# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 loop_ _publ_author_address ; State Key Lab of Rare Earth Resource Utilization Changchun Institute of Applied Chemistry CAS, Changchun 130022 P.R. China ; #TrackingRef '- CCDC872774-872776.CIF' _publ_contact_author 'Prof Dr Wuping Liao' _publ_contact_author_email wpliao@ciac.jl.cn _publ_contact_author_name 'Prof Dr Wuping Liao' _publ_author_name 'Wuping Liao' data_CIAC-201 _database_code_depnum_ccdc_archive 'CCDC 872774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '((CH3)4N)4 ((Co4Cl(C40H44O4S4))4 (C8H4O4)8' _chemical_melting_point ? _chemical_formula_moiety 'C240 H256 Cl4 Co16 N4 O48 S16' _chemical_formula_sum 'C240 H256 Cl4 Co16 N4 O48 S16' # FOUR (CH3)4N+ cations are included by charge balance. # Unidentified solvents are not included. _chemical_formula_weight 5562.13 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I m m m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 21.3405(5) _cell_length_b 30.1083(6) _cell_length_c 30.8273(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19807.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9903 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 22.82 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.933 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5384 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9027 _exptl_absorpt_correction_T_max 0.9239 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58520 _diffrn_reflns_av_R_equivalents 0.1343 _diffrn_reflns_av_sigmaI/netI 0.1043 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 23.01 _reflns_number_total 7434 _reflns_number_gt 4051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-hydrogen atoms except the disordered butyl carbon atoms were refined anisotropically. ; _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^)+(0.1326P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7434 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1248 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.2458 _refine_ls_wR_factor_gt 0.2152 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.12287(4) -0.27865(5) 0.0460(4) Uani 1 2 d S . . Co2 Co 0.10772(4) 0.17977(3) -0.32658(3) 0.0443(3) Uani 1 1 d . . . Co3 Co 0.0000 0.23492(4) -0.37718(4) 0.0454(4) Uani 1 2 d S . . Cl1 Cl 0.0000 0.15038(8) -0.35905(8) 0.0462(7) Uani 1 2 d S . . S1 S 0.17947(9) 0.22413(6) -0.27810(6) 0.0474(5) Uani 1 1 d . . . S2 S 0.0000 0.31935(8) -0.36514(10) 0.0529(8) Uani 1 2 d S . . S3 S 0.0000 0.12419(9) -0.19597(9) 0.0511(7) Uani 1 2 d S . . O1 O 0.0655(2) 0.23795(14) -0.33139(14) 0.0449(12) Uani 1 1 d . . . O2 O 0.0651(2) 0.16939(13) -0.26973(15) 0.0412(12) Uani 1 1 d . . . O3 O -0.1456(2) 0.11904(15) -0.32545(17) 0.0597(15) Uani 1 1 d . . . O4 O -0.0684(2) 0.07827(14) -0.29093(17) 0.0565(14) Uani 1 1 d . . . O5 O 0.1453(2) 0.19054(15) -0.38663(16) 0.0480(12) Uani 1 1 d . . . O6 O 0.0687(2) 0.22617(15) -0.42150(15) 0.0517(13) Uani 1 1 d . . . C1 C 0.0909(3) 0.2760(2) -0.3167(2) 0.0492(19) Uani 1 1 d . . . C2 C 0.1437(3) 0.2749(2) -0.2901(2) 0.0478(19) Uani 1 1 d . . . C3 C 0.1721(4) 0.3150(3) -0.2780(3) 0.074(3) Uani 1 1 d . . . H3A H 0.2082 0.3140 -0.2611 0.089 Uiso 1 1 calc R . . C4 C 0.1482(4) 0.3570(3) -0.2903(3) 0.082(3) Uani 1 1 d . . . C5 C 0.0943(4) 0.3575(3) -0.3160(3) 0.072(3) Uani 1 1 d . . . H5A H 0.0768 0.3847 -0.3238 0.087 Uiso 1 1 calc R . . C6 C 0.0664(3) 0.3189(2) -0.3302(2) 0.051(2) Uani 1 1 d . . . C7 C 0.0909(3) 0.1779(2) -0.2328(2) 0.0380(17) Uani 1 1 d . . . C8 C 0.0671(3) 0.1613(2) -0.1932(3) 0.052(2) Uani 1 1 d . . . C9 C 0.0955(4) 0.1684(3) -0.1541(3) 0.066(2) Uani 1 1 d . . . H9A H 0.0787 0.1560 -0.1290 0.079 Uiso 1 1 calc R . . C10 C 0.1494(4) 0.1941(3) -0.1520(3) 0.073(3) Uani 1 1 d . . . C11 C 0.1726(4) 0.2123(3) -0.1906(3) 0.064(2) Uani 1 1 d . . . H11A H 0.2080 0.2303 -0.1896 0.076 Uiso 1 1 calc R . . C12 C 0.1451(4) 0.2044(2) -0.2287(2) 0.052(2) Uani 1 1 d . . . C13 C 0.1801(6) 0.4005(4) -0.2790(4) 0.109(4) Uiso 1 1 d . . . C14 C 0.1814(6) 0.2001(4) -0.1056(4) 0.114(4) Uiso 1 1 d . . . C15 C 0.1880(8) 0.4292(6) -0.3171(5) 0.195(7) Uiso 1 1 d . . . H15A H 0.2152 0.4534 -0.3099 0.293 Uiso 1 1 calc R . . H15B H 0.1479 0.4405 -0.3258 0.293 Uiso 1 1 calc R . . H15C H 0.2059 0.4123 -0.3404 0.293 Uiso 1 1 calc R . . C16 C 0.2468(5) 0.3949(4) -0.2625(3) 0.110(4) Uiso 1 1 d . . . H16A H 0.2459 0.3828 -0.2337 0.166 Uiso 1 1 calc R . . H16B H 0.2673 0.4233 -0.2621 0.166 Uiso 1 1 calc R . . H16C H 0.2692 0.3751 -0.2813 0.166 Uiso 1 1 calc R . . C17 C 0.1406(7) 0.4244(4) -0.2507(4) 0.153(5) Uiso 1 1 d . . . H17A H 0.1352 0.4079 -0.2243 0.229 Uiso 1 1 calc R . . H17B H 0.1006 0.4288 -0.2642 0.229 Uiso 1 1 calc R . . H17C H 0.1591 0.4527 -0.2443 0.229 Uiso 1 1 calc R . . C18 C 0.2486(5) 0.2186(4) -0.1106(3) 0.115(4) Uiso 1 1 d . . . H18A H 0.2738 0.1977 -0.1265 0.172 Uiso 1 1 calc R . . H18B H 0.2666 0.2232 -0.0824 0.172 Uiso 1 1 calc R . . H18C H 0.2473 0.2462 -0.1260 0.172 Uiso 1 1 calc R . . C19 C 0.1876(7) 0.1534(5) -0.0810(4) 0.167(5) Uiso 1 1 d . . . H19A H 0.2075 0.1323 -0.0998 0.250 Uiso 1 1 calc R . . H19B H 0.1467 0.1429 -0.0732 0.250 Uiso 1 1 calc R . . H19C H 0.2124 0.1572 -0.0553 0.250 Uiso 1 1 calc R . . C20 C 0.1460(7) 0.2261(5) -0.0787(4) 0.165(6) Uiso 1 1 d . . . H20A H 0.1644 0.2263 -0.0502 0.247 Uiso 1 1 calc R . . H20B H 0.1043 0.2143 -0.0770 0.247 Uiso 1 1 calc R . . H20C H 0.1445 0.2558 -0.0898 0.247 Uiso 1 1 calc R . . C21 C -0.1201(4) 0.0838(3) -0.3102(3) 0.058(2) Uani 1 1 d . . . C22 C -0.1542(3) 0.0396(2) -0.3178(3) 0.058(2) Uani 1 1 d . . . C23 C -0.2172(4) 0.0399(2) -0.3333(3) 0.070(3) Uani 1 1 d . . . H23A H -0.2381 0.0666 -0.3376 0.084 Uiso 1 1 calc R . . C24 C -0.2467(5) 0.0000 -0.3419(4) 0.086(4) Uani 1 2 d S . . H24A H -0.2869 0.0000 -0.3536 0.103 Uiso 1 2 calc SR . . C25 C -0.1257(5) 0.0000 -0.3106(4) 0.054(3) Uani 1 2 d S . . H25A H -0.0848 0.0000 -0.3002 0.065 Uiso 1 2 calc SR . . C26 C 0.1200(4) 0.2071(2) -0.4194(2) 0.0462(19) Uani 1 1 d . . . C27 C 0.1552(3) 0.2019(3) -0.4610(2) 0.054(2) Uani 1 1 d . . . C28 C 0.2189(4) 0.1903(3) -0.4625(3) 0.074(3) Uani 1 1 d . . . H28A H 0.2403 0.1859 -0.4365 0.089 Uiso 1 1 calc R . . C29 C 0.2499(5) 0.1853(4) -0.5000 0.076(4) Uani 1 2 d S . . H29A H 0.2924 0.1784 -0.5000 0.092 Uiso 1 2 calc SR . . C30 C 0.1265(5) 0.2091(3) -0.5000 0.050(3) Uani 1 2 d S . . H30A H 0.0854 0.2194 -0.5000 0.060 Uiso 1 2 calc SR . . 