1 Co3 71.75(10) . . ? C12 N1 C11 130.0(8) . . ? C12 N1 Co1 101.6(6) . . ? C11 N1 Co1 128.4(7) . . ? O1 C1 Co1 179.0(11) . . ? O2 C2 Co1 174.8(12) . . ? O3 C3 Co3 177.8(11) . . ? O4 C4 Co3 177.2(12) . . ? O5 C5 Co3 179.3(11) . . ? O6 C6 Co2 177.5(12) . . ? O7 C7 Co2 177.4(13) . . ? N1 C11 C10 104.7(9) . . ? N1 C11 C8 114.1(9) . . ? C10 C11 C8 107.9(12) . . ? N1 C11 C9 106.7(9) . . ? C10 C11 C9 110.9(11) . . ? C8 C11 C9 112.2(12) . . ? N1 C12 C13 130.6(9) . . ? N1 C12 Co2 111.1(7) . . ? C13 C12 Co2 118.3(7) . . ? C14 C13 C18 118.9(10) . . ? C14 C13 C12 119.4(9) . . ? C18 C13 C12 121.6(9) . . ? C15 C14 C13 120.5(11) . . ? C14 C15 C16 119.5(12) . . ? C17 C16 C15 119.7(12) . . ? C16 C17 C18 121.9(12) . . ? C17 C18 C13 119.5(11) . . ? _refine_diff_density_max 0.837 _refine_diff_density_min -1.479 _refine_diff_density_rms 0.373 data_mm9609 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Co3(M3-S)(CO)7{PhCCHC(O)Ph}]' _chemical_formula_analytical ? _chemical_formula_sum 'C22 H11 Co3 O8 S' _chemical_formula_weight 612.16 _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' '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 11.422(2) _cell_length_b 13.324(2) _cell_length_c 7.872(2) _cell_angle_alpha 91.42(2) _cell_angle_beta 98.71(2) _cell_angle_gamma 93.640(10) _cell_volume 1181.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method ? _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 2.215 _exptl_absorpt_correction_type 'empirical (10 psi scans)' _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7-R' _diffrn_measurement_method 'omega 2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 3295 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 22.52 _reflns_number_total 3102 _reflns_number_observed 2389 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _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 9 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^)+(0.0327P)^2^+0.2776P] 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 3093 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_obs 0.0349 _refine_ls_wR_factor_all 0.0863 _refine_ls_wR_factor_obs 0.0778 _refine_ls_goodness_of_fit_all 1.057 _refine_ls_goodness_of_fit_obs 1.097 _refine_ls_restrained_S_all 1.059 _refine_ls_restrained_S_obs 1.097 _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 0.72645(5) 0.76733(4) 0.77330(8) 0.0463(2) Uani 1 d . . Co2 Co 0.79234(6) 0.59293(5) 0.71858(9) 0.0544(2) Uani 1 d . . Co3 Co 0.67912(6) 0.68840(5) 0.47504(8) 0.0528(2) Uani 1 d . . S1 S 0.85307(11) 