# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 loop_ _publ_author_address ; State Key Lab of Rare Earth Resource Utilization Changchun Institute of Applied Chemistry CAS, Changchun 130022 P.R. China ; #TrackingRef '- CCDC869988-revised.cif' _publ_contact_author 'Wuping Liao' _publ_contact_author_email wpliao@ciac.jl.cn _publ_contact_author_name 'Wuping Liao' loop_ _publ_author_name 'Shangchao Du' 'Wuping Liao.' data_1-Co-BTC _database_code_depnum_ccdc_archive 'CCDC 869988' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co24(OH)6(C40H44S4O12)6(C9H3O6)8) _chemical_melting_point ? _chemical_formula_moiety 'C312 H294 Co24 O126 S24' _chemical_formula_sum 'C312 H294 Co24 O126 S24' # Excluding the disordered counter cations and solvents. _chemical_formula_weight 8243.23 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 Tetragonal _symmetry_space_group_name_H-M 'I 4/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 26.3094(9) _cell_length_b 26.3094(9) _cell_length_c 44.152(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 30562(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9456 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.896 # Unidentified solvents are not included in the calculation. _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8412 _exptl_absorpt_coefficient_mu 0.765 # Unidentified solvents are not included in the calculation. _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6166 _exptl_absorpt_correction_T_max 0.7345 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 220985 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 25.10 _reflns_number_total 13804 _reflns_number_gt 11902 _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. Since the data resolution is low due to the disordered solvents and cations, the constraints and restraints are applied to make the bond lengths, bond angles, and atomic displacements more meaningful. dfix 1.45 c29 c33 dfix 1.45 c30 c36 isor 0.0001 c29 c30 c35 isor 0.0001 c37 isor 0.0001 O18 delu 0.001 simu 0.001 ; _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^)+(0.1304P)^2^+281.2834P] 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 13804 _refine_ls_number_parameters 571 _refine_ls_number_restraints 581 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2441 _refine_ls_wR_factor_gt 0.2372 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.225 _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 0.83931(3) 0.24340(3) 0.048996(16) 0.0228(2) Uani 1 1 d U . . Co2 Co 0.77127(4) 0.19893(4) 0.0000 0.0227(2) Uani 1 2 d SU . . Co3 Co 0.93211(3) -0.04500(3) 0.174406(16) 0.0252(2) Uani 1 1 d U . . Co4 Co 0.90732(4) 0.28689(4) 0.0000 0.0236(2) Uani 1 2 d SU . . S1 S 0.78883(5) 0.32351(5) 0.09016(3) 0.0274(3) Uani 1 1 d U . . S2 S 0.66184(7) 0.24201(7) 0.0000 0.0258(4) Uani 1 2 d SU . . S3 S 0.91648(7) 0.40353(8) 0.0000 0.0272(4) Uani 1 2 d SU . . S4 S 0.87501(6) -0.08489(6) 0.23053(3) 0.0359(3) Uani 1 1 d U . . C1 C 0.7275(2) 0.2812(2) 0.04428(15) 0.0349(5) Uani 1 1 d U . . C2 C 0.6777(2) 0.2796(3) 0.03181(16) 0.0384(6) Uani 1 1 d U . . C3 C 0.6373(3) 0.3086(3) 0.04252(17) 0.0435(6) Uani 1 1 d U . . H3 H 0.6050 0.3054 0.0332 0.052 Uiso 1 1 calc R . . C4 C 0.6431(3) 0.3423(3) 0.06651(18) 0.0475(6) Uani 1 1 d U . . C5 C 0.6909(3) 0.3428(3) 0.08052(17) 0.0442(6) Uani 1 1 d U . . H5 H 0.6957 0.3634 0.0980 0.053 Uiso 1 1 calc R . . C6 C 0.7315(2) 0.3143(3) 0.06983(16) 0.0392(5) Uani 1 1 d U . . C7 C 0.8531(2) 0.3610(2) 0.04470(14) 0.0331(5) Uani 1 1 d U . . C8 C 0.8230(3) 0.3713(2) 0.07079(14) 0.0359(5) Uani 1 1 d U . . C9 C 0.8174(3) 0.4196(2) 0.08299(15) 0.0403(6) Uani 1 1 d U . . H9 H 0.7971 0.4239 0.1006 0.048 Uiso 1 1 calc R . . C10 C 0.8405(3) 0.4615(3) 0.07021(16) 0.0451(6) Uani 1 1 d U . . C11 C 0.8705(3) 0.4535(2) 0.04469(15) 0.0404(6) Uani 1 1 d U . . H11 H 0.8872 0.4816 0.0356 0.048 Uiso 1 1 calc R . . C12 C 0.8767(3) 0.4053(2) 0.03216(14) 0.0358(6) Uani 1 1 d U . . C13 C 0.8964(3) 0.0200(3) 0.22910(16) 0.0446(6) Uani 1 1 d U . . C14 C 0.8722(3) -0.0217(3) 0.24386(17) 0.0491(6) Uani 1 1 d U . . C15 C 0.8433(3) -0.0161(3) 0.26972(18) 0.0536(7) Uani 1 1 d U . . H15 H 0.8284 -0.0454 0.2787 0.064 Uiso 1 1 calc R . . C16 C 0.8353(3) 0.0316(3) 0.28307(19) 0.0573(6) Uani 1 1 d U . . C17 C 0.8001(2) 0.1385(2) 0.05424(13) 0.0281(5) Uani 1 1 d U . . C18 C 0.8046(2) 0.0868(2) 0.06924(13) 0.0285(5) Uani 1 1 d U . . C19 C 0.8340(2) 0.0808(2) 0.09502(13) 0.0285(5) Uani 1 1 d U . . H19 H 0.8502 0.1095 0.1038 0.034 Uiso 1 1 calc R . . C20 C 0.8400(2) 0.0331(2) 0.10824(13) 0.0289(5) Uani 1 1 d U . . C21 C 0.7808(2) 0.0451(2) 0.05628(13) 0.0291(5) Uani 1 1 d U . . H21 H 0.7607 0.0493 0.0385 0.035 Uiso 1 1 calc R . . C22 C 0.8742(2) 0.0258(2) 0.13505(13) 0.0291(5) Uani 1 1 d U . . C23 C 0.7627(2) -0.0486(2) 0.05435(13) 0.0306(5) Uani 1 1 d U . . C24 C 0.7861(2) -0.0030(2) 0.06919(13) 0.0296(5) Uani 1 1 d U . . C25 C 0.8159(2) -0.0090(2) 0.09510(13) 0.0293(5) Uani 1 1 d U . . H25 H 0.8198 -0.0417 0.1039 0.035 Uiso 1 1 calc R . . C26 C 0.8588(3) 0.0724(3) 0.26990(17) 0.0528(7) Uani 1 1 d U . . H26 H 0.8548 0.1051 0.2787 0.063 Uiso 1 1 calc R . . C27 C 0.8884(3) 0.0675(3) 0.24400(16) 0.0484(6) Uani 1 1 d U . . C28 C 0.8354(3) 0.5153(3) 0.08379(18) 0.0516(6) Uani 1 1 d U . . C29 C 0.5992(3) 0.3784(3) 0.07523(19) 0.0531(7) Uani 1 1 d DU . . C30 C 0.8052(3) 0.0340(3) 0.3136(2) 0.0611(7) Uani 1 1 d DU . . C31 C 0.6108(3) 0.4087(3) 0.1015(2) 0.0596(10) Uani 1 1 d U . . H31A H 0.6426 0.4272 0.0981 0.089 Uiso 1 1 calc R . . H31B H 0.6145 0.3865 0.1192 0.089 Uiso 1 1 calc R . . H31C H 0.5832 0.4330 0.1050 0.089 Uiso 1 1 calc R . . C32 C 0.5520(3) 0.3461(3) 0.0793(2) 0.0594(10) Uani 1 1 d U . . H32A H 0.5581 0.3208 0.0952 0.089 Uiso 1 1 calc R . . H32B H 0.5441 0.3287 0.0603 0.089 Uiso 1 1 calc R . . H32C H 0.5234 0.3678 0.0852 0.089 Uiso 1 1 calc R . . C33 C 0.5886(3) 0.4176(3) 0.0506(2) 0.0635(11) Uani 1 1 d DU . . H33A H 0.5631 0.4419 0.0578 0.095 Uiso 1 1 calc R . . H33B H 0.5759 0.4004 0.0324 0.095 Uiso 1 1 calc R . . H33C H 0.6201 0.4357 0.0456 0.095 Uiso 1 1 calc R . . C34 C 0.7570(4) 0.0057(4) 0.3096(2) 0.0678(11) Uani 1 1 d U . . H34A H 0.7371 0.0073 0.3284 0.102 Uiso 1 1 calc R . . H34B H 0.7645 -0.0299 0.3048 0.102 Uiso 1 1 calc R . . H34C H 0.7374 0.0209 0.2930 0.102 Uiso 1 1 calc R . . C35 C 0.8049(4) 0.0829(3) 0.3260(2) 0.0639(10) Uani 1 1 d U . . H35A H 0.7861 0.1059 0.3127 0.096 Uiso 1 1 calc R . . H35B H 0.8400 0.0950 0.3282 0.096 Uiso 1 1 calc R . . H35C H 0.7885 0.0820 0.3460 0.096 Uiso 1 1 calc R . . C36 C 0.8353(4) 0.0057(4) 0.3392(2) 0.0687(11) Uani 1 1 d DU . . H36A H 0.8682 0.0224 0.3423 0.103 Uiso 1 1 calc R . . H36B H 0.8408 -0.0298 0.3333 0.103 Uiso 1 1 calc R . . H36C H 0.8157 0.0068 0.3581 0.103 Uiso 1 1 calc R . . C37 C 0.8179(3) 0.5519(3) 0.0607(2) 0.0597(10) Uani 1 1 d U . . H37A H 0.7858 0.5400 0.0519 0.090 Uiso 1 1 calc R . . H37B H 0.8436 0.5546 0.0446 0.090 Uiso 1 1 calc R . . H37C H 0.8128 0.5852 0.0700 0.090 Uiso 1 1 calc R . . C38 C 0.8832(3) 0.5334(3) 0.09333(19) 0.0584(10) Uani 1 1 d U . . H38A H 0.9061 0.5356 0.0759 0.088 Uiso 1 1 calc R . . H38B H 0.8976 0.5100 0.1083 0.088 Uiso 1 1 calc R . . H38C H 0.8793 0.5671 0.1024 0.088 Uiso 1 1 calc R . . C39 C 0.8010(4) 0.5153(3) 0.1113(2) 0.0626(11) Uani 1 1 d U . . H39A H 0.7981 0.5499 0.1193 0.094 Uiso 1 1 calc R . . H39B H 0.8153 0.4930 0.1269 0.094 Uiso 1 1 calc R . . H39C H 0.7672 0.5029 0.1055 0.094 Uiso 1 1 calc R . . O1 O 0.76546(15) 0.25531(15) 0.03351(9) 0.0304(5) Uani 1 1 d U . . O2 O 0.85831(16) 0.31584(15) 0.03303(9) 0.0309(5) Uani 1 1 d U . . O3 O 0.92352(19) 0.01535(17) 0.20464(10) 0.0405(6) Uani 1 1 d U . . O4 O 0.81815(15) 0.27670(15) 0.09051(9) 0.0279(4) Uani 1 1 d U . . O5 O 0.77559(15) 0.34371(16) 0.11935(9) 0.0315(6) Uani 