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 0.0233(8) 0.0444(8) 0.0702(10) 0.0036(7) 0.000 0.000 Co2 0.0264(6) 0.0456(6) 0.0608(7) 0.0033(5) -0.0013(5) -0.0017(4) Co3 0.0246(8) 0.0529(8) 0.0589(10) 0.0028(7) 0.000 0.000 Cl1 0.0249(13) 0.0495(14) 0.0643(17) -0.0049(13) 0.000 0.000 S1 0.0297(10) 0.0477(10) 0.0648(13) 0.0032(9) -0.0041(10) -0.0032(9) S2 0.0314(15) 0.0490(15) 0.078(2) 0.0101(14) 0.000 0.000 S3 0.0291(15) 0.0595(16) 0.0649(19) 0.0131(14) 0.000 0.000 O1 0.030(3) 0.041(3) 0.064(3) 0.005(2) -0.007(2) -0.008(2) O2 0.031(3) 0.031(2) 0.061(3) 0.004(2) 0.001(2) -0.011(2) O3 0.030(3) 0.042(3) 0.107(4) 0.000(3) -0.008(3) 0.011(2) O4 0.020(3) 0.048(3) 0.101(4) -0.001(3) -0.007(3) -0.005(2) O5 0.024(3) 0.059(3) 0.061(3) 0.000(3) -0.001(3) 0.002(2) O6 0.027(3) 0.068(3) 0.060(3) 0.011(3) 0.002(2) 0.006(3) C1 0.031(4) 0.063(5) 0.053(5) -0.003(4) 0.009(4) -0.003(4) C2 0.037(4) 0.036(4) 0.070(5) 0.005(4) -0.011(4) -0.013(3) C3 0.054(6) 0.063(5) 0.104(7) -0.005(5) -0.032(5) -0.006(5) C4 0.061(6) 0.050(5) 0.135(8) -0.009(5) -0.052(6) -0.002(4) C5 0.064(6) 0.046(5) 0.108(7) 0.016(5) -0.017(6) 0.003(4) C6 0.043(5) 0.044(4) 0.067(5) -0.002(4) -0.019(4) -0.001(4) C7 0.050(5) 0.036(4) 0.029(4) -0.004(3) -0.006(4) 0.005(4) C8 0.021(4) 0.065(5) 0.070(6) 0.020(4) -0.008(4) -0.013(4) C9 0.040(5) 0.084(6) 0.074(6) 0.031(5) -0.013(5) -0.017(5) C10 0.072(7) 0.098(6) 0.049(6) 0.011(5) -0.018(5) -0.022(6) C11 0.037(5) 0.085(6) 0.069(6) 0.008(5) -0.007(5) -0.014(4) C12 0.042(5) 0.050(4) 0.064(6) 0.013(4) -0.020(4) -0.008(4) C21 0.029(5) 0.075(6) 0.070(6) -0.017(5) -0.003(4) -0.012(4) C22 0.031(4) 0.050(4) 0.091(6) 0.007(4) 0.000(4) -0.002(4) C23 0.035(5) 0.048(5) 0.128(8) -0.001(5) -0.015(5) -0.002(4) C24 0.033(7) 0.091(10) 0.134(12) 0.000 -0.039(8) 0.000 C25 0.032(6) 0.020(5) 0.112(9) 0.000 -0.006(6) 0.000 C26 0.035(5) 0.057(4) 0.047(5) 0.007(4) -0.014(4) -0.006(4) C27 0.032(4) 0.087(6) 0.043(5) 0.007(4) -0.011(4) -0.006(4) C28 0.041(5) 0.130(8) 0.052(6) 0.011(5) -0.026(5) 0.009(5) C29 0.031(7) 0.136(12) 0.062(9) 0.000 0.000 0.030(7) C30 0.034(6) 0.077(7) 0.038(7) 0.000 0.000 0.001(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 O2 1.992(4) . ? Co1 O2 1.992(4) 11 ? Co1 O4 2.019(4) . ? Co1 O4 2.019(4) 11 ? Co1 S3 2.549(3) . ? Co1 Cl1 2.613(3) . ? Co2 O1 1.975(4) . ? Co2 O2 1.999(5) . ? Co2 O3 1.999(5) 11 ? Co2 O5 2.043(5) . ? Co2 S1 2.522(2) . ? Co2 Cl1 2.6588(15) . ? Co3 O1 1.989(4) 11 ? Co3 O1 1.989(4) . ? Co3 O6 2.021(5) 11 ? Co3 O6 2.021(5) . ? Co3 S2 2.569(3) . ? Co3 Cl1 2.606(3) . ? Cl1 Co2 2.6589(15) 11 ? S1 C2 1.748(7) . ? S1 C12 1.792(8) . ? S2 C6 1.779(7) . ? S2 C6 1.779(7) 11 ? S3 C8 1.819(7) 11 ? S3 C8 1.819(7) . ? O1 C1 1.345(8) . ? O2 C7 1.290(7) . ? O3 C21 1.282(9) . ? O3 Co2 1.999(5) 11 ? O4 C21 1.264(8) . ? O5 C26 1.248(8) . ? O6 C26 1.238(8) . ? C1 C2 1.393(9) . ? C1 C6 1.455(9) . ? C2 C3 1.405(9) . ? C3 C4 1.413(10) . ? C3 H3A 0.9300 . ? C4 C5 1.397(11) . ? C4 C13 1.518(13) . ? C5 C6 1.378(10) . ? C5 H5A 0.9300 . ? C7 C12 1.410(10) . ? C7 C8 1.414(9) . ? C8 C9 1.366(10) . ? C9 C10 1.389(11) . ? C9 H9A 0.9300 . ? C10 C11 1.402(10) . ? C10 C14 1.593(13) . ? C11 C12 1.336(10) . ? C11 H11A 0.9300 . ? C13 C17 1.411(15) . ? C13 C15 1.465(16) . ? C13 C16 1.520(14) . ? C14 C20 1.369(15) . ? C14 C18 1.547(15) . ? C14 C19 1.602(16) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.535(10) . ? C22 C25 1.356(8) . ? C22 C23 1.427(10) . ? C23 C24 1.382(9) . ? C23 H23A 0.9300 . ? C24 C23 1.382(9) 12 ? C24 H24A 0.9300 . ? C25 C22 1.356(8) 12 ? C25 H25A 0.9300 . ? C26 C27 1.495(10) . ? C27 C30 1.366(8) . ? C27 C28 1.405(10) . ? C28 C29 1.342(9) . ? C28 H28A 0.9300 . ? C29 C28 1.342(9) 10_554 ? C29 H29A 0.9300 . ? C30 C27 1.366(8) 10_554 ? C30 H30A 0.9300 . ? 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 O2 Co1 O2 88.5(2) . 11 ? O2 Co1 O4 176.1(2) . . ? O2 Co1 O4 89.40(18) 11 . ? O2 Co1 O4 89.40(18) . 11 ? O2 Co1 O4 176.1(2) 11 11 ? O4 Co1 O4 92.6(3) . 11 ? O2 Co1 S3 81.43(15) . . ? O2 Co1 S3 81.43(15) 11 . ? O4 Co1 S3 101.42(16) . . ? O4 Co1 S3 101.41(16) 11 . ? O2 Co1 Cl1 84.73(14) . . ? O2 Co1 Cl1 84.73(14) 11 . ? O4 Co1 Cl1 91.89(16) . . ? O4 Co1 Cl1 91.89(16) 11 . ? S3 Co1 Cl1 160.63(10) . . ? O1 Co2 O2 89.84(18) . . ? O1 Co2 O3 175.3(2) . 11 ? O2 Co2 O3 91.46(19) . 11 ? O1 Co2 O5 88.28(18) . . ? O2 Co2 O5 176.04(19) . . ? O3 Co2 O5 90.1(2) 11 . ? O1 Co2 S1 81.46(13) . . ? O2 Co2 S1 80.77(13) . . ? O3 Co2 S1 103.22(15) 11 . ? O5 Co2 S1 102.39(14) . . ? O1 Co2 Cl1 82.69(13) . . ? O2 Co2 Cl1 83.38(14) . . ? O3 Co2 Cl1 92.95(15) 11 . ? O5 Co2 Cl1 92.91(14) . . ? S1 Co2 Cl1 157.55(7) . . ? O1 Co3 O1 89.3(3) 11 . ? O1 Co3 O6 88.61(18) 11 11 ? O1 Co3 O6 174.64(19) . 11 ? O1 Co3 O6 174.64(19) 11 . ? O1 Co3 O6 88.61(18) . . ? O6 Co3 O6 93.0(3) 11 . ? O1 Co3 S2 81.49(14) 11 . ? O1 Co3 S2 81.49(14) . . ? O6 Co3 S2 103.10(14) 11 . ? O6 Co3 S2 103.10(14) . . ? O1 Co3 Cl1 83.84(13) 11 . ? O1 Co3 Cl1 83.84(13) . . ? O6 Co3 Cl1 91.01(14) 11 . ? O6 Co3 Cl1 91.01(14) . . ? S2 Co3 Cl1 159.31(11) . . ? Co3 Cl1 Co1 120.86(10) . . ? Co3 Cl1 Co2 75.86(6) . . ? Co1 Cl1 Co2 75.43(6) . . ? Co3 Cl1 Co2 75.86(6) . 11 ? Co1 Cl1 Co2 75.42(6) . 11 ? Co2 Cl1 Co2 119.67(10) . 11 ? C2 S1 C12 106.9(3) . . ? C2 S1 Co2 94.1(2) . . ? C12 S1 Co2 94.5(2) . . ? C6 S2 C6 105.5(5) . 11 ? C6 S2 Co3 94.6(2) . . ? C6 S2 Co3 94.6(2) 11 . ? C8 S3 C8 103.9(5) 11 . ? C8 S3 Co1 93.2(3) 11 . ? C8 S3 Co1 93.2(3) . . ? C1 O1 Co2 123.1(4) . . ? C1 O1 Co3 124.1(4) . . ? Co2 O1 Co3 109.4(2) . . ? C7 O2 Co1 124.0(4) . . ? C7 O2 Co2 123.2(4) . . ? Co1 O2 Co2 107.8(2) . . ? C21 O3 Co2 126.3(4) . 11 ? C21 O4 Co1 129.2(5) . . ? C26 O5 Co2 128.8(5) . . ? C26 O6 Co3 131.7(5) . . ? O1 C1 C2 120.2(6) . . ? O1 C1 C6 121.0(6) . . ? C2 C1 C6 118.7(6) . . ? C1 C2 C3 119.1(7) . . ? C1 C2 S1 120.0(5) . . ? C3 C2 S1 120.5(6) . . ? C2 C3 C4 122.7(7) . . ? C2 C3 H3A 118.6 . . ? C4 C3 H3A 118.6 . . ? C5 C4 C3 117.4(7) . . ? C5 C4 C13 119.3(8) . . ? C3 C4 C13 123.2(8) . . ? C6 C5 C4 121.8(7) . . ? C6 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C5 C6 C1 120.2(7) . . ? C5 C6 S2 122.1(6) . . ? C1 C6 S2 117.8(5) . . ? O2 C7 C12 122.8(6) . . ? O2 C7 C8 122.5(7) . . ? C12 C7 C8 114.7(6) . . ? C9 C8 C7 123.3(6) . . ? C9 C8 S3 119.0(6) . . ? C7 C8 S3 117.4(6) . . ? C8 C9 C10 119.7(7) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C9 C10 C11 118.1(7) . . ? C9 C10 C14 117.4(8) . . ? C11 C10 C14 124.4(8) . . ? C12 C11 C10 121.4(8) . . ? C12 C11 H11A 119.3 . . ? C10 C11 H11A 119.3 . . ? C11 C12 C7 122.7(7) . . ? C11 C12 S1 120.5(6) . . ? C7 C12 S1 116.6(6) . . ? C17 C13 C15 105.3(12) . . ? C17 C13 C4 108.3(11) . . ? C15 C13 C4 112.1(11) . . ? C17 C13 C16 114.1(11) . . ? C15 C13 C16 103.1(11) . . ? C4 C13 C16 113.6(10) . . ? C20 C14 C18 111.5(11) . . ? C20 C14 C10 111.9(11) . . ? C18 C14 C10 110.5(9) . . ? C20 C14 C19 105.1(11) . . ? C18 C14 C19 106.6(10) . . ? C10 C14 C19 111.1(10) . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 O3 130.6(7) . . ? O4 C21 C22 111.8(7) . . ? O3 C21 C22 117.5(6) . . ? C25 C22 C23 118.9(7) . . ? C25 C22 C21 121.6(7) . . ? C23 C22 C21 119.5(6) . . ? C24 C23 C22 119.3(8) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 C23 120.6(10) . 12 ? C23 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 12 . ? C22 C25 C22 123.0(10) . 12 ? C22 C25 H25A 118.5 . . ? C22 C25 H25A 118.5 12 . ? O6 C26 O5 127.6(7) . . ? O6 C26 C27 116.5(7) . . ? O5 C26 C27 115.9(7) . . ? C30 C27 C28 116.4(8) . . ? C30 C27 C26 121.0(7) . . ? C28 C27 C26 122.6(7) . . ? C29 C28 C27 122.2(8) . . ? C29 C28 H28A 118.9 . . ? C27 C28 H28A 118.9 . . ? C28 C29 C28 119.2(10) 10_554 . ? C28 C29 H29A 120.4 10_554 . ? C28 C29 H29A 120.4 . . ? C27 C30 C27 123.3(10) . 10_554 ? C27 C30 H30A 118.4 . . ? C27 C30 H30A 118.4 10_554 . ? 