0.73157(9) 0.6120(2) 0.0554(3) Uani 1 d . . C1 C 0.8155(5) 0.8149(4) 0.9627(8) 0.0701(15) Uani 1 d . . O1 O 0.8735(4) 0.8496(4) 1.0815(6) 0.125(2) Uani 1 d . . C2 C 0.8870(5) 0.5970(4) 0.9190(9) 0.075(2) Uani 1 d . . O2 O 0.9481(4) 0.6017(3) 1.0489(7) 0.110(2) Uani 1 d . . C3 C 0.8476(5) 0.4901(4) 0.6013(9) 0.081(2) Uani 1 d . . O3 O 0.8820(5) 0.4250(3) 0.5353(8) 0.137(2) Uani 1 d . . O4 O 0.5758(3) 0.5056(3) 0.8312(5) 0.0787(11) Uani 1 d . . C4 C 0.6604(5) 0.5398(4) 0.7864(7) 0.0592(13) Uani 1 d . . O5 O 0.7139(4) 0.5417(4) 0.2042(6) 0.109(2) Uani 1 d . . C5 C 0.7012(5) 0.5984(4) 0.3050(8) 0.075(2) Uani 1 d . . O6 O 0.4370(3) 0.6279(3) 0.5345(5) 0.0808(11) Uani 1 d . . C6 C 0.5313(5) 0.6509(4) 0.5137(6) 0.0612(13) Uani 1 d . . O7 O 0.6293(4) 0.8671(3) 0.2746(5) 0.0952(14) Uani 1 d . . C7 C 0.6480(5) 0.7983(4) 0.3535(7) 0.0664(14) Uani 1 d . . C8 C 0.3962(4) 0.8071(3) 0.9055(6) 0.0485(11) Uani 1 d . . C9 C 0.3549(5) 0.7161(4) 0.9584(9) 0.087(2) Uani 1 d . . H9 H 0.4024(5) 0.6618(4) 0.9617(9) 0.072(5) Uiso 1 calc R . C10 C 0.2444(6) 0.7038(4) 1.0065(11) 0.113(3) Uani 1 d . . H10 H 0.2185(6) 0.6420(4) 1.0449(11) 0.072(5) Uiso 1 calc R . C11 C 0.1729(5) 0.7817(4) 0.9981(8) 0.084(2) Uani 1 d . . H11 H 0.0975(5) 0.7727(4) 1.0286(8) 0.072(5) Uiso 1 calc R . C12 C 0.2110(5) 0.8724(4) 0.9453(7) 0.0668(14) Uani 1 d . . H12 H 0.1619(5) 0.9257(4) 0.9395(7) 0.072(5) Uiso 1 calc R . C13 C 0.3228(4) 0.8853(4) 0.9003(6) 0.0569(13) Uani 1 d . . H13 H 0.3492(4) 0.9480(4) 0.8659(6) 0.072(5) Uiso 1 calc R . C14 C 0.5134(4) 0.8169(3) 0.8494(5) 0.0452(11) Uani 1 d . . O15 O 0.5767(3) 0.7411(2) 0.8606(4) 0.0491(8) Uani 1 d . . C16 C 0.5613(4) 0.9049(3) 0.7813(6) 0.0482(11) Uani 1 d . . H16 H 0.5208(4) 0.9634(3) 0.7705(6) 0.072(5) Uiso 1 calc R . C17 C 0.6707(4) 0.8993(3) 0.7320(6) 0.0446(11) Uani 1 d . . C18 C 0.7320(4) 0.9871(3) 0.6646(6) 0.0489(11) Uani 1 d . . C19 C 0.6713(4) 1.0677(4) 0.5993(6) 0.0608(13) Uani 1 d . . H19 H 0.5893(4) 1.0657(4) 0.5942(6) 0.072(5) Uiso 1 calc R . C20 C 0.7297(5) 1.1508(4) 0.5415(7) 0.073(2) Uani 1 d . . H20 H 0.6865(5) 1.2041(4) 0.4990(7) 0.072(5) Uiso 1 calc R . C21 C 0.8494(5) 1.1562(4) 0.5458(7) 0.072(2) Uani 1 d . . H21 H 0.8881(5) 1.2124(4) 0.5063(7) 0.072(5) Uiso 1 calc R . C22 C 0.9125(5) 1.0771(4) 0.6097(7) 0.0665(15) Uani 1 d . . H22 H 0.9945(5) 1.0802(4) 0.6144(7) 0.072(5) Uiso 1 calc R . C23 C 0.8549(4) 0.9931(3) 0.6668(6) 0.0564(13) Uani 1 d . . H23 H 0.8985(4) 0.9397(3) 0.7073(6) 0.072(5) 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 