1 1 d U . . O6 O 0.6918(2) 0.1954(2) 0.0000 0.0262(5) Uani 1 2 d SU . . O7 O 0.6079(2) 0.2353(2) 0.0000 0.0282(8) Uani 1 2 d SU . . O8 O 0.9456(2) 0.3566(2) 0.0000 0.0286(5) Uani 1 2 d SU . . O9 O 0.9458(2) 0.4492(2) 0.0000 0.0309(8) Uani 1 2 d SU . . O10 O 0.87487(16) -0.08475(17) 0.19770(9) 0.0354(5) Uani 1 1 d U . . O11 O 0.83397(17) -0.11225(18) 0.24448(10) 0.0408(8) Uani 1 1 d U . . O12 O 0.87876(15) -0.01837(15) 0.14532(9) 0.0296(5) Uani 1 1 d U . . O13 O 0.89640(16) 0.06462(15) 0.14486(9) 0.0297(6) Uani 1 1 d U . . O14 O 0.77433(15) 0.14148(14) 0.03058(9) 0.0283(5) Uani 1 1 d U . . O15 O 0.82319(15) 0.17488(15) 0.06676(9) 0.0286(5) Uani 1 1 d U . . O16 O 0.76939(16) -0.09110(15) 0.06674(9) 0.0308(6) Uani 1 1 d U . . O17 O 0.73799(16) -0.04121(15) 0.03035(9) 0.0317(6) Uani 1 1 d U . . O18 O 0.8558(2) 0.2175(2) 0.0000 0.0255(5) Uani 1 2 d SU . . H18A H 0.8756 0.1868 0.0000 0.031 Uiso 1 2 d SR . . O19 O 1.0000 0.0000 0.1565(2) 0.0325(8) Uani 1 4 d SU . . H19A H 1.0000 0.0000 0.1349 0.049 Uiso 1 4 d 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(4) 0.0244(4) 0.0208(4) -0.0007(3) 0.0004(3) -0.0001(3) Co2 0.0276(5) 0.0221(5) 0.0184(5) 0.000 0.000 0.0013(4) Co3 0.0319(4) 0.0302(4) 0.0134(4) 0.0019(3) 0.0007(3) 0.0015(3) Co4 0.0245(5) 0.0287(5) 0.0177(5) 0.000 0.000 0.0016(4) S1 0.0284(6) 0.0314(6) 0.0223(6) -0.0069(5) 0.0050(4) -0.0047(5) S2 0.0242(7) 0.0253(8) 0.0279(9) 0.000 0.000 -0.0043(6) S3 0.0235(8) 0.0320(7) 0.0260(8) 0.000 0.000 -0.0064(6) S4 0.0400(8) 0.0443(7) 0.0233(7) 0.0077(5) 0.0060(5) -0.0032(6) C1 0.0289(8) 0.0368(10) 0.0390(11) -0.0155(8) -0.0043(7) 0.0032(7) C2 0.0292(9) 0.0417(11) 0.0441(12) -0.0163(9) -0.0057(9) 0.0027(9) C3 0.0327(9) 0.0479(12) 0.0498(12) -0.0179(9) -0.0047(10) 0.0047(9) C4 0.0388(8) 0.0513(11) 0.0525(11) -0.0201(9) -0.0032(9) 0.0057(8) C5 0.0371(9) 0.0473(12) 0.0481(12) -0.0222(10) -0.0022(9) 0.0041(9) C6 0.0337(8) 0.0415(12) 0.0424(12) -0.0196(9) -0.0039(8) 0.0026(8) C7 0.0415(11) 0.0288(7) 0.0290(11) -0.0023(7) 0.0115(8) -0.0040(8) C8 0.0449(12) 0.0324(8) 0.0305(11) -0.0033(8) 0.0133(9) -0.0034(9) C9 0.0518(13) 0.0345(8) 0.0347(12) -0.0052(9) 0.0151(10) -0.0033(10) C10 0.0583(12) 0.0370(8) 0.0401(11) -0.0049(9) 0.0158(10) -0.0055(9) C11 0.0524(13) 0.0319(9) 0.0368(12) -0.0022(9) 0.0131(10) -0.0063(10) C12 0.0452(12) 0.0300(8) 0.0323(12) -0.0009(9) 0.0118(9) -0.0057(9) C13 0.0572(14) 0.0449(9) 0.0317(11) -0.0090(9) 0.0073(10) -0.0031(11) C14 0.0601(14) 0.0495(10) 0.0377(12) -0.0039(9) 0.0080(11) -0.0058(11) C15 0.0637(14) 0.0538(11) 0.0432(12) -0.0035(9) 0.0114(10) -0.0058(11) C16 0.0660(12) 0.0569(10) 0.0491(10) -0.0059(8) 0.0118(9) -0.0035(10) C17 0.0360(11) 0.0265(7) 0.0217(9) 0.0025(7) -0.0028(8) -0.0026(8) C18 0.0368(10) 0.0263(8) 0.0223(9) 0.0020(7) -0.0038(8) -0.0009(8) C19 0.0365(11) 0.0264(9) 0.0227(10) 0.0015(8) -0.0041(9) -0.0008(9) C20 0.0366(10) 0.0267(9) 0.0234(9) 0.0016(7) -0.0045(8) -0.0003(8) C21 0.0380(11) 0.0262(8) 0.0231(10) 0.0017(9) -0.0048(9) -0.0005(9) C22 0.0354(10) 0.0275(10) 0.0245(10) 0.0023(8) -0.0048(8) -0.0002(8) C23 0.0411(12) 0.0265(9) 0.0243(10) 0.0010(9) -0.0062(9) -0.0003(9) C24 0.0389(11) 0.0263(8) 0.0236(10) 0.0014(8) -0.0053(8) -0.0002(9) C25 0.0379(11) 0.0264(9) 0.0237(10) 0.0015(9) -0.0050(9) -0.0001(9) C26 0.0639(14) 0.0522(11) 0.0422(12) -0.0116(10) 0.0116(10) -0.0014(11) C27 0.0607(14) 0.0479(10) 0.0366(12) -0.0118(10) 0.0086(11) -0.0011(12) C28 0.0678(14) 0.0389(10) 0.0482(12) -0.0073(9) 0.0147(11) -0.0033(11) C29 0.0463(9) 0.0553(10) 0.0577(10) -0.0160(8) 0.0004(8) 0.0090(8) C30 0.0667(11) 0.0623(10) 0.0544(10) -0.0041(8) 0.0129(8) -0.0014(8) C31 0.053(2) 0.061(2) 0.0645(17) -0.0241(14) 0.0035(18) 0.0124(17) C32 0.0448(14) 0.067(2) 0.067(2) -0.0185(18) 0.0061(18) 0.0078(14) C33 0.058(2) 0.0619(19) 0.0703(18) -0.0091(15) -0.0022(19) 0.0151(15) C34 0.0712(17) 0.071(2) 0.062(2) -0.008(2) 0.0187(14) -0.0076(16) C35 