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 O1 Co3 Cl1 Co1 -45.00(13) 11 . . . ? O1 Co3 Cl1 Co1 45.00(13) . . . . ? O6 Co3 Cl1 Co1 -133.49(14) 11 . . . ? O6 Co3 Cl1 Co1 133.49(14) . . . . ? S2 Co3 Cl1 Co1 0.0 . . . . ? O1 Co3 Cl1 Co2 -108.07(14) 11 . . . ? O1 Co3 Cl1 Co2 -18.07(14) . . . . ? O6 Co3 Cl1 Co2 163.43(15) 11 . . . ? O6 Co3 Cl1 Co2 70.42(14) . . . . ? S2 Co3 Cl1 Co2 -63.07(4) . . . . ? O1 Co3 Cl1 Co2 18.07(14) 11 . . 11 ? O1 Co3 Cl1 Co2 108.07(14) . . . 11 ? O6 Co3 Cl1 Co2 -70.42(14) 11 . . 11 ? O6 Co3 Cl1 Co2 -163.44(15) . . . 11 ? S2 Co3 Cl1 Co2 63.07(4) . . . 11 ? O2 Co1 Cl1 Co3 -44.47(12) . . . . ? O2 Co1 Cl1 Co3 44.46(12) 11 . . . ? O4 Co1 Cl1 Co3 133.68(13) . . . . ? O4 Co1 Cl1 Co3 -133.69(13) 11 . . . ? S3 Co1 Cl1 Co3 0.0 . . . . ? O2 Co1 Cl1 Co2 18.83(13) . . . . ? O2 Co1 Cl1 Co2 107.76(13) 11 . . . ? O4 Co1 Cl1 Co2 -163.02(14) . . . . ? O4 Co1 Cl1 Co2 -70.39(14) 11 . . . ? S3 Co1 Cl1 Co2 63.29(4) . . . . ? O2 Co1 Cl1 Co2 -107.76(13) . . . 11 ? O2 Co1 Cl1 Co2 -18.83(13) 11 . . 11 ? O4 Co1 Cl1 Co2 70.39(14) . . . 11 ? O4 Co1 Cl1 Co2 163.02(14) 11 . . 11 ? S3 Co1 Cl1 Co2 -63.29(4) . . . 11 ? O1 Co2 Cl1 Co3 18.25(14) . . . . ? O2 Co2 Cl1 Co3 108.94(13) . . . . ? O3 Co2 Cl1 Co3 -159.93(16) 11 . . . ? O5 Co2 Cl1 Co3 -69.64(14) . . . . ? S1 Co2 Cl1 Co3 63.6(2) . . . . ? O1 Co2 Cl1 Co1 -109.49(14) . . . . ? O2 Co2 Cl1 Co1 -18.80(12) . . . . ? O3 Co2 Cl1 Co1 72.33(16) 11 . . . ? O5 Co2 Cl1 Co1 162.62(14) . . . . ? S1 Co2 Cl1 Co1 -64.1(2) . . . . ? O1 Co2 Cl1 Co2 -46.07(16) . . . 11 ? O2 Co2 Cl1 Co2 44.62(15) . . . 11 ? O3 Co2 Cl1 Co2 135.75(18) 11 . . 11 ? O5 Co2 Cl1 Co2 -133.96(16) . . . 11 ? S1 Co2 Cl1 Co2 -0.7(3) . . . 11 ? O1 Co2 S1 C2 -6.6(3) . . . . ? O2 Co2 S1 C2 -97.9(3) . . . . ? O3 Co2 S1 C2 172.8(3) 11 . . . ? O5 Co2 S1 C2 79.7(3) . . . . ? Cl1 Co2 S1 C2 -52.2(3) . . . . ? O1 Co2 S1 C12 100.7(3) . . . . ? O2 Co2 S1 C12 9.5(3) . . . . ? O3 Co2 S1 C12 -79.8(3) 11 . . . ? O5 Co2 S1 C12 -172.9(3) . . . . ? Cl1 Co2 S1 C12 55.2(3) . . . . ? O1 Co3 S2 C6 98.3(3) 11 . . . ? O1 Co3 S2 C6 7.7(3) . . . . ? O6 Co3 S2 C6 -175.1(3) 11 . . . ? O6 Co3 S2 C6 -78.9(3) . . . . ? Cl1 Co3 S2 C6 53.0(3) . . . . ? O1 Co3 S2 C6 -7.7(3) 11 . . 11 ? O1 Co3 S2 C6 -98.3(3) . . . 11 ? O6 Co3 S2 C6 78.9(3) 11 . . 11 ? O6 Co3 S2 C6 175.2(3) . . . 11 ? Cl1 Co3 S2 C6 -53.0(3) . . . 11 ? O2 Co1 S3 C8 96.9(3) . . . 11 ? O2 Co1 S3 C8 7.2(3) 11 . . 11 ? O4 Co1 S3 C8 -80.4(3) . . . 11 ? O4 Co1 S3 C8 -175.4(3) 11 . . 11 ? Cl1 Co1 S3 C8 52.1(2) . . . 11 ? O2 Co1 S3 C8 -7.2(3) . . . . ? O2 Co1 S3 C8 -96.9(3) 11 . . . ? O4 Co1 S3 C8 175.4(3) . . . . ? O4 Co1 S3 C8 80.4(3) 11 . . . ? Cl1 Co1 S3 C8 -52.1(2) . . . . ? O2 Co2 O1 C1 91.6(5) . . . . ? O3 Co2 O1 C1 -162(2) 11 . . . ? O5 Co2 O1 C1 -91.9(5) . . . . ? S1 Co2 O1 C1 10.9(5) . . . . ? Cl1 Co2 O1 C1 174.9(5) . . . . ? O2 Co2 O1 Co3 -108.3(2) . . . . ? O3 Co2 O1 Co3 -2(3) 11 . . . ? O5 Co2 O1 Co3 68.2(2) . . . . ? S1 Co2 O1 Co3 171.0(2) . . . . ? Cl1 Co2 O1 Co3 -24.95(17) . . . . ? O1 Co3 O1 C1 -90.8(5) 11 . . . ? O6 Co3 O1 C1 -158.3(19) 11 . . . ? O6 Co3 O1 C1 94.1(5) . . . . ? S2 Co3 O1 C1 -9.3(5) . . . . ? Cl1 Co3 O1 C1 -174.7(5) . . . . ? O1 Co3 O1 Co2 109.31(19) 11 . . . ? O6 Co3 O1 Co2 42(2) 11 . . . ? O6 Co3 O1 Co2 -65.7(2) . . . . ? S2 Co3 O1 Co2 -169.2(2) . . . . ? Cl1 Co3 O1 Co2 25.43(17) . . . . ? O2 Co1 O2 C7 93.6(5) 11 . . . ? O4 Co1 O2 C7 150(3) . . . . ? O4 Co1 O2 C7 -89.6(5) 11 . . . ? S3 Co1 O2 C7 12.0(5) . . . . ? Cl1 Co1 O2 C7 178.4(5) . . . . ? O2 Co1 O2 Co2 -110.72(17) 11 . . . ? O4 Co1 O2 Co2 -55(3) . . . . ? O4 Co1 O2 Co2 66.1(2) 11 . . . ? S3 Co1 O2 Co2 167.72(19) . . . . ? Cl1 Co1 O2 Co2 -25.87(17) . . . . ? O1 Co2 O2 C7 -95.9(5) . . . . ? O3 Co2 O2 C7 88.6(5) 11 . . . ? O5 Co2 O2 C7 -158(2) . . . . ? S1 Co2 O2 C7 -14.6(4) . . . . ? Cl1 Co2 O2 C7 -178.6(4) . . . . ? O1 Co2 O2 Co1 108.1(2) . . . . ? O3 Co2 O2 Co1 -67.3(2) 11 . . . ? O5 Co2 O2 Co1 46(3) . . . . ? S1 Co2 O2 Co1 -170.50(19) . . . . ? Cl1 Co2 O2 Co1 25.46(17) . . . . ? O2 Co1 O4 C21 -20(3) . . . . ? O2 Co1 O4 C21 35.8(6) 11 . . . ? O4 Co1 O4 C21 -140.9(6) 11 . . . ? S3 Co1 O4 C21 116.9(6) . . . . ? Cl1 Co1 O4 C21 -49.0(6) . . . . ? O1 Co2 O5 C26 -40.5(6) . . . . ? O2 Co2 O5 C26 21(3) . . . . ? O3 Co2 O5 C26 135.1(6) 11 . . . ? S1 Co2 O5 C26 -121.3(5) . . . . ? Cl1 Co2 O5 C26 42.1(6) . . . . ? O1 Co3 O6 C26 -34(2) 11 . . . ? O1 Co3 O6 C26 33.5(6) . . . . ? O6 Co3 O6 C26 -141.3(5) 11 . . . ? S2 Co3 O6 C26 114.5(6) . . . . ? Cl1 Co3 O6 C26 -50.3(6) . . . . ? Co2 O1 C1 C2 -11.9(9) . . . . ? Co3 O1 C1 C2 -169.1(5) . . . . ? Co2 O1 C1 C6 164.5(5) . . . . ? Co3 O1 C1 C6 7.3(9) . . . . ? O1 C1 C2 C3 175.1(7) . . . . ? C6 C1 C2 C3 -1.3(11) . . . . ? O1 C1 C2 S1 3.4(10) . . . . ? C6 C1 C2 S1 -173.1(5) . . . . ? C12 S1 C2 C1 -92.2(7) . . . . ? Co2 S1 C2 C1 3.8(6) . . . . ? C12 S1 C2 C3 96.2(7) . . . . ? Co2 S1 C2 C3 -167.8(7) . . . . ? C1 C2 C3 C4 2.3(14) . . . . ? S1 C2 C3 C4 174.0(7) . . . . ? C2 C3 C4 C5 -0.6(15) . . . . ? C2 C3 C4 C13 -177.3(9) . . . . ? C3 C4 C5 C6 -2.2(15) . . . . ? C13 C4 C5 C6 174.7(9) . . . . ? C4 C5 C6 C1 3.1(13) . . . . ? C4 C5 C6 S2 -176.8(7) . . . . ? O1 C1 C6 C5 -177.7(7) . . . . ? C2 C1 C6 C5 -1.3(11) . . . . ? O1 C1 C6 S2 2.2(9) . . . . ? C2 C1 C6 S2 178.6(6) . . . . ? C6 S2 C6 C5 -91.2(8) 11 . . . ? Co3 S2 C6 C5 172.7(7) . . . . ? C6 S2 C6 C1 88.9(6) 11 . . . ? Co3 S2 C6 C1 -7.2(6) . . . . ? Co1 O2 C7 C12 167.0(5) . . . . ? Co2 O2 C7 C12 14.9(8) . . . . ? Co1 O2 C7 C8 -13.0(9) . . . . ? Co2 O2 C7 C8 -165.0(5) . . . . ? O2 C7 C8 C9 177.0(7) . . . . ? C12 C7 C8 C9 -2.9(11) . . . . ? O2 C7 C8 S3 3.5(9) . . . . ? C12 C7 C8 S3 -176.5(5) . . . . ? C8 S3 C8 C9 96.5(7) 11 . . . ? Co1 S3 C8 C9 -169.4(6) . . . . ? C8 S3 C8 C7 -89.7(7) 11 . . . ? Co1 S3 C8 C7 4.4(6) . . . . ? C7 C8 C9 C10 2.0(12) . . . . ? S3 C8 C9 C10 175.4(7) . . . . ? C8 C9 C10 C11 0.5(13) . . . . ? C8 C9 C10 C14 -178.4(8) . . . . ? C9 C10 C11 C12 -1.9(14) . . . . ? C14 C10 C11 C12 177.0(9) . . . . ? C10 C11 C12 C7 0.8(13) . . . . ? C10 C11 C12 S1 -174.6(7) . . . . ? O2 C7 C12 C11 -178.4(7) . . . . ? C8 C7 C12 C11 1.5(11) . . . . ? O2 C7 C12 S1 -2.8(9) . . . . ? C8 C7 C12 S1 177.2(5) . . . . ? C2 S1 C12 C11 -95.2(7) . . . . ? Co2 S1 C12 C11 169.1(6) . . . . ? C2 S1 C12 C7 89.1(6) . . . . ? Co2 S1 C12 C7 -6.6(6) . . . . ? C5 C4 C13 C17 68.7(14) . . . . ? C3 C4 C13 C17 -114.7(12) . . . . ? C5 C4 C13 C15 -47.1(15) . . . . ? C3 C4 C13 C15 129.6(13) . . . . ? C5 C4 C13 C16 -163.4(9) . . . . ? C3 C4 C13 C16 13.2(15) . . . . ? C9 C10 C14 C20 -70.0(14) . . . . ? C11 C10 C14 C20 111.1(13) . . . . ? C9 C10 C14 C18 165.2(9) . . . . ? C11 C10 C14 C18 -13.7(14) . . . . ? C9 C10 C14 C19 47.1(14) . . . . ? C11 C10 C14 C19 -131.8(11) . . . . ? Co1 O4 C21 O3 -4.1(13) . . . . ? Co1 O4 C21 C22 172.4(5) . . . . ? Co2 O3 C21 O4 3.8(12) 11 . . . ? Co2 O3 C21 C22 -172.6(5) 11 . . . ? O4 C21 C22 C25 -10.0(12) . . . . ? O3 C21 C22 C25 167.0(9) . . . . ? O4 C21 C22 C23 170.8(8) . . . . ? O3 C21 C22 C23 -12.2(11) . . . . ? C25 C22 C23 C24 -2.1(15) . . . . ? C21 C22 C23 C24 177.1(9) . . . . ? C22 C23 C24 C23 3.7(19) . . . 12 ? C23 C22 C25 C22 0.6(17) . . . 12 ? C21 C22 C25 C22 -178.6(7) . . . 