0.0417(4) 0.0439(4) 0.0548(4) -0.0007(3) 0.0128(3) 0.0045(3) Co2 0.0469(4) 0.0437(4) 0.0761(5) 0.0051(3) 0.0190(3) 0.0064(3) Co3 0.0579(4) 0.0486(4) 0.0544(4) -0.0015(3) 0.0179(3) 0.0017(3) S1 0.0458(7) 0.0467(7) 0.0786(9) -0.0004(6) 0.0266(6) 0.0003(5) C1 0.049(3) 0.083(4) 0.078(4) -0.004(3) 0.008(3) 0.017(3) O1 0.092(4) 0.172(5) 0.097(4) -0.043(3) -0.031(3) 0.024(3) C2 0.054(4) 0.064(4) 0.105(5) 0.017(3) 0.006(3) 0.003(3) O2 0.082(3) 0.105(3) 0.129(4) 0.028(3) -0.025(3) -0.001(3) C3 0.084(4) 0.051(3) 0.119(5) 0.004(3) 0.043(4) 0.014(3) O3 0.164(5) 0.070(3) 0.195(6) -0.018(3) 0.080(5) 0.040(3) O4 0.067(3) 0.079(3) 0.091(3) 0.018(2) 0.022(2) -0.010(2) C4 0.059(3) 0.051(3) 0.067(3) 0.010(3) 0.009(3) 0.002(3) O5 0.132(4) 0.104(3) 0.095(3) -0.039(3) 0.041(3) 0.000(3) C5 0.095(5) 0.064(4) 0.069(4) -0.011(3) 0.029(3) -0.002(3) O6 0.054(2) 0.095(3) 0.093(3) -0.003(2) 0.013(2) -0.004(2) C6 0.064(4) 0.064(3) 0.054(3) -0.002(3) 0.005(3) 0.004(3) O7 0.136(4) 0.071(3) 0.077(3) 0.018(2) 0.006(3) 0.013(3) C7 0.077(4) 0.065(3) 0.056(3) -0.002(3) 0.010(3) 0.002(3) C8 0.046(3) 0.045(3) 0.059(3) -0.005(2) 0.022(2) 0.000(2) C9 0.071(4) 0.059(4) 0.147(6) 0.019(4) 0.063(4) 0.015(3) C10 0.089(5) 0.059(4) 0.215(9) 0.032(4) 0.090(5) 0.009(3) C11 0.060(4) 0.080(4) 0.124(5) -0.006(4) 0.048(4) 0.003(3) C12 0.056(3) 0.064(3) 0.086(4) -0.006(3) 0.026(3) 0.015(3) C13 0.052(3) 0.049(3) 0.074(3) -0.003(2) 0.023(3) 0.000(2) C14 0.042(3) 0.049(3) 0.046(3) -0.005(2) 0.011(2) 0.002(2) O15 0.050(2) 0.044(2) 0.059(2) 0.0037(14) 0.023(2) 0.0070(15) C16 0.043(3) 0.042(3) 0.061(3) 0.004(2) 0.013(2) 0.005(2) C17 0.041(3) 0.043(3) 0.048(3) -0.003(2) 0.005(2) -0.006(2) C18 0.047(3) 0.047(3) 0.053(3) -0.012(2) 0.011(2) -0.005(2) C19 0.048(3) 0.060(3) 0.074(4) 0.011(3) 0.008(3) -0.001(2) C20 0.081(4) 0.055(3) 0.086(4) 0.021(3) 0.018(3) 0.007(3) C21 0.088(5) 0.055(3) 0.080(4) 0.001(3) 0.039(3) -0.014(3) C22 0.053(3) 0.061(3) 0.086(4) -0.019(3) 0.026(3) -0.017(3) C23 0.049(3) 0.048(3) 0.073(3) -0.011(2) 0.018(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C1 1.753(6) . ? Co1 C17 1.926(4) . ? Co1 O15 1.953(3) . ? Co1 S1 2.1316(14) . ? Co1 Co3 2.5163(11) . ? Co1 Co2 2.5342(9) . ? Co2 C2 1.770(7) . ? Co2 C4 1.785(5) . ? Co2 C3 1.831(6) . ? Co2 S1 2.1650(14) . ? Co2 Co3 2.5582(11) . ? Co3 C7 1.794(6) . ? Co3 C6 1.803(6) . ? Co3 C5 1.832(6) . ? Co3 S1 2.1487(15) . ? C1 O1 1.131(6) . ? C2 O2 1.145(7) . ? C3 O3 1.122(6) . ? O4 C4 1.149(6) . ? O5 C5 1.114(6) . ? O6 C6 1.137(6) . ? O7 C7 1.134(6) . ? C8 C9 1.370(6) . ? C8 