0.0665(14) 0.0653(11) 0.0598(13) -0.0075(9) 0.0072(10) 0.0013(9) C36 0.081(2) 0.0699(19) 0.0556(16) 0.0028(18) 0.0131(17) 0.0011(19) C37 0.0667(14) 0.0516(11) 0.0609(13) 0.0000(10) 0.0074(10) 0.0022(10) C38 0.0754(18) 0.046(2) 0.054(2) -0.0092(18) 0.0040(14) -0.0070(17) C39 0.085(2) 0.047(2) 0.0560(18) -0.0125(15) 0.0243(17) 0.001(2) O1 0.0271(8) 0.0307(10) 0.0333(12) -0.0104(8) -0.0046(7) 0.0031(7) O2 0.0379(12) 0.0277(7) 0.0271(12) -0.0018(7) 0.0105(9) -0.0041(9) O3 0.0533(15) 0.0419(11) 0.0263(11) -0.0088(9) 0.0034(9) -0.0027(11) O4 0.0297(10) 0.0317(8) 0.0225(8) -0.0045(7) 0.0044(7) -0.0046(8) O5 0.0338(16) 0.0355(15) 0.0252(11) -0.0091(11) 0.0081(9) -0.0064(12) O6 0.0265(7) 0.0251(11) 0.0271(13) 0.000 0.000 -0.0039(8) O7 0.0248(10) 0.0289(18) 0.0308(18) 0.000 0.000 -0.0046(11) O8 0.0246(11) 0.0340(9) 0.0272(13) 0.000 0.000 -0.0049(7) O9 0.0272(17) 0.0340(12) 0.0313(18) 0.000 0.000 -0.0081(12) O10 0.0393(11) 0.0434(11) 0.0235(9) 0.0065(7) 0.0051(9) -0.0035(9) O11 0.0430(16) 0.0499(15) 0.0294(15) 0.0083(14) 0.0107(13) -0.0037(13) O12 0.0340(10) 0.0281(11) 0.0267(11) 0.0031(8) -0.0054(9) -0.0002(10) O13 0.0362(13) 0.0283(11) 0.0247(12) 0.0019(10) -0.0050(10) -0.0010(10) O14 0.0362(11) 0.0269(9) 0.0219(11) 0.0036(7) -0.0031(9) -0.0032(9) O15 0.0363(13) 0.0275(7) 0.0220(10) 0.0012(7) -0.0016(9) -0.0038(9) O16 0.0417(14) 0.0262(10) 0.0245(13) 0.0008(10) -0.0064(11) -0.0004(11) O17 0.0427(14) 0.0274(12) 0.0252(12) 0.0010(10) -0.0074(10) -0.0008(11) O18 0.0273(7) 0.0288(9) 0.0206(8) 0.000 0.000 -0.0019(7) O19 0.0273(10) 0.0273(10) 0.043(3) 0.000 0.000 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 O15 2.011(4) . ? Co1 O16 2.020(4) 4_665 ? Co1 O1 2.083(4) . ? Co1 O2 2.093(4) . ? Co1 O4 2.106(4) . ? Co1 O18 2.310(2) . ? Co2 O14 2.028(4) . ? Co2 O14 2.028(4) 10 ? Co2 O6 2.093(5) . ? Co2 O1 2.101(4) . ? Co2 O1 2.101(4) 10 ? Co2 O18 2.277(5) . ? Co3 O13 2.022(4) 3_645 ? Co3 O12 2.027(4) . ? Co3 O3 2.086(4) . ? Co3 O3 2.092(5) 3_645 ? Co3 O10 2.102(4) . ? Co3 O19 2.285(3) . ? Co4 O17 2.014(4) 4_665 ? Co4 O17 2.014(4) 11_665 ? Co4 O2 2.090(4) 10 ? Co4 O2 2.090(4) . ? Co4 O8 2.093(6) . ? Co4 O18 2.275(5) . ? S1 O5 1.437(4) . ? S1 O4 1.453(4) . ? S1 C8 1.766(6) . ? S1 C6 1.771(6) . ? S2 O7 1.429(6) . ? S2 O6 1.458(6) . ? S2 C2 1.768(6) 10 ? S2 C2 1.768(6) . ? S3 O9 1.427(6) . ? S3 O8 1.453(6) . ? S3 C12 1.765(6) . ? S3 C12 1.765(6) 10 ? S4 O11 1.436(5) . ? S4 O10 1.450(4) . ? S4 C14 1.764(8) . ? S4 C27 1.770(8) 3_645 ? C1 O1 1.298(7) . ? C1 C2 1.423(8) . ? C1 C6 1.430(8) . ? C2 C3 1.391(9) . ? C3 C4 1.389(10) . ? C3 H3 0.9500 . ? C4 C5 1.403(10) . ? C4 C29 1.543(10) . ? C5 C6 1.387(9) . ? C5 H5 0.9500 . ? C7 O2 1.302(7) . ? C7 C8 1.423(8) . ? C7 C12 1.432(8) . ? C8 C9 1.389(9) . ? C9 C10 1.380(9) . ? C9 H9 0.9500 . ? C10 C11 1.392(9) . ? C10 C28 1.542(10) . ? C11 C12 1.392(9) . ? C11 H11 0.9500 . ? C13 O3 1.300(8) . ? C13 C14 1.426(10) . ? C13 C27 1.429(10) . ? C14 C15 1.380(10) . ? C15 C16 1.403(11) . ? C15 H15 0.9500 . ? C16 C26 1.369(12) . ? C16 C30 1.565(11) . ? C17 O14 1.248(7) . ? C17 O15 1.261(7) . ? C17 C18 1.518(8) . ? C18 C19 1.385(8) . ? C18 C21 1.388(8) . ? C19 C20 1.391(8) . ? C19 H19 0.9500 . ? C20 C25 1.403(8) . ? C20 C22 1.500(8) . ? C21 C24 1.395(8) . ? C21 H21 0.9500 . ? C22 O12 1.253(7) . ? C22 O13 1.254(7) . ? C23 O16 1.257(7) . ? C23 O17 1.258(7) . ? C23 C24 1.499(8) . ? C24 C25 1.395(8) . ? C25 H25 0.9500 . ? C26 C27 1.389(10) . ? C26 H26 0.9500 . ? C27 S4 1.770(8) 4_665 ? C28 C38 1.410(12) . ? C28 C37 1.477(12) . ? C28 C39 1.514(11) . ? C29 C31 1.439(11) . ? C29 C32 1.516(11) . ? C29 C33 1.526(11) . ? C30 C35 1.399(12) . ? C30 C34 1.481(12) . ? C30 C36 1.570(11) . ? 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 . ? O3 Co3 2.092(5) 4_665 ? O13 Co3 2.021(4) 4_665 ? O16 Co1 2.020(4) 3_645 ? O17 Co4 2.014(4) 3_645 ? O18 Co1 2.310(2) 10 ? O18 H18A 0.9599 . ? O19 Co3 2.285(3) 3_645 ? O19 Co3 2.285(3) 2_755 ? O19 Co3 2.285(3) 4_665 ? O19 H19A 0.9533 . ? 