12 ? Co3 O6 C26 O5 -6.2(11) . . . . ? Co3 O6 C26 C27 171.8(5) . . . . ? Co2 O5 C26 O6 10.4(11) . . . . ? Co2 O5 C26 C27 -167.7(4) . . . . ? O6 C26 C27 C30 -13.7(11) . . . . ? O5 C26 C27 C30 164.6(8) . . . . ? O6 C26 C27 C28 165.4(7) . . . . ? O5 C26 C27 C28 -16.4(11) . . . . ? C30 C27 C28 C29 -1.7(14) . . . . ? C26 C27 C28 C29 179.2(10) . . . . ? C27 C28 C29 C28 -2(2) . . . 10_554 ? C28 C27 C30 C27 5.6(16) . . . 10_554 ? C26 C27 C30 C27 -175.3(6) . . . 10_554 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.800 _refine_diff_density_min -0.960 _refine_diff_density_rms 0.105 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.081 -0.072 -0.013 10847 3538 ' ' _platon_squeeze_details ; ; ###END data_CIAC-202 _database_code_depnum_ccdc_archive 'CCDC 872775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '((CH3)4N)4 ((Co4Cl(C40H44O4S4))4 (C7NH3O4)8' _chemical_melting_point ? _chemical_formula_moiety 'C232 H248 Cl4 Co16 N12 O48 S16' _chemical_formula_sum 'C232 H248 Cl4 Co16 N12 O48 S16' # FOUR (CH3)4N+ cations are included by charge balance. # Unidentified solvents are not included. _chemical_formula_weight 5570.06 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'I 4/m m m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x, -y, -z' 'y, x, -z' '-x, y, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x, y, z' '-y, -x, z' 'x, -y, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 30.1467(13) _cell_length_b 30.1467(13) _cell_length_c 21.2135(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19279.3(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5300 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.23 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5384 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8791 _exptl_absorpt_correction_T_max 0.9219 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83385 _diffrn_reflns_av_R_equivalents 0.1314 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5190 _reflns_number_gt 3894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+2.1111P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5190 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.22899(2) 0.122346(19) 0.5000 0.02184(17) Uani 1 2 d S . . Co2 Co 0.177278(13) 0.177278(13) 0.39209(3) 0.02092(17) Uani 1 2 d S . . S1 S 0.22381(3) 0.22381(3) 0.32018(5) 0.0234(3) Uani 1 2 d S . . S2 S 0.31355(4) 0.12869(4) 0.5000 0.0259(3) Uani 1 2 d S . . Cl1 Cl 0.14558(3) 0.14558(3) 0.5000 0.0230(3) Uani 1 4 d S . . O1 O 0.23560(6) 0.16859(7) 0.43381(9) 0.0228(5) Uani 1 1 d . . . O2 O 0.18197(7) 0.11530(7) 0.35534(10) 0.0254(5) Uani 1 1 d . . . O3 O 0.21609(7) 0.07623(7) 0.43236(9) 0.0255(5) Uani 1 1 d . . . N1 N 0.19635(12) 0.0000 0.37336(16) 0.0228(8) Uani 1 2 d S . . C1 C 0.27360(10) 0.18042(9) 0.40891(14) 0.0213(7) Uani 1 1 d . . . C2 C 0.27541(10) 0.20797(11) 0.35581(15) 0.0257(7) Uani 1 1 d . . . C3 C 0.31566(11) 0.21844(12) 0.32692(19) 0.0409(9) Uani 1 1 d . . . H3 H 0.3159 0.2372 0.2909 0.049 Uiso 1 1 calc R . . C4 C 0.35522(12) 0.20196(15) 0.3499(2) 0.0532(12) Uani 1 1 d . . . C5 C 0.35403(11) 0.17559(13) 0.40470(17) 0.0413(9) Uani 1 1 d . . . H5 H 0.3810 0.1645 0.4218 0.050 Uiso 1 1 calc R . . C6 C 0.31444(10) 0.16549(10) 0.43412(15) 0.0267(7) Uani 1 1 d . . . C7 C 0.40029(14) 0.2117(2) 0.3172(2) 0.0767(17) Uani 1 1 d . . . C8 C 0.39383(15) 0.23066(19) 0.2523(3) 0.094(2) Uani 1 1 d . . . H8A H 0.3865 0.2622 0.2556 0.140 Uiso 1 1 calc R . . H8B H 0.3696 0.2150 0.2311 0.140 Uiso 1 1 calc R . . H8C H 0.4212 0.2272 0.2279 0.140 Uiso 1 1 calc R . . C9 C 0.4281(2) 0.2381(3) 0.3586(4) 0.126(3) Uani 1 1 d . . . H9A H 0.4568 0.2434 0.3382 0.189 Uiso 1 1 calc R . . H9B H 0.4327 0.2222 0.3983 0.189 Uiso 1 1 calc R . . H9C H 0.4136 0.2665 0.3671 0.189 Uiso 1 1 calc R . . C10 C 0.42520(19) 0.1652(3) 0.3061(3) 0.137(3) Uani 1 1 d . . . H10A H 0.4504 0.1697 0.2776 0.205 Uiso 1 1 calc R . . H10B H 0.4045 0.1439 0.2873 0.205 Uiso 1 1 calc R . . H10C H 0.4359 0.1538 0.3465 0.205 Uiso 1 1 calc R . . C11 C 0.19574(10) 0.08017(10) 0.38012(14) 0.0246(7) Uani 1 1 d . . . C12 C 0.18666(10) 0.03797(10) 0.34432(15) 0.0258(7) Uani 1 1 d . . . C13 C 0.16766(14) 0.03982(12) 0.28480(18) 0.0443(10) Uani 1 1 d . . . H13 H 0.1616 0.0675 0.2651 0.053 Uiso 1 1 calc R . . C14 C 0.1577(2) 0.0000 0.2549(3) 0.0529(17) Uani 1 2 d S . . H14 H 0.1442 0.0000 0.2144 0.063 Uiso 1 2 calc SR . . 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 0.0286(3) 0.0209(3) 0.0160(3) 0.000 0.000 0.0013(3) Co2 0.0221(2) 0.0221(2) 0.0186(3) 0.00090(17) 0.00090(17) 0.0015(3) S1 0.0254(4) 0.0254(4) 0.0193(6) 0.0029(3) 0.0029(3) 0.0046(5) S2 0.0278(6) 0.0287(6) 0.0212(6) 0.000 0.000 0.0077(5) Cl1 0.0262(5) 0.0262(5) 0.0166(7) 0.000 0.000 -0.0010(7) O1 0.0240(11) 0.0232(11) 0.0212(11) 0.0051(9) 0.0009(9) 0.0026(9) O2 0.0341(13) 0.0226(11) 0.0194(11) 0.0025(9) 0.0014(9) 0.0032(10) O3 0.0381(13) 0.0229(11) 0.0156(11) 0.0020(9) -0.0027(10) 0.0022(10) N1 0.027(2) 0.025(2) 0.0161(19) 0.000 0.0018(16) 0.000 C1 0.0235(16) 0.0181(15) 0.0223(16) -0.0021(13) -0.0005(13) -0.0002(13) C2 0.0248(17) 0.0294(17) 0.0230(17) 0.0034(14) -0.0018(13) 0.0029(14) C3 0.0255(19) 0.053(2) 0.044(2) 0.0221(19) 0.0010(16) -0.0001(17) C4 0.025(2) 0.077(3) 0.057(3) 0.027(2) 0.0076(19) 0.001(2) C5 0.0195(17) 0.064(3) 0.041(2) 0.019(2) 0.0006(15) 0.0055(17) C6 0.0283(18) 0.0298(18) 0.0221(17) 0.0033(14) -0.0012(13) 0.0003(14) C7 0.029(2) 0.122(5) 0.079(4) 0.049(3) 0.006(2) -0.002(3) C8 0.039(3) 0.140(5) 0.101(4) 0.062(4) 0.034(3) 0.004(3) C9 0.067(4) 0.179(7) 0.134(6) 0.012(5) 0.017(4) -0.056(4) C10 0.074(4) 0.202(8) 0.134(6) 0.082(6) 0.060(4) 0.066(5) C11 0.0255(17) 0.0272(17) 0.0213(17) 0.0038(14) 0.0057(13) -0.0032(14) C12 0.0310(18) 0.0253(17) 0.0211(17) 0.0004(14) -0.0008(14) -0.0011(14) C13 0.070(3) 0.028(2) 0.035(2) 0.0042(16) -0.018(2) 0.0052(19) C14 0.093(5) 0.032(3) 0.034(3) 0.000 -0.033(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.989(2) 19_556 ? Co1 O1 1.989(2) . ? Co1 O3 2.035(2) 19_556 ? Co1 O3 2.035(2) . ? Co1 S2 2.5565(13) . ? Co1 Cl1 2.6103(9) . ? Co2 O1 1.986(2) 24 ? Co2 O1 1.986(2) . ? Co2 O2 2.029(2) . ? Co2 O2 2.029(2) 24 ? Co2 S1 2.5025(12) . ? Co2 Cl1 2.6584(10) . ? S1 C2 1.794(3) 24 ? S1 C2 1.794(3) . ? S2 C6 1.784(3) 19_556 ? S2 C6 1.785(3) . ? Cl1 Co1 2.6103(9) 6_556 ? Cl1 Co2 2.6584(10) 19_556 ? O1 C1 1.311(3) . ? O2 C11 1.253(4) . ? O3 C11 1.272(4) . ? N1 C12 1.332(3) 23 ? N1 C12 1.332(3) . ? C1 C2 1.401(4) . ? C1 C6 1.416(4) . ? C2 C3 1.396(4) . ? C3 C4 1.381(5) . ? C3 H3 0.9500 . ? C4 C5 1.409(5) . ? C4 C7 1.553(5) . ? C5 C6 1.381(4) . ? C5 H5 0.9500 . ? C7 C9 1.451(8) . ? C7 C8 1.504(6) . ? C7 C10 1.606(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.507(4) . ? C12 C13 1.387(5) . ? C13 C14 1.391(4) . ? C13 H13 0.9500 . ? C14 C13 1.391(4) 23 ? C14 H14 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 O1 Co1 O1 89.83(12) 19_556 . ? O1 Co1 O3 90.02(8) 19_556 19_556 ? O1 Co1 O3 174.70(9) . 19_556 ? O1 Co1 O3 174.70(9) 19_556 . ? O1 Co1 O3 90.02(8) . . ? O3 Co1 O3 89.64(11) 19_556 . ? O1 Co1 S2 81.23(6) 19_556 . ? O1 Co1 S2 81.23(6) . . ? O3 Co1 S2 103.98(7) 19_556 . ? O3 Co1 S2 103.98(7) . . ? O1 Co1 Cl1 84.75(6) 19_556 . ? O1 Co1 Cl1 84.75(6) . . ? O3 Co1 Cl1 89.96(7) 19_556 . ? O3 Co1 Cl1 89.96(7) . . ? S2 Co1 Cl1 160.15(5) . . ? O1 Co2 O1 92.01(12) 24 . ? O1 Co2 O2 174.59(9) 24 . ? O1 Co2 O2 89.31(8) . . ? O1 Co2 O2 89.31(8) 24 24 ? O1 Co2 O2 174.59(9) . 