C13 1.376(6) . ? C8 C14 1.471(6) . ? C9 C10 1.373(7) . ? C10 C11 1.357(8) . ? C11 C12 1.355(7) . ? C12 C13 1.378(7) . ? C14 O15 1.276(5) . ? C14 C16 1.414(6) . ? C16 C17 1.369(6) . ? C17 C18 1.476(6) . ? C18 C19 1.382(6) . ? C18 C23 1.398(6) . ? C19 C20 1.380(7) . ? C20 C21 1.360(7) . ? C21 C22 1.376(7) . ? C22 C23 1.382(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Co1 C17 89.5(2) . . ? C1 Co1 O15 99.5(2) . . ? C17 Co1 O15 84.25(15) . . ? C1 Co1 S1 103.1(2) . . ? C17 Co1 S1 111.82(13) . . ? O15 Co1 S1 152.19(10) . . ? C1 Co1 Co3 157.3(2) . . ? C17 Co1 Co3 100.50(13) . . ? O15 Co1 Co3 101.76(9) . . ? S1 Co1 Co3 54.31(4) . . ? C1 Co1 Co2 106.2(2) . . ? C17 Co1 Co2 160.71(13) . . ? O15 Co1 Co2 103.56(9) . . ? S1 Co1 Co2 54.47(4) . . ? Co3 Co1 Co2 60.87(3) . . ? C2 Co2 C4 98.6(2) . . ? C2 Co2 C3 102.5(3) . . ? C4 Co2 C3 104.8(2) . . ? C2 Co2 S1 100.5(2) . . ? C4 Co2 S1 138.2(2) . . ? C3 Co2 S1 106.7(2) . . ? C2 Co2 Co1 91.9(2) . . ? C4 Co2 Co1 89.5(2) . . ? C3 Co2 Co1 157.7(2) . . ? S1 Co2 Co1 53.25(4) . . ? C2 Co2 Co3 148.5(2) . . ? C4 Co2 Co3 93.7(2) . . ? C3 Co2 Co3 102.2(2) . . ? S1 Co2 Co3 53.33(4) . . ? Co1 Co2 Co3 59.22(3) . . ? C7 Co3 C6 99.4(2) . . ? C7 Co3 C5 101.1(2) . . ? C6 Co3 C5 102.5(2) . . ? C7 Co3 S1 101.2(2) . . ? C6 Co3 S1 140.7(2) . . ? C5 Co3 S1 105.9(2) . . ? C7 Co3 Co1 100.0(2) . . ? C6 Co3 Co1 90.0(2) . . ? C5 Co3 Co1 153.3(2) . . ? S1 Co3 Co1 53.68(4) . . ? C7 Co3 Co2 153.7(2) . . ? C6 Co3 Co2 97.4(2) . . ? C5 Co3 Co2 94.8(2) . . ? S1 Co3 Co2 53.92(4) . . ? Co1 Co3 Co2 59.91(3) . . ? Co1 S1 Co3 72.01(5) . . ? Co1 S1 Co2 72.28(5) . . ? Co3 S1 Co2 72.75(5) . . ? O1 C1 Co1 176.9(6) . . ? O2 C2 Co2 178.6(5) . . ? O3 C3 Co2 177.3(6) . . ? O4 C4 Co2 179.5(5) . . ? O5 C5 Co3 178.2(5) . . ? O6 C6 Co3 178.5(5) . . ? O7 C7 Co3 178.8(5) . . ? C9 C8 C13 117.8(4) . . ? C9 C8 C14 119.7(4) . . ? C13 C8 C14 122.4(4) . . ? C8 C9 C10 121.1(5) . . ? C11 C10 C9 120.1(5) . . ? C12 C11 C10 120.3(5) . . ? C11 C12 C13 119.7(5) . . ? C12 C13 C8 121.1(4) . . ? O15 C14 C16 117.0(4) . . ? O15 C14 C8 118.4(4) . . ? C16 C14 C8 124.5(4) . . ? C14 O15 Co1 112.4(3) . . ? C17 C16 C14 116.3(4) . . ? C16 C17 C18 121.5(4) . . ? C16 C17 Co1 110.0(3) . . ? C18 C17 Co1 128.5(3) . . ? C19 C18 C23 117.0(4) . . ? C19 C18 C17 121.8(4) . . ? C23 C18 C17 121.2(4) . . ? C20 C19 C18 121.4(5) . . ? C21 C20 C19 121.0(5) . . ? C20 C21 C22 119.0(5) . . ? C21 C22 C23 120.4(5) . . ? C22 C23 C18 121.1(5) . . ? _refine_diff_density_max 0.343 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.056