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 O15 Co1 O16 83.72(16) . 4_665 ? O15 Co1 O1 93.79(16) . . ? O16 Co1 O1 176.16(17) 4_665 . ? O15 Co1 O2 176.46(16) . . ? O16 Co1 O2 93.77(17) 4_665 . ? O1 Co1 O2 88.59(17) . . ? O15 Co1 O4 88.72(16) . . ? O16 Co1 O4 88.36(16) 4_665 . ? O1 Co1 O4 88.66(16) . . ? O2 Co1 O4 88.72(15) . . ? O15 Co1 O18 98.05(17) . . ? O16 Co1 O18 98.25(18) 4_665 . ? O1 Co1 O18 84.98(17) . . ? O2 Co1 O18 84.76(17) . . ? O4 Co1 O18 170.99(17) . . ? O14 Co2 O14 83.5(2) . 10 ? O14 Co2 O6 90.39(16) . . ? O14 Co2 O6 90.38(16) 10 . ? O14 Co2 O1 93.45(16) . . ? O14 Co2 O1 176.33(17) 10 . ? O6 Co2 O1 87.63(15) . . ? O14 Co2 O1 176.33(17) . 10 ? O14 Co2 O1 93.45(16) 10 10 ? O6 Co2 O1 87.63(15) . 10 ? O1 Co2 O1 89.6(2) . 10 ? O14 Co2 O18 96.93(16) . . ? O14 Co2 O18 96.93(16) 10 . ? O6 Co2 O18 170.2(2) . . ? O1 Co2 O18 85.41(15) . . ? O1 Co2 O18 85.41(15) 10 . ? O13 Co3 O12 83.35(16) 3_645 . ? O13 Co3 O3 176.22(18) 3_645 . ? O12 Co3 O3 93.86(18) . . ? O13 Co3 O3 94.68(18) 3_645 3_645 ? O12 Co3 O3 176.58(18) . 3_645 ? O3 Co3 O3 88.0(3) . 3_645 ? O13 Co3 O10 88.10(17) 3_645 . ? O12 Co3 O10 89.19(17) . . ? O3 Co3 O10 89.32(18) . . ? O3 Co3 O10 87.95(17) 3_645 . ? O13 Co3 O19 97.9(2) 3_645 . ? O12 Co3 O19 98.2(2) . . ? O3 Co3 O19 85.0(2) . . ? O3 Co3 O19 84.8(2) 3_645 . ? O10 Co3 O19 170.9(2) . . ? O17 Co4 O17 83.4(2) 4_665 11_665 ? O17 Co4 O2 175.68(17) 4_665 10 ? O17 Co4 O2 93.96(17) 11_665 10 ? O17 Co4 O2 93.96(17) 4_665 . ? O17 Co4 O2 175.68(17) 11_665 . ? O2 Co4 O2 88.5(2) 10 . ? O17 Co4 O8 87.78(17) 4_665 . ? O17 Co4 O8 87.78(17) 11_665 . ? O2 Co4 O8 88.71(16) 10 . ? O2 Co4 O8 88.71(16) . . ? O17 Co4 O18 98.02(16) 4_665 . ? O17 Co4 O18 98.02(16) 11_665 . ? O2 Co4 O18 85.71(15) 10 . ? O2 Co4 O18 85.71(15) . . ? O8 Co4 O18 172.2(2) . . ? O5 S1 O4 115.6(3) . . ? O5 S1 C8 107.1(3) . . ? O4 S1 C8 109.7(3) . . ? O5 S1 C6 107.4(3) . . ? O4 S1 C6 110.0(3) . . ? C8 S1 C6 106.6(3) . . ? O7 S2 O6 115.7(3) . . ? O7 S2 C2 107.6(3) . 10 ? O6 S2 C2 110.1(3) . 10 ? O7 S2 C2 107.6(3) . . ? O6 S2 C2 110.1(3) . . ? C2 S2 C2 105.2(5) 10 . ? O9 S3 O8 115.5(3) . . ? O9 S3 C12 107.4(3) . . ? O8 S3 C12 109.6(3) . . ? O9 S3 C12 107.4(3) . 10 ? O8 S3 C12 109.6(3) . 10 ? C12 S3 C12 107.2(5) . 10 ? O11 S4 O10 115.4(3) . . ? O11 S4 C14 107.3(3) . . ? O10 S4 C14 109.3(3) . . ? O11 S4 C27 107.4(3) . 3_645 ? O10 S4 C27 109.8(3) . 3_645 ? C14 S4 C27 107.3(4) . 3_645 ? O1 C1 C2 123.4(5) . . ? O1 C1 C6 123.6(5) . . ? C2 C1 C6 113.0(5) . . ? C3 C2 C1 123.8(6) . . ? C3 C2 S2 113.4(5) . . ? C1 C2 S2 122.8(5) . . ? C4 C3 C2 121.8(6) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C3 C4 C5 116.1(6) . . ? C3 C4 C29 120.1(6) . . ? C5 C4 C29 123.7(6) . . ? C6 C5 C4 122.4(6) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C1 122.8(6) . . ? C5 C6 S1 114.2(5) . . ? C1 C6 S1 123.0(5) . . ? O2 C7 C8 123.5(5) . . ? O2 C7 C12 123.0(5) . . ? C8 C7 C12 113.5(5) . . ? C9 C8 C7 123.2(6) . . ? C9 C8 S1 114.1(5) . . ? C7 C8 S1 122.7(5) . . ? C10 C9 C8 121.7(6) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 C11 117.3(6) . . ? C9 C10 C28 122.4(6) . . ? C11 C10 C28 120.3(6) . . ? C10 C11 C12 121.8(6) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C7 122.5(6) . . ? C11 C12 S3 114.4(5) . . ? C7 C12 S3 123.1(5) . . ? O3 C13 C14 123.6(6) . . ? O3 C13 C27 123.0(7) . . ? C14 C13 C27 113.4(6) . . ? C15 C14 C13 122.8(7) . . ? C15 C14 S4 113.6(6) . . ? C13 C14 S4 123.6(5) . . ? C14 C15 C16 121.7(8) . . ? C14 C15 H15 119.2 . . ? C16 C15 H15 119.2 . . ? C26 C16 C15 117.2(7) . . ? C26 C16 C30 124.2(7) . . ? C15 C16 C30 118.3(7) . . ? O14 C17 O15 125.5(5) . . ? O14 C17 C18 117.6(5) . . ? O15 C17 C18 116.9(5) . . ? C19 C18 C21 120.0(5) . . ? C19 C18 C17 120.3(5) . . ? C21 C18 C17 119.6(5) . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C25 119.1(5) . . ? C19 C20 C22 121.0(5) . . ? C25 C20 C22 119.7(5) . . ? C18 C21 C24 120.2(5) . . ? C18 C21 H21 119.9 . . ? C24 C21 H21 119.9 . . ? O12 C22 O13 125.8(5) . . ? O12 C22 C20 117.6(5) . . ? O13 C22 C20 116.6(5) . . ? O16 C23 O17 125.2(5) . . ? O16 C23 C24 117.6(5) . . ? O17 C23 C24 117.1(5) . . ? C25 C24 C21 119.6(5) . . ? C25 C24 C23 119.9(5) . . ? C21 C24 C23 120.4(5) . . ? C24 C25 C20 120.2(5) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? C16 C26 C27 122.0(7) . . ? C16 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C26 C27 C13 122.9(7) . . ? C26 C27 S4 114.8(6) . 4_665 ? C13 C27 S4 122.3(5) . 4_665 ? C38 C28 C37 105.3(7) . . ? C38 C28 C39 107.1(7) . . ? C37 C28 C39 111.6(7) . . ? C38 C28 C10 110.4(7) . . ? C37 C28 C10 110.8(7) . . ? C39 C28 C10 111.3(6) . . ? C31 C29 C32 112.8(7) . . ? C31 C29 C33 103.9(7) . . ? C32 C29 C33 108.4(7) . . ? C31 C29 C4 112.5(7) . . ? C32 C29 C4 107.3(6) . . ? C33 C29 C4 112.0(7) . . ? C35 C30 C34 120.4(8) . . ? C35 C30 C16 112.2(8) . . ? C34 C30 C16 108.1(7) . . ? C35 C30 C36 98.9(8) . . ? C34 C30 C36 106.2(8) . . ? C16 C30 C36 110.2(7) . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 H34A 109.5 . . ? C30 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C30 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C30 C35 H35A 109.5 . . ? C30 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C30 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C30 C36 H36A 109.5 . . ? C30 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C30 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C28 C37 H37A 109.5 . . ? C28 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C28 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 . . ? C1 O1 Co1 132.5(4) . . ? C1 O1 Co2 133.2(4) . . ? Co1 O1 Co2 93.28(16) . . ? C7 O2 Co4 132.3(4) . . ? C7 O2 Co1 132.3(4) . . ? Co4 O2 Co1 92.91(16) . . ? C13 O3 Co3 131.4(4) . . ? C13 O3 Co3 133.3(4) . 4_665 ? Co3 O3 Co3 92.97(18) . 4_665 ? S1 O4 Co1 118.9(2) . . ? S2 O6 Co2 120.2(3) . . ? S3 O8 Co4 119.4(3) . . ? S4 O10 Co3 119.3(3) . . ? C22 O12 Co3 128.0(4) . . ? C22 O13 Co3 127.8(4) . 4_665 ? C17 O14 Co2 128.7(4) . . ? C17 O15 Co1 127.7(4) . . ? C23 O16 Co1 127.9(4) . 3_645 ? C23 O17 Co4 128.6(4) . 3_645 ? Co4 O18 Co2 138.9(3) . . ? Co4 O18 Co1 82.80(14) . 10 ? Co2 O18 Co1 83.08(14) . 10 ? Co4 O18 Co1 82.80(14) . . ? Co2 O18 Co1 83.08(14) . . ? Co1 O18 Co1 139.0(3) 10 . ? Co4 O18 H18A 110.5 . . ? Co2 O18 H18A 110.5 . . ? Co1 O18 H18A 110.5 10 . ? Co1 O18 H18A 110.5 . . ? Co3 O19 Co3 83.09(14) . 3_645 ? Co3 O19 Co3 139.4(4) . 2_755 ? Co3 O19 Co3 83.09(14) 3_645 2_755 ? Co3 O19 Co3 83.09(14) . 4_665 ? Co3 O19 Co3 139.4(4) 3_645 4_665 ? Co3 O19 Co3 83.09(14) 2_755 4_665 ? Co3 O19 H19A 110.3 . . ? Co3 O19 H19A 110.3 3_645 . ? Co3 O19 H19A 110.3 2_755 . ? Co3 O19 H19A 110.3 4_665 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.725 _refine_diff_density_min -2.179 _refine_diff_density_rms 0.131 # 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 0.000 0.000 0.000 607 154 ' ' 2 0.406 -0.024 0.013 14182 6252 ' ' 3 0.000 0.000 0.328 164 60 ' ' 4 0.000 0.000 0.500 577 261 ' ' 5 0.000 0.000 0.672 164 60 ' ' 6 0.500 0.500 0.000 578 261 ' ' 7 0.500 0.500 0.500 607 154 ' ' 8 0.500 0.500 0.172 164 60 ' ' 9 0.500 0.500 0.828 164 59 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_PLAT230 ; PROBLEM: Hirshfeld Test Diff for S4 -- C27_a .. 7.2 su RESPONSE: It is due to disorder. ; _vrf_PLAT232 ; PROBLEM: Hirshfeld Test Diff (M-X) Co3 -- O3_a .. 