24 ? O2 Co2 O2 88.90(12) . 24 ? O1 Co2 S1 81.33(6) 24 . ? O1 Co2 S1 81.33(6) . . ? O2 Co2 S1 104.05(6) . . ? O2 Co2 S1 104.05(6) 24 . ? O1 Co2 Cl1 83.52(6) 24 . ? O1 Co2 Cl1 83.52(6) . . ? O2 Co2 Cl1 91.42(6) . . ? O2 Co2 Cl1 91.43(6) 24 . ? S1 Co2 Cl1 158.12(5) . . ? C2 S1 C2 106.5(2) 24 . ? C2 S1 Co2 94.60(11) 24 . ? C2 S1 Co2 94.59(11) . . ? C6 S2 C6 103.1(2) 19_556 . ? C6 S2 Co1 93.52(11) 19_556 . ? C6 S2 Co1 93.52(11) . . ? Co1 Cl1 Co1 121.13(6) . 6_556 ? Co1 Cl1 Co2 75.53(3) . 19_556 ? Co1 Cl1 Co2 75.53(3) 6_556 19_556 ? Co1 Cl1 Co2 75.53(3) . . ? Co1 Cl1 Co2 75.53(3) 6_556 . ? Co2 Cl1 Co2 118.89(6) 19_556 . ? C1 O1 Co2 123.93(18) . . ? C1 O1 Co1 124.26(18) . . ? Co2 O1 Co1 108.56(10) . . ? C11 O2 Co2 129.8(2) . . ? C11 O3 Co1 130.0(2) . . ? C12 N1 C12 118.4(4) 23 . ? O1 C1 C2 121.3(3) . . ? O1 C1 C6 121.4(3) . . ? C2 C1 C6 117.3(3) . . ? C3 C2 C1 121.4(3) . . ? C3 C2 S1 120.6(2) . . ? C1 C2 S1 117.6(2) . . ? C4 C3 C2 121.0(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 118.2(3) . . ? C3 C4 C7 122.0(4) . . ? C5 C4 C7 119.8(3) . . ? C6 C5 C4 121.3(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 120.7(3) . . ? C5 C6 S2 120.3(2) . . ? C1 C6 S2 118.7(2) . . ? C9 C7 C8 114.8(5) . . ? C9 C7 C4 109.8(5) . . ? C8 C7 C4 111.5(4) . . ? C9 C7 C10 107.3(5) . . ? C8 C7 C10 104.9(5) . . ? C4 C7 C10 108.1(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C11 O3 127.2(3) . . ? O2 C11 C12 116.2(3) . . ? O3 C11 C12 116.6(3) . . ? N1 C12 C13 123.1(3) . . ? N1 C12 C11 116.9(3) . . ? C13 C12 C11 120.0(3) . . ? C12 C13 C14 118.0(3) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? C13 C14 C13 119.3(5) . 23 ? C13 C14 H14 120.3 . . ? C13 C14 H14 120.3 23 . ? 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 O1 Co2 S1 C2 -6.80(12) 24 . . 24 ? O1 Co2 S1 C2 -100.19(13) . . . 24 ? O2 Co2 S1 C2 172.72(12) . . . 24 ? O2 Co2 S1 C2 80.29(13) 24 . . 24 ? Cl1 Co2 S1 C2 -53.49(11) . . . 24 ? O1 Co2 S1 C2 100.19(13) 24 . . . ? O1 Co2 S1 C2 6.80(12) . . . . ? O2 Co2 S1 C2 -80.29(13) . . . . ? O2 Co2 S1 C2 -172.72(12) 24 . . . ? Cl1 Co2 S1 C2 53.50(11) . . . . ? O1 Co1 S2 C6 6.08(12) 19_556 . . 19_556 ? O1 Co1 S2 C6 97.27(12) . . . 19_556 ? O3 Co1 S2 C6 -81.74(12) 19_556 . . 19_556 ? O3 Co1 S2 C6 -174.91(12) . . . 19_556 ? Cl1 Co1 S2 C6 51.68(11) . . . 19_556 ? O1 Co1 S2 C6 -97.28(12) 19_556 . . . ? O1 Co1 S2 C6 -6.08(12) . . . . ? O3 Co1 S2 C6 174.90(12) 19_556 . . . ? O3 Co1 S2 C6 81.73(12) . . . . ? Cl1 Co1 S2 C6 -51.68(11) . . . . ? O1 Co1 Cl1 Co1 45.16(6) 19_556 . . 6_556 ? O1 Co1 Cl1 Co1 -45.16(6) . . . 6_556 ? O3 Co1 Cl1 Co1 135.18(6) 19_556 . . 6_556 ? O3 Co1 Cl1 Co1 -135.18(6) . . . 6_556 ? S2 Co1 Cl1 Co1 0.0 . . . 6_556 ? O1 Co1 Cl1 Co2 -17.63(6) 19_556 . . 19_556 ? O1 Co1 Cl1 Co2 -107.95(6) . . . 19_556 ? O3 Co1 Cl1 Co2 72.39(6) 19_556 . . 19_556 ? O3 Co1 Cl1 Co2 162.03(6) . . . 19_556 ? S2 Co1 Cl1 Co2 -62.79(2) . . . 19_556 ? O1 Co1 Cl1 Co2 107.95(6) 19_556 . . . ? O1 Co1 Cl1 Co2 17.63(6) . . . . ? O3 Co1 Cl1 Co2 -162.03(6) 19_556 . . . ? O3 Co1 Cl1 Co2 -72.39(6) . . . . ? S2 Co1 Cl1 Co2 62.79(2) . . . . ? O1 Co2 Cl1 Co1 -110.47(6) 24 . . . ? O1 Co2 Cl1 Co1 -17.70(6) . . . . ? O2 Co2 Cl1 Co1 71.45(6) . . . . ? O2 Co2 Cl1 Co1 160.38(6) 24 . . . ? S1 Co2 Cl1 Co1 -64.08(2) . . . . ? O1 Co2 Cl1 Co1 17.70(6) 24 . . 6_556 ? O1 Co2 Cl1 Co1 110.47(6) . . . 6_556 ? O2 Co2 Cl1 Co1 -160.39(6) . . . 6_556 ? O2 Co2 Cl1 Co1 -71.45(6) 24 . . 6_556 ? S1 Co2 Cl1 Co1 64.08(2) . . . 6_556 ? O1 Co2 Cl1 Co2 -46.39(6) 24 . . 19_556 ? O1 Co2 Cl1 Co2 46.38(6) . . . 19_556 ? O2 Co2 Cl1 Co2 135.53(6) . . . 19_556 ? O2 Co2 Cl1 Co2 -135.53(6) 24 . . 19_556 ? S1 Co2 Cl1 Co2 0.0 . . . 19_556 ? O1 Co2 O1 C1 -92.4(2) 24 . . . ? O2 Co2 O1 C1 92.9(2) . . . . ? O2 Co2 O1 C1 163.6(8) 24 . . . ? S1 Co2 O1 C1 -11.5(2) . . . . ? Cl1 Co2 O1 C1 -175.6(2) . . . . ? O1 Co2 O1 Co1 107.29(9) 24 . . . ? O2 Co2 O1 Co1 -67.46(10) . . . . ? O2 Co2 O1 Co1 3.2(10) 24 . . . ? S1 Co2 O1 Co1 -171.79(9) . . . . ? Cl1 Co2 O1 Co1 24.05(8) . . . . ? O1 Co1 O1 C1 90.5(2) 19_556 . . . ? O3 Co1 O1 C1 179(100) 19_556 . . . ? O3 Co1 O1 C1 -94.8(2) . . . . ? S2 Co1 O1 C1 9.4(2) . . . . ? Cl1 Co1 O1 C1 175.3(2) . . . . ? O1 Co1 O1 Co2 -109.21(9) 19_556 . . . ? O3 Co1 O1 Co2 -20.8(10) 19_556 . . . ? O3 Co1 O1 Co2 65.49(10) . . . . ? S2 Co1 O1 Co2 169.63(9) . . . . ? Cl1 Co1 O1 Co2 -24.47(8) . . . . ? O1 Co2 O2 C11 -63.6(10) 24 . . . ? O1 Co2 O2 C11 40.5(3) . . . . ? O2 Co2 O2 C11 -134.4(2) 24 . . . ? S1 Co2 O2 C11 121.4(2) . . . . ? Cl1 Co2 O2 C11 -43.0(3) . . . . ? O1 Co1 O3 C11 53.9(10) 19_556 . . . ? O1 Co1 O3 C11 -34.4(3) . . . . ? O3 Co1 O3 C11 140.3(2) 19_556 . . . ? S2 Co1 O3 C11 -115.4(3) . . . . ? Cl1 Co1 O3 C11 50.3(3) . . . . ? Co2 O1 C1 C2 12.5(4) . . . . ? Co1 O1 C1 C2 169.8(2) . . . . ? Co2 O1 C1 C6 -166.8(2) . . . . ? Co1 O1 C1 C6 -9.5(4) . . . . ? O1 C1 C2 C3 -176.1(3) . . . . ? C6 C1 C2 C3 3.3(5) . . . . ? O1 C1 C2 S1 -3.7(4) . . . . ? C6 C1 C2 S1 175.6(2) . . . . ? C2 S1 C2 C3 -95.3(3) 24 . . . ? Co2 S1 C2 C3 168.5(3) . . . . ? C2 S1 C2 C1 92.3(3) 24 . . . ? Co2 S1 C2 C1 -3.9(3) . . . . ? C1 C2 C3 C4 -0.1(6) . . . . ? S1 C2 C3 C4 -172.3(3) . . . . ? C2 C3 C4 C5 -2.3(7) . . . . ? C2 C3 C4 C7 177.7(4) . . . . ? C3 C4 C5 C6 1.5(7) . . . . ? C7 C4 C5 C6 -178.5(4) . . . . ? C4 C5 C6 C1 1.8(6) . . . . ? C4 C5 C6 S2 175.3(3) . . . . ? O1 C1 C6 C5 175.3(3) . . . . ? C2 C1 C6 C5 -4.0(5) . . . . ? O1 C1 C6 S2 1.6(4) . . . . ? C2 C1 C6 S2 -177.7(2) . . . . ? C6 S2 C6 C5 96.1(3) 19_556 . . . ? Co1 S2 C6 C5 -169.4(3) . . . . ? C6 S2 C6 C1 -90.2(3) 19_556 . . . ? Co1 S2 C6 C1 4.3(3) . . . . ? C3 C4 C7 C9 114.9(6) . . . . ? C5 C4 C7 C9 -65.1(7) . . . . ? C3 C4 C7 C8 -13.6(7) . . . . ? C5 C4 C7 C8 166.4(5) . . . . ? C3 C4 C7 C10 -128.4(5) . . . . ? C5 C4 C7 C10 51.6(6) . . . . ? Co2 O2 C11 O3 -10.7(5) . . . . ? Co2 O2 C11 C12 168.51(19) . . . . ? Co1 O3 C11 O2 6.9(5) . . . . ? Co1 O3 C11 C12 -172.31(19) . . . . ? C12 N1 C12 C13 -1.2(6) 23 . . . ? C12 N1 C12 C11 176.7(2) 23 . . . ? O2 C11 C12 N1 -172.3(3) . . . . ? O3 C11 C12 N1 7.0(4) . . . . ? O2 C11 C12 C13 5.6(5) . . . . ? O3 C11 C12 C13 -175.1(3) . . . . ? N1 C12 C13 C14 1.1(6) . . . . ? C11 C12 C13 C14 -176.6(4) . . . . ? C12 C13 C14 C13 -1.1(9) . . . 23 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.718 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.073 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.098 -0.047 -0.055 10313 3526 ' ' _platon_squeeze_details ; ; ###END data_CIAC-203 _database_code_depnum_ccdc_archive 'CCDC 872776' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;(((Co4Cl2(H2O)2(C40H44O4S4))((Co4Cl2(H2O)2 (C40H45O4S4))Cl) (C8H4O4)2 ; _chemical_melting_point ? _chemical_formula_moiety 'C96 H105 Cl5 Co8 O20 S8' _chemical_formula_sum 'C96 H105 Cl5 Co8 O20 S8' #excluding the disorder solvent molecules. _chemical_formula_weight 2483.97 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' Cl Cl 0.1484 0.1585 '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 11.6208(8) _cell_length_b 17.0306(11) _cell_length_c 19.8020(13) _cell_angle_alpha 97.9850(10) _cell_angle_beta 99.9590(10) _cell_angle_gamma 101.2320(10) _cell_volume 3725.