14.4 su RESPONSE: It is due to disorder. ; _vrf_PLAT420_dsc120105sq ; PROBLEM: D-H Without Acceptor O18 - H18A ... ? D-H Without Acceptor O19 - H19A ... ? RESPONSE: Unidentified solvents or cations may form hydrogen bonds with these hydrogens. ; #END # Attachment '- CCDC869989-revised.cif' data_2-Co-BTB _database_code_depnum_ccdc_archive 'CCDC 869989' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co24(OH)6(C40H44S4O12)6(C27H15O6)8) _chemical_melting_point ? _chemical_formula_moiety 'C456 H390 Co24 O126 S24' _chemical_formula_sum 'C456 H390 Co24 O126 S24' # Excluding the disordered counter cations and solvents. _chemical_formula_weight 10069.44 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 Tetragonal _symmetry_space_group_name_H-M 'I 4/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 34.1605(10) _cell_length_b 34.1605(10) _cell_length_c 54.943(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 64116(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7849 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 17.07 _exptl_crystal_description BLOCK _exptl_crystal_colour VIOLET _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.522 # Excluding the disordered counter cations and solvents. _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10332 _exptl_absorpt_coefficient_mu 0.370 # Excluding the disordered counter cations and solvents. _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8661 _exptl_absorpt_correction_T_max 0.9132 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 233931 _diffrn_reflns_av_R_equivalents 0.1454 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 0.70 _diffrn_reflns_theta_max 18.88 _reflns_number_total 12876 _reflns_number_gt 8145 _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. Since the data resolution is low due to the disordered solvents and cations, the constraints and restraints are applied to make the bond lengths and bond angles more meaningful. dfix 1.50 C15 c16 dfix 1.47 C15 c17 dfix 1.47 C26 c27 dfix 1.47 C26 c28 ; _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^)+(0.0998P)^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 12876 _refine_ls_number_parameters 668 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1157 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1770 _refine_ls_wR_factor_gt 0.1576 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.019 _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 0.15825(4) 0.32788(3) 0.0000 0.0668(4) Uani 1 2 d S . . Co2 Co 0.23012(3) 0.22563(3) 0.0000 0.0636(4) Uani 1 2 d S . . Co3 Co 0.53691(3) 0.44978(3) 0.234826(14) 0.0739(3) Uani 1 1 d . . . Co4 Co 0.19395(2) 0.27708(2) 0.038726(16) 0.0665(3) Uani 1 1 d . . . S1 S 0.19965(8) 0.13965(8) 0.0000 0.0630(7) Uani 1 2 d S . . S2 S 0.06770(9) 0.33030(8) 0.0000 0.0740(8) Uani 1 2 d S . . S3 S 0.13404(6) 0.23556(5) 0.07233(3) 0.0720(6) Uani 1 1 d . . . S4 S 0.56943(6) 0.40713(7) 0.28042(4) 0.0918(7) Uani 1 1 d . . . O1 O 0.13752(14) 0.28921(12) 0.02633(8) 0.0726(13) Uani 1 1 d . . . O2 O 0.18641(11) 0.21897(12) 0.02693(7) 0.0619(12) Uani 1 1 d . . . O3 O 0.55933(13) 0.49066(12) 0.25921(8) 0.0805(14) Uani 1 1 d . . . O4 O 0.10262(18) 0.35468(15) 0.0000 0.0697(17) Uani 1 2 d S . . O5 O 0.03163(19) 0.35085(18) 0.0000 0.0858(19) Uani 1 2 d S . . O6 O 0.16914(12) 0.25923(12) 0.07240(7) 0.0745(12) Uani 1 1 d . . . O7 O 0.11996(13) 0.22536(12) 0.09574(8) 0.0885(14) Uani 1 1 d . . . O8 O 0.23411(16) 0.16402(16) 0.0000 0.0647(16) Uani 1 2 d S . . O9 O 0.20588(16) 0.09847(18) 0.0000 0.0725(17) Uani 1 2 d S . . O10 O 0.63179(14) 0.17524(15) 0.02402(10) 0.0958(18) Uani 1 1 d . . . O11 O 0.66911(16) 0.20142(14) 0.05330(9) 0.0945(17) Uani 1 1 d . . . O12 O 0.24866(15) 0.26649(14) 0.05265(9) 0.0876(15) Uani 1 1 d . . . O13 O 0.27480(13) 0.22907(15) 0.02438(9) 0.0854(16) Uani 1 1 d . . . O14 O 0.51829(17) 0.40682(14) 0.21133(8) 0.0949(16) Uani 1 1 d . . . O15 O 0.57020(13) 0.40790(13) 0.25401(8) 0.0907(14) Uani 1 1 d . . . O16 O 0.59217(14) 0.37663(15) 0.29117(9) 0.1117(17) Uani 1 1 d . . . O17 O 0.45363(17) 0.41781(15) 0.21148(9) 0.0984(19) Uani 1 1 d . . . O18 O 0.5000 0.5000 0.22322(13) 0.071(2) Uani 1 4 d S . . H18D H 0.5000 0.5000 0.2059 0.106 Uiso 1 4 d SR . . O19 O 0.20832(15) 0.28704(15) 0.0000 0.0669(17) Uani 