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5453 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.05 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1270 _exptl_absorpt_coefficient_mu 1.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8686 _exptl_absorpt_correction_T_max 0.8966 _exptl_absorpt_process_details sadabs _exptl_special_details ; ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20661 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.1098 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.17 _reflns_number_total 13204 _reflns_number_gt 7559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13204 _refine_ls_number_parameters 620 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1224 _refine_ls_wR_factor_gt 0.1124 _refine_ls_goodness_of_fit_ref 0.879 _refine_ls_restrained_S_all 0.879 _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 0.88221(5) 0.93931(4) 0.38107(3) 0.01947(16) Uani 1 1 d . . . Co2 Co 0.64462(5) 0.80856(4) 0.29005(3) 0.02014(16) Uani 1 1 d . . . Co3 Co 0.78076(5) 0.64934(4) 0.28908(3) 0.02373(17) Uani 1 1 d . . . Co4 Co 1.01829(5) 0.78197(4) 0.38111(3) 0.02172(16) Uani 1 1 d . . . S1 S 0.96984(10) 1.05154(7) 0.32554(6) 0.0211(3) Uani 1 1 d . . . S2 S 0.56529(10) 0.83639(7) 0.17104(6) 0.0203(3) Uani 1 1 d . . . S3 S 0.79986(10) 0.58353(7) 0.17160(6) 0.0224(3) Uani 1 1 d . . . S4 S 1.20020(10) 0.79863(7) 0.32936(6) 0.0237(3) Uani 1 1 d . . . Cl1 Cl 0.79760(10) 0.78133(7) 0.39347(6) 0.0262(3) Uani 1 1 d . . . Cl2 Cl 1.0000 1.0000 0.5000 0.0387(5) Uani 1 2 d S . . Cl3 Cl 0.59321(15) 0.56293(11) 0.29213(9) 0.0690(5) Uani 1 1 d . . . O1 O 0.7834(2) 0.89580(17) 0.28407(14) 0.0185(7) Uani 1 1 d . . . O2 O 0.6952(2) 0.71918(17) 0.23359(14) 0.0192(7) Uani 1 1 d . . . O3 O 0.9409(3) 0.71812(18) 0.28599(14) 0.0223(7) Uani 1 1 d . . . O4 O 1.0177(2) 0.89305(17) 0.35942(14) 0.0202(7) Uani 1 1 d . . . O5 O 0.7471(3) 0.9795(2) 0.41372(16) 0.0310(8) Uani 1 1 d . . . O6 O 0.5829(2) 0.88683(19) 0.35360(15) 0.0268(8) Uani 1 1 d . . . O7 O 0.8616(3) 0.58763(19) 0.35655(17) 0.0365(9) Uani 1 1 d . . . O8 O 1.0261(3) 0.67934(19) 0.41868(16) 0.0324(9) Uani 1 1 d . . . O9 O 0.4968(3) 0.7174(2) 0.30278(16) 0.0326(8) Uani 1 1 d . . . O10 O 1.0930(3) 0.8384(2) 0.48576(16) 0.0374(9) Uani 1 1 d . . . C1 C 0.7749(4) 0.9458(3) 0.2380(2) 0.0187(10) Uani 1 1 d . . . C2 C 0.8572(4) 1.0201(3) 0.2474(2) 0.0217(11) Uani 1 1 d . . . C3 C 0.8453(4) 1.0711(3) 0.1996(2) 0.0221(11) Uani 1 1 d . . . H3A H 0.9019 1.1216 0.2076 0.027 Uiso 1 1 calc R . . C4 C 0.7547(4) 1.0522(3) 0.1402(2) 0.0226(11) Uani 1 1 d . . . C5 C 0.6720(4) 0.9784(3) 0.1312(2) 0.0231(11) Uani 1 1 d . . . H5A H 0.6082 0.9634 0.0915 0.028 Uiso 1 1 calc R . . C6 C 0.6807(4) 0.9262(3) 0.1791(2) 0.0209(11) Uani 1 1 d . . . C7 C 0.6784(4) 0.7082(3) 0.1648(2) 0.0178(10) Uani 1 1 d . . . C8 C 0.6179(4) 0.7563(2) 0.1264(2) 0.0179(10) Uani 1 1 d . . . C9 C 0.5893(4) 0.7394(3) 0.0529(2) 0.0205(10) Uani 1 1 d . . . H9A H 0.5469 0.7727 0.0284 0.025 Uiso 1 1 calc R . . C10 C 0.6221(4) 0.6749(3) 0.0157(2) 0.0243(11) Uani 1 1 d . . . C11 C 0.6884(4) 0.6290(3) 0.0539(2) 0.0214(11) Uani 1 1 d . . . H11A H 0.7147 0.5858 0.0299 0.026 Uiso 1 1 calc R . . C12 C 0.7164(4) 0.6461(3) 0.1271(2) 0.0217(11) Uani 1 1 d . . . C13 C 1.0039(4) 0.6953(3) 0.2406(2) 0.0227(11) Uani 1 1 d . . . C14 C 0.9536(4) 0.6357(3) 0.1810(2) 0.0209(11) Uani 1 1 d . . . C15 C 1.0219(4) 0.6141(3) 0.1328(2) 0.0237(11) Uani 1 1 d . . . H15A H 0.9845 0.5734 0.0930 0.028 Uiso 1 1 calc R . . C16 C 1.1427(4) 0.6502(3) 0.1412(2) 0.0240(11) Uani 1 1 d . . . C17 C 1.1937(4) 0.7076(3) 0.2022(2) 0.0218(11) Uani 1 1 d . . . H17A H 1.2765 0.7327 0.2104 0.026 Uiso 1 1 calc R . . C18 C 1.1286(4) 0.7290(3) 0.2505(2) 0.0212(11) Uani 1 1 d . . . C19 C 1.0946(4) 0.9306(3) 0.3244(2) 0.0209(11) Uani 1 1 d . . . C20 C 1.1880(4) 0.8942(3) 0.3064(2) 0.0199(10) Uani 1 1 d . . . C21 C 1.2711(4) 0.9355(3) 0.2740(2) 0.0296(12) Uani 1 1 d . . . H21A H 1.3334 0.9106 0.2628 0.036 Uiso 1 1 calc R . . C22 C 1.2678(4) 1.0123(3) 0.2568(2) 0.0297(12) Uani 1 1 d . . . C23 C 1.1722(4) 1.0449(3) 0.2725(2) 0.0277(12) Uani 1 1 d . . . H23A H 1.1649 1.0960 0.2605 0.033 Uiso 1 1 calc R . . C24 C 1.0876(4) 1.0052(3) 0.3052(2) 0.0176(10) Uani 1 1 d . . . C25 C 0.7485(4) 1.1126(3) 0.0899(2) 0.0324(13) Uani 1 1 d . . . C26 C 0.5839(5) 0.6504(3) -0.0642(2) 0.0317(13) Uani 1 1 d . . . C27 C 1.2194(4) 0.6311(3) 0.0884(3) 0.0334(13) Uani 1 1 d . . . C28 C 1.3635(5) 1.0547(4) 0.2224(3) 0.0482(16) Uani 1 1 d . . . C29 C 0.8583(5) 1.1202(4) 0.0574(3) 0.0632(19) Uani 1 1 d . . . H29A H 0.9308 1.1382 0.0942 0.095 Uiso 1 1 calc R . . H29B H 0.8564 1.1599 0.0262 0.095 Uiso 1 1 calc R . . H29C H 0.8586 1.0672 0.0309 0.095 Uiso 1 1 calc R . . C30 C 0.7446(6) 1.1943(3) 0.1292(3) 0.0567(18) Uani 1 1 d . . . H30A H 0.6729 1.1888 0.1495 0.085 Uiso 1 1 calc R . . H30B H 0.7421 1.2332 0.0971 0.085 Uiso 1 1 calc R . . H30C H 0.8163 1.2140 0.1664 0.085 Uiso 1 1 calc R . . C31 C 0.6356(5) 1.0852(4) 0.0314(3) 0.061(2) Uani 1 1 d . . . H31A H 0.5641 1.0808 0.0518 0.092 Uiso 1 1 calc R . . H31B H 0.6356 1.0322 0.0048 0.092 Uiso 1 1 calc R . . H31C H 0.6353 1.1253 0.0004 0.092 Uiso 1 1 calc R . . C32 C 0.5295(6) 0.7133(4) -0.0966(3) 0.0589(19) Uani 1 1 d . . . H32A H 0.5878 0.7656 -0.0850 0.088 Uiso 1 1 calc R . . H32B H 0.4576 0.7191 -0.0785 0.088 Uiso 1 1 calc R . . H32C H 0.5076 0.6960 -0.1473 0.088 Uiso 1 1 calc R . . C33 C 0.6943(6) 0.6422(4) -0.0956(3) 0.068(2) Uani 1 1 d . . . H33A H 0.7514 0.6950 -0.0855 0.102 Uiso 1 1 calc R . . H33B H 0.6692 0.6242 -0.1462 0.102 Uiso 1 1 calc R . . H33C H 0.7326 0.6022 -0.0751 0.102 Uiso 1 1 calc R . . C34 C 0.4946(6) 0.5671(4) -0.0814(3) 0.0628(19) Uani 1 1 d . . . H34A H 0.4241 0.5715 -0.0615 0.094 Uiso 1 1 calc R . . H34B H 0.5331 0.5268 -0.0616 0.094 Uiso 1 1 calc R . . H34C H 0.4700 0.5502 -0.1321 0.094 Uiso 1 1 calc R . . C35 C 1.1550(5) 0.5622(3) 0.0286(3) 0.0472(16) Uani 1 1 d . . . H35A H 1.2085 0.5537 -0.0036 0.071 Uiso 1 1 calc R . . H35B H 1.0832 0.5761 0.0037 0.071 Uiso 1 1 calc R . . H35C H 1.1316 0.5122 0.0469 0.071 Uiso 1 1 calc R . . C36 C 1.3347(4) 0.6090(3) 0.1249(3) 0.0427(14) Uani 1 1 d . . . H36A H 1.3839 0.5980 0.0907 0.064 Uiso 1 1 calc R . . H36B H 1.3129 0.5605 0.1455 0.064 Uiso 1 1 calc R . . H36C H 1.3803 0.6545 0.1616 0.064 Uiso 1 1 calc R . . C37 C 1.2578(5) 0.7090(3) 0.0576(3) 0.0434(14) Uani 1 1 d . . . H37A H 1.3077 0.6982 0.0238 0.065 Uiso 1 1 calc R . . H37B H 1.3037 0.7534 0.0953 0.065 Uiso 1 1 calc R . . H37C H 1.1863 0.7246 0.0344 0.065 Uiso 1 1 calc R . . C38 C 1.3596(7) 1.0067(5) 0.1514(4) 0.109(3) Uani 1 1 d . . . H38A H 1.2809 1.0012 0.1214 0.163 Uiso 1 1 calc R . . H38B H 1.3731 0.9526 0.1564 0.163 Uiso 1 1 calc R . . H38C H 1.4221 1.0353 0.1305 0.163 Uiso 1 1 calc R . . C39 C 1.3578(7) 1.1385(5) 0.2185(5) 0.125(4) Uani 1 1 d . . . H39A H 1.3647 1.1687 0.2654 0.187 Uiso 1 1 calc R . . H39B H 1.2810 1.1395 0.1893 0.187 Uiso 1 1 calc R . . H39C H 1.4237 1.1636 0.1981 0.187 Uiso 1 1 calc R . . C40 C 1.4899(5) 1.0577(5) 0.2642(4) 0.088(3) Uani 1 1 d . . . H40A H 1.5013 1.0901 0.3108 0.131 Uiso 1 1 calc R . . H40B H 1.5504 1.0826 0.2400 0.131 Uiso 1 1 calc R . . H40C H 1.4982 1.0023 0.2684 0.131 Uiso 1 1 calc R . . C41 C 0.5675(4) 0.9747(3) 0.4525(2) 0.0265(12) Uani 1 1 d . . . C42 C 0.4477(5) 0.9387(3) 0.4445(3) 0.0456(16) Uani 1 1 d . . . H42A H 0.4106 0.8961 0.4061 0.055 Uiso 1 1 calc R . . C43 C 0.6195(5) 1.0368(4) 0.5087(3) 0.0514(18) Uani 1 1 d . . . H43A H 0.7018 1.0628 0.5152 0.062 Uiso 1 1 calc R . . C44 C 0.6376(4) 0.9440(3) 0.4028(2) 0.0264(12) Uani 1 1 d . . . C45 C 0.9763(4) 0.5523(3) 0.4545(2) 0.0290(12) Uani 1 1 d . . . C46 C 0.8955(5) 0.4816(3) 0.4516(3) 0.0467(17) Uani 1 1 d . . . H46A H 0.8227 0.4683 0.4178 0.056 Uiso 1 1 calc R . . C47 C 0.9172(5) 0.4293(3) 0.4965(3) 0.0512(18) Uani 1 1 d . . . H47A H 0.8595 0.3805 0.4939 0.061 Uiso 1 1 calc R . . C48 C 0.9542(4) 0.6109(3) 0.4063(2) 0.0299(12) 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 0.0177(3) 0.0234(4) 0.0168(3) 0.0023(3) 0.0039(3) 0.0041(3) Co2 0.0181(3) 0.0219(4) 0.0191(3) 0.0017(3) 0.0032(3) 0.0033(3) Co3 0.0221(4) 0.0263(4) 0.0237(4) 0.0111(3) 0.0018(3) 0.0055(3) Co4 0.0244(4) 0.0199(4) 0.0199(3) 0.0057(3) 0.0005(3) 0.0046(3) S1 0.0208(6) 0.0175(6) 0.0230(6) 0.0023(5) 0.0011(5) 0.0035(5) S2 0.0182(6) 0.0197(6) 0.0218(6) 0.0010(5) 0.0012(5) 0.0060(5) S3 0.0194(6) 0.0180(6) 0.0283(7) 0.0054(5) -0.0013(5) 0.0057(5) S4 0.0196(6) 0.0240(7) 0.0249(6) 0.0018(5) -0.0014(5) 0.0058(5) Cl1 0.0246(6) 0.0334(7) 0.0205(6) 0.0093(5) 0.0038(5) 0.0040(5) Cl2 0.0424(11) 0.0447(12) 0.0227(9) -0.0100(8) -0.0082(8) 0.0196(9) Cl3 0.0607(11) 0.0662(12) 0.0887(13) 0.0358(10) 0.0202(10) 0.0145(9) O1 0.0199(17) 0.0201(17) 0.0171(16) 0.0080(13) 0.0031(13) 0.0055(13) O2 0.0183(17) 0.0249(18) 0.0145(16) 0.0035(13) 0.0003(13) 0.0074(13) O3 0.0199(17) 0.0250(19) 0.0204(17) -0.0016(14) 0.0038(14) 0.0054(14) O4 0.0180(17) 0.0232(18) 0.0210(16) 0.0080(14) 0.0064(13) 0.0036(13) O5 0.0174(18) 0.040(2) 0.0322(19) -0.0045(16) 0.0069(15) 0.0033(15) O6 0.0176(17) 0.035(2) 0.0224(17) -0.0078(15) 0.0032(14) 0.0029(14) O7 0.035(2) 0.029(2) 0.037(2) 0.0184(17) -0.0121(17) -0.0033(16) O8 0.036(2) 0.023(2) 0.035(2) 0.0110(16) -0.0055(16) 0.0049(15) O9 0.0236(19) 0.035(2) 0.036(2) 0.0042(16) 0.0064(15) 0.0024(15) O10 0.043(2) 0.037(2) 0.0279(19) 0.0009(16) -0.0039(16) 0.0125(17) C1 0.021(3) 0.019(3) 0.021(2) 0.005(2) 0.007(2) 0.013(2) C2 0.019(3) 0.023(3) 0.022(2) 0.003(2) 0.002(2) 0.007(2) C3 0.020(3) 0.016(3) 0.031(3) 0.005(2) 0.004(2) 0.0045(19) C4 0.027(3) 0.021(3) 0.025(3) 0.009(2) 0.007(2) 0.013(2) C5 0.027(3) 0.022(3) 0.023(3) 0.008(2) 0.003(2) 0.011(2) C6 0.018(2) 0.021(3) 0.017(2) -0.004(2) -0.0026(19) -0.0002(19) C7 0.012(2) 0.024(3) 0.016(2) 0.0055(19) 0.0027(18) -0.0028(18) C8 0.021(2) 0.012(2) 0.020(2) 0.0044(19) 0.0027(19) 0.0028(18) C9 0.027(3) 0.017(3) 0.019(2) 0.007(2) 0.003(2) 0.007(2) C10 0.025(3) 0.026(3) 0.018(2) 0.004(2) 0.000(2) 0.002(2) C11 0.023(3) 0.017(3) 0.024(3) 0.003(2) 0.003(2) 0.005(2) C12 0.019(3) 0.017(3) 0.027(3) 0.006(2) 0.000(2) 0.0048(19) C13 0.028(3) 0.021(3) 0.023(3) 0.007(2) 0.007(2) 0.013(2) C14 0.017(2) 0.021(3) 0.025(3) 0.006(2) 0.002(2) 0.006(2) C15 0.023(3) 0.020(3) 0.024(3) -0.002(2) -0.004(2) 0.007(2) C16 0.025(3) 0.018(3) 0.030(3) 0.004(2) 0.006(2) 0.004(2) C17 0.014(2) 0.023(3) 0.031(3) 0.005(2) 0.008(2) 0.0059(19) C18 0.018(2) 0.015(2) 0.027(3) -0.001(2) -0.003(2) 0.0042(19) C19 0.025(3) 0.016(3) 0.016(2) 0.0022(19) -0.005(2) -0.001(2) C20 0.020(3) 0.018(3) 0.021(2) 0.002(2) 0.005(2) 0.003(2) C21 0.020(3) 0.038(3) 0.031(3) -0.002(2) 0.010(2) 0.006(2) C22 0.027(3) 0.034(3) 0.030(3) 0.009(2) 0.014(2) 0.001(2) C23 0.031(3) 0.023(3) 0.026(3) 0.003(2) 0.003(2) 0.002(2) C24 0.013(2) 0.020(3) 0.019(2) 0.0020(19) 0.0052(19) 0.0024(19) C25 0.035(3) 0.032(3) 0.031(3) 0.015(2) 0.005(2) 0.005(2) C26 0.046(3) 0.036(3) 0.015(2) 0.002(2) 0.004(2) 0.016(3) C27 0.032(3) 0.036(3) 0.034(3) 0.001(2) 0.013(2) 0.011(2) C28 0.048(4) 0.051(4) 0.053(4) 0.022(3) 0.027(3) 0.005(3) C29 0.069(5) 0.072(5) 0.072(5) 0.049(4) 0.032(4) 0.030(4) C30 0.079(5) 0.038(4) 0.058(4) 0.023(3) 0.005(3) 0.023(3) C31 0.069(5) 0.062(5) 0.051(4) 0.037(3) -0.009(3) 0.008(3) C32 0.105(5) 0.053(4) 0.021(3) 0.007(3) -0.004(3) 0.039(4) C33 0.092(5) 0.091(6) 0.026(3) 0.002(3) 0.018(3) 0.032(4) C34 0.083(5) 0.058(5) 0.033(3) -0.007(3) -0.011(3) 0.014(4) C35 0.041(3) 0.051(4) 0.041(3) -0.013(3) 0.019(3) -0.004(3) C36 0.035(3) 0.042(4) 0.054(4) -0.001(3) 0.015(3) 0.017(3) C37 0.041(3) 0.045(4) 0.049(4) 0.015(3) 0.014(3) 0.012(3) C38 0.099(7) 0.155(9) 0.078(6) 0.021(6) 0.064(5) 0.003(6) C39 0.114(7) 0.099(7) 0.237(11) 0.113(8) 0.137(7) 0.059(6) C40 0.042(4) 0.112(7) 0.114(6) 0.043(5) 0.038(4) -0.005(4) C41 0.015(3) 0.037(3) 0.025(3) -0.003(2) 0.007(2) 0.006(2) C42 0.036(3) 0.049(4) 0.038(3) -0.027(3) 0.006(3) 0.002(3) C43 0.019(3) 0.069(4) 0.049(4) -0.028(3) 0.011(3) -0.007(3) C44 0.024(3) 0.026(3) 0.028(3) -0.001(2) 0.003(2) 0.009(2) C45 0.032(3) 0.021(3) 0.030(3) 0.004(2) -0.005(2) 0.006(2) C46 0.045(4) 0.032(3) 0.050(4) 0.019(3) -0.018(3) -0.007(3) C47 0.041(3) 0.045(4) 0.059(4) 0.035(3) -0.017(3) -0.003(3) C48 0.031(3) 0.027(3) 0.031(3) 0.010(2) 0.002(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 1.977(3) . ? Co1 O5 1.999(3) . ? Co1 O1 2.016(3) . ? Co1 S1 2.4722(13) . ? Co1 Cl2 2.4791(6) . ? Co1 Cl1 2.7391(13) . ? Co2 O1 2.001(3) . ? Co2 O2 2.004(3) . ? Co2 O6 2.023(3) . ? Co2 O9 2.156(3) . ? Co2 S2 2.5214(12) . ? Co2 Cl1 2.6259(12) . ? Co3 O3 2.012(3) . ? Co3 O2 2.014(3) . ? Co3 O7 2.028(3) . ? Co3 Cl3 2.3959(18) . ? Co3 S3 2.5035(14) . ? Co4 O4 1.998(3) . ? Co4 O3 2.001(3) . ? Co4 O8 2.004(3) . ? Co4 O10 2.115(3) . ? Co4 S4 2.4891(14) . ? Co4 Cl1 2.6161(13) . ? S1 C24 1.784(4) . ? S1 C2 1.787(4) . ? S2 C8 1.786(4) . ? S2 C6 1.795(4) . ? S3 C12 1.794(4) . ? S3 C14 1.799(4) . ? S4 C20 1.775(5) . ? S4 C18 1.786(4) . ? Cl2 Co1 2.4792(6) 2_776 ? O1 C1 1.336(5) . ? O2 C7 1.323(5) . ? O3 C13 1.318(5) . ? O4 C19 1.343(5) . ? O5 C44 1.265(5) . ? O6 C44 1.258(5) . ? O7 C48 1.282(5) . ? O8 C48 1.260(5) . ? C1 C2 1.397(6) . ? C1 C6 1.407(5) . ? C2 C3 1.377(6) . ? C3 C4 1.389(6) . ? C3 H3A 0.9500 . ? C4 C5 1.395(6) . ? C4 C25 1.530(6) . ? C5 C6 1.391(6) . ? C5 H5A 0.9500 . ? C7 C12 1.396(6) . ? C7 C8 1.398(6) . ? C8 C9 1.412(5) . ? C9 C10 1.389(6) . ? C9 H9A 0.9500 . ? C10 C11 1.403(6) . ? C10 C26 1.543(6) . ? C11 C12 1.406(6) . ? C11 H11A 0.9500 . ? C13 C14 1.401(6) . ? C13 C18 1.419(6) . ? C14 C15 1.398(6) . ? C15 C16 1.389(6) . ? C15 H15A 0.9500 . ? C16 C17 1.401(6) . ? C16 C27 1.529(6) . ? C17 C18 1.371(6) . ? C17 H17A 0.9500 . ? C19 C24 1.390(6) . ? C19 C20 1.423(6) . ? C20 C21 1.384(6) . ? C21 C22 1.402(7) . ? C21 H21A 0.9500 . ? C22 C23 1.397(7) . ? C22 C28 1.519(7) . ? C23 C24 1.386(6) . ? C23 H23A 0.9500 . ? C25 C30 1.510(7) . ? C25 C29 1.516(7) . ? C25 C31 1.538(6) . ? C26 C32 1.507(7) . ? C26 C34 1.540(7) . ? C26 C33 1.540(7) . ? C27 C35 1.519(6) . ? C27 C36 1.548(6) . ? C27 C37 1.554(7) . ? C28 C39 1.453(9) . ? C28 C38 1.512(9) . ? C28 C40 1.544(8) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.380(6) . ? C41 C43 1.383(6) . ? C41 C44 1.486(6) . ? C42 C43 1.382(7) 2_676 ? C42 H42A 0.9500 . ? C43 C42 1.382(7) 2_676 ? C43 H43A 0.9500 . ? C45 C46 1.362(6) . ? C45 C47 1.386(6) 2_766 ? C45 C48 1.502(6) . ? C46 C47 1.370(7) . ? C46 H46A 0.9500 . ? C47 C45 1.386(6) 2_766 ? C47 H47A 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 O4 Co1 O5 172.71(13) . . ? O4 Co1 O1 92.38(12) . . ? O5 Co1 O1 92.35(12) . . ? O4 Co1 S1 84.04(9) . . ? O5 Co1 S1 102.06(10) . . ? O1 Co1 S1 82.88(8) . . ? O4 Co1 Cl2 89.95(8) . . ? O5 Co1 Cl2 85.55(9) . . ? O1 Co1 Cl2 176.82(9) . . ? S1 Co1 Cl2 95.21(3) . . ? O4 Co1 Cl1 80.78(9) . . ? O5 Co1 Cl1 94.56(10) . . ? O1 Co1 Cl1 80.24(8) . . ? S1 Co1 Cl1 156.72(4) . . ? Cl2 Co1 Cl1 102.29(3) . . ? O1 Co2 O2 94.90(12) . . ? O1 Co2 O6 91.99(12) . . ? O2 Co2 O6 172.15(12) . . ? O1 Co2 O9 176.71(12) . . ? O2 Co2 O9 87.41(12) . . ? O6 Co2 O9 85.55(13) . . ? O1 Co2 S2 81.49(8) . . ? O2 Co2 S2 82.26(8) . . ? O6 Co2 S2 102.52(9) . . ? O9 Co2 S2 101.15(9) . . ? O1 Co2 Cl1 83.42(8) . . ? O2 Co2 Cl1 84.13(8) . . ? O6 Co2 Cl1 92.95(9) . . ? O9 Co2 Cl1 94.52(9) . . ? S2 Co2 Cl1 158.68(5) . . ? O3 Co3 O2 90.88(12) . . ? O3 Co3 O7 90.61(12) . . ? O2 Co3 O7 172.15(14) . . ? O3 Co3 Cl3 177.81(10) . . ? O2 Co3 Cl3 90.81(9) . . ? O7 Co3 Cl3 87.90(10) . . ? O3 Co3 S3 81.81(9) . . ? O2 Co3 S3 83.29(9) . . ? O7 Co3 S3 104.55(11) . . ? Cl3 Co3 S3 97.01(6) . . ? O4 Co4 O3 97.92(12) . . ? O4 Co4 O8 170.92(13) . . ? O3 Co4 O8 90.99(12) . . ? O4 Co4 O10 87.50(12) . . ? O3 Co4 O10 173.99(13) . . ? O8 Co4 O10 83.52(13) . . ? O4 Co4 S4 82.77(9) . . ? O3 Co4 S4 82.30(9) . . ? O8 Co4 S4 100.23(11) . . ? O10 Co4 S4 101.03(10) . . ? O4 Co4 Cl1 83.61(9) . . ? O3 Co4 Cl1 83.99(9) . . ? O8 Co4 Cl1 95.67(10) . . ? O10 Co4 Cl1 94.10(10) . . ? S4 Co4 Cl1 159.12(4) . . ? C24 S1 C2 103.2(2) . . ? C24 S1 Co1 93.83(15) . . ? C2 S1 Co1 93.81(15) . . ? C8 S2 C6 105.0(2) . . ? C8 S2 Co2 93.69(14) . . ? C6 S2 Co2 94.12(14) . . ? C12 S3 C14 103.8(2) . . ? C12 S3 Co3 92.96(16) . . ? C14 S3 Co3 94.41(15) . . ? C20 S4 C18 102.7(2) . . ? C20 S4 Co4 94.64(16) . . ? C18 S4 Co4 94.60(16) . . ? Co4 Cl1 Co2 119.94(5) . . ? Co4 Cl1 Co1 77.86(4) . . ? Co2 Cl1 Co1 74.68(3) . . ? Co1 Cl2 Co1 179.998(16) . 2_776 ? C1 O1 Co2 122.3(3) . . ? C1 O1 Co1 119.6(3) . . ? Co2 O1 Co1 108.25(13) . . ? C7 O2 Co2 122.9(3) . . ? C7 O2 Co3 121.8(3) . . ? Co2 O2 Co3 115.31(13) . . ? C13 O3 Co4 122.2(3) . . ? C13 O3 Co3 121.3(3) . . ? Co4 O3 Co3 109.42(14) . . ? C19 O4 Co1 120.8(3) . . ? C19 O4 Co4 122.9(3) . . ? Co1 O4 Co4 115.76(14) . . ? C44 O5 Co1 128.9(3) . . ? C44 O6 Co2 131.1(3) . . ? C48 O7 Co3 131.4(3) . . ? C48 O8 Co4 131.9(3) . . ? O1 C1 C2 121.4(4) . . ? O1 C1 C6 120.9(4) . . ? C2 C1 C6 117.6(4) . . ? C3 C2 C1 120.2(4) . . ? C3 C2 S1 120.6(3) . . ? C1 C2 S1 118.9(3) . . ? C2 C3 C4 123.2(4) . . ? C2 C3 H3A 118.4 . . ? C4 C3 H3A 118.4 . . ? C3 C4 C5 116.5(4) . . ? C3 C4 C25 119.6(4) . . ? C5 C4 C25 123.9(4) . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C5 C6 C1 120.8(4) . . ? C5 C6 S2 120.7(3) . . ? C1 C6 S2 118.3(3) . . ? O2 C7 C12 121.4(4) . . ? O2 C7 C8 121.6(4) . . ? C12 C7 C8 117.0(4) . . ? C7 C8 C9 121.5(4) . . ? C7 C8 S2 119.5(3) . . ? C9 C8 S2 118.8(3) . . ? C10 C9 C8 121.2(4) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C9 C10 C11 117.5(4) . . ? C9 C10 C26 122.6(4) . . ? C11 C10 C26 119.8(4) . . ? C10 C11 C12 121.0(4) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C7 C12 C11 121.6(4) . . ? C7 C12 S3 120.4(3) . . ? C11 C12 S3 118.0(3) . . ? O3 C13 C14 122.7(4) . . ? O3 C13 C18 121.3(4) . . ? C14 C13 C18 116.0(4) . . ? C15 C14 C13 121.4(4) . . ? C15 C14 S3 121.1(3) . . ? C13 C14 S3 117.3(3) . . ? C16 C15 C14 122.1(4) . . ? C16 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C15 C16 C17 116.2(4) . . ? C15 C16 C27 123.9(4) . . ? C17 C16 C27 119.9(4) . . ? C18 C17 C16 122.5(4) . . ? C18 C17 H17A 118.7 . . ? C16 C17 H17A 118.7 . . ? C17 C18 C13 121.5(4) . . ? C17 C18 S4 120.5(3) . . ? C13 C18 S4 117.9(4) . . ? O4 C19 C24 122.4(4) . . ? O4 C19 C20 119.9(4) . . ? C24 C19 C20 117.8(4) . . ? C21 C20 C19 119.5(4) . . ? C21 C20 S4 121.0(4) . . ? C19 C20 S4 119.5(3) . . ? C20 C21 C22 123.2(5) . . ? C20 C21 H21A 118.4 . . ? C22 C21 H21A 118.4 . . ? C23 C22 C21 115.9(4) . . ? C23 C22 C28 123.8(5) . . ? C21 C22 C28 120.3(5) . . ? C24 C23 C22 122.3(5) . . ? C24 C23 H23A 118.8 . . ? C22 C23 H23A 118.8 . . ? C23 C24 C19 121.2(4) . . ? C23 C24 S1 119.9(4) . . ? C19 C24 S1 118.9(3) . . ? C30 C25 C29 110.2(5) . . ? C30 C25 C4 109.5(4) . . ? C29 C25 C4 108.8(4) . . ? C30 C25 C31 107.5(5) . . ? C29 C25 C31 108.8(5) . . ? C4 C25 C31 112.1(4) . . ? C32 C26 C34 111.0(5) . . ? C32 C26 C33 107.4(5) . . ? C34 C26 C33 108.7(5) . . ? C32 C26 C10 111.9(4) . . ? C34 C26 C10 108.2(4) . . ? C33 C26 C10 109.7(4) . . ? C35 C27 C16 113.7(4) . . ? C35 C27 C36 108.4(4) . . ? C16 C27 C36 110.2(4) . . ? C35 C27 C37 108.4(4) . . ? C16 C27 C37 108.2(4) . . ? C36 C27 C37 107.8(4) . . ? C39 C28 C38 111.3(6) . . ? C39 C28 C22 112.9(5) . . ? C38 C28 C22 111.2(5) . . ? C39 C28 C40 106.3(6) . . ? C38 C28 C40 104.2(6) . . ? C22 C28 C40 110.5(5) . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C25 C31 H31A 109.5 . . ? C25 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C25 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C26 C33 H33A 109.5 . . ? C26 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C26 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C26 C34 H34A 109.5 . . ? C26 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C26 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C27 C35 H35A 109.5 . . ? C27 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C27 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C27 C36 H36A 109.5 . . ? C27 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C27 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C27 C37 H37A 109.5 . . ? C27 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C27 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C28 C38 H38A 109.5 . . ? C28 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C28 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C28 C39 H39A 109.5 . . ? C28 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C28 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C28 C40 H40A 109.5 . . ? C28 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C28 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C43 118.3(4) . . ? C42 C41 C44 119.6(4) . . ? C43 C41 C44 122.1(4) . . ? C41 C42 C43 121.4(5) . 2_676 ? C41 C42 H42A 119.3 . . ? C43 C42 H42A 119.3 2_676 . ? C42 C43 C41 120.3(5) 2_676 . ? C42 C43 H43A 119.9 2_676 . ? C41 C43 H43A 119.9 . . ? O6 C44 O5 126.3(4) . . ? O6 C44 C41 117.6(4) . . ? O5 C44 C41 116.1(4) . . ? C46 C45 C47 118.9(5) . 2_766 ? C46 C45 C48 122.3(4) . . ? C47 C45 C48 118.8(4) 2_766 . ? C45 C46 C47 121.3(5) . . ? C45 C46 H46A 119.4 . . ? C47 C46 H46A 119.4 . . ? C46 C47 C45 119.8(5) . 2_766 ? C46 C47 H47A 120.1 . . ? C45 C47 H47A 120.1 2_766 . ? O8 C48 O7 125.3(4) . . ? O8 C48 C45 117.7(4) . . ? O7 C48 C45 116.9(4) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.230 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.088 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.031 -0.034 -0.034 1513 480 ' ' _platon_squeeze_details ; ; ###END