1 2 d S . . H19A H 0.2313 0.3032 0.0000 0.080 Uiso 1 2 d SR . . C1 C 0.1023(3) 0.28303(19) 0.03599(13) 0.0637(19) Uani 1 1 d . . . C2 C 0.0957(2) 0.25937(19) 0.05702(14) 0.0690(19) Uani 1 1 d . . . C3 C 0.0587(3) 0.2535(2) 0.06615(16) 0.112(3) Uani 1 1 d . . . H3 H 0.0560 0.2380 0.0799 0.135 Uiso 1 1 calc R . . C4 C 0.0268(2) 0.2688(3) 0.05644(18) 0.123(3) Uani 1 1 d . . . C5 C -0.0160(4) 0.2610(4) 0.0683(3) 0.201(5) Uiso 1 1 d . . . C6 C -0.0401(4) 0.2462(4) 0.0481(3) 0.298(8) Uiso 1 1 d . . . H6A H -0.0246 0.2452 0.0336 0.446 Uiso 1 1 calc R . . H6B H -0.0620 0.2633 0.0456 0.446 Uiso 1 1 calc R . . H6C H -0.0494 0.2204 0.0520 0.446 Uiso 1 1 calc R . . C7 C -0.0323(4) 0.2998(4) 0.0740(3) 0.280(7) Uiso 1 1 d . . . H7A H -0.0248 0.3181 0.0616 0.420 Uiso 1 1 calc R . . H7B H -0.0225 0.3086 0.0894 0.420 Uiso 1 1 calc R . . H7C H -0.0604 0.2982 0.0747 0.420 Uiso 1 1 calc R . . C8 C -0.0126(4) 0.2381(4) 0.0908(2) 0.254(6) Uiso 1 1 d . . . H8A H 0.0042 0.2516 0.1020 0.381 Uiso 1 1 calc R . . H8B H -0.0018 0.2129 0.0872 0.381 Uiso 1 1 calc R . . H8C H -0.0380 0.2350 0.0980 0.381 Uiso 1 1 calc R . . C9 C 0.16740(19) 0.1878(2) 0.03568(13) 0.0600(19) Uani 1 1 d . . . C10 C 0.16985(19) 0.1499(3) 0.02542(11) 0.0667(19) Uani 1 1 d . . . C11 C 0.1492(2) 0.1187(2) 0.03434(15) 0.094(3) Uani 1 1 d . . . H11 H 0.1510 0.0944 0.0268 0.113 Uiso 1 1 calc R . . C12 C 0.1262(3) 0.1233(3) 0.05408(18) 0.107(3) Uani 1 1 d . . . C13 C 0.1230(2) 0.1603(3) 0.06417(13) 0.089(2) Uani 1 1 d . . . H13 H 0.1061 0.1634 0.0773 0.106 Uiso 1 1 calc R . . C14 C 0.1425(2) 0.1917(2) 0.05623(13) 0.0640(19) Uani 1 1 d . . . C15 C 0.1021(4) 0.0877(4) 0.0643(2) 0.193(5) Uiso 1 1 d D . . C16 C 0.1155(4) 0.0509(4) 0.0584(2) 0.257(6) Uiso 1 1 d D . . H16A H 0.1123 0.0465 0.0413 0.386 Uiso 1 1 calc R . . H16B H 0.1009 0.0316 0.0673 0.386 Uiso 1 1 calc R . . H16C H 0.1427 0.0489 0.0626 0.386 Uiso 1 1 calc R . . C17 C 0.1188(5) 0.0811(5) 0.0904(3) 0.341(9) Uiso 1 1 d D . . H17A H 0.1385 0.0611 0.0899 0.512 Uiso 1 1 calc R . . H17B H 0.0981 0.0733 0.1011 0.512 Uiso 1 1 calc R . . H17C H 0.1302 0.1051 0.0962 0.512 Uiso 1 1 calc R . . C18 C 0.0626(4) 0.0969(4) 0.0717(3) 0.286(7) Uiso 1 1 d . . . H18A H 0.0446 0.0898 0.0590 0.429 Uiso 1 1 calc R . . H18B H 0.0605 0.1245 0.0748 0.429 Uiso 1 1 calc R . . H18C H 0.0563 0.0827 0.0863 0.429 Uiso 1 1 calc R . . C19 C 0.0673(3) 0.29991(18) 0.02603(12) 0.071(2) Uani 1 1 d . . . C20 C 0.0310(2) 0.2930(2) 0.03640(15) 0.099(3) Uani 1 1 d . . . H20 H 0.0090 0.3049 0.0298 0.119 Uiso 1 1 calc R . . C21 C 0.5797(2) 0.4874(3) 0.27943(14) 0.078(2) Uani 1 1 d . . . C22 C 0.5874(2) 0.4519(2) 0.29124(16) 0.078(2) Uani 1 1 d . . . C23 C 0.6092(3) 0.4507(3) 0.31154(18) 0.122(3) Uani 1 1 d . . . H23 H 0.6133 0.4262 0.3184 0.146 Uiso 1 1 calc R . . C24 C 0.6254(3) 0.4805(4) 0.32262(15) 0.132(4) Uani 1 1 d . . . C25 C 0.6203(3) 0.5176(3) 0.31211(16) 0.114(3) Uani 1 1 d . . . H25 H 0.6319 0.5397 0.3188 0.137 Uiso 1 1 calc R . . C26 C 0.6555(4) 0.4823(4) 0.3470(2) 0.194(5) Uiso 1 1 d D . . C27 C 0.6945(5) 0.4894(5) 0.3402(3) 0.337(9) Uiso 1 1 d D . . H27A H 0.6954 0.5107 0.3288 0.506 Uiso 1 1 calc R . . H27B H 0.7052 0.4663 0.3328 0.506 Uiso 1 1 calc R . . H27C H 0.7096 0.4960 0.3544 0.506 Uiso 1 1 calc R . . C28 C 0.6292(4) 0.4923(4) 0.3655(3) 0.299(8) Uiso 1 1 d D . . H28A H 0.6035 0.4829 0.3614 0.448 Uiso 1 1 calc R . . H28B H 0.6285 0.5202 0.3673 0.448 Uiso 1 1 calc R . . H28C H 0.6374 0.4805 0.3805 0.448 Uiso 1 1 calc R . . C29 C 0.6582(4) 0.4395(4) 0.3538(2) 0.243(6) Uiso 1 1 d . . . H29A H 0.6669 0.4247 0.3400 0.364 Uiso 1 1 calc R . . H29B H 0.6329 0.4303 0.3588 0.364 Uiso 1 1 calc R . . H29C H 0.6765 0.4364 0.3669 0.364 Uiso 1 1 calc R . . C30 C 0.5971(2) 0.5201(3) 0.29107(14) 0.088(2) Uani 1 1 d . . . C31 C 0.6373(2) 0.1943(2) 0.04336(17) 0.077(2) Uani 1 1 d . . . C32 C 0.6017(2) 0.2109(2) 0.05613(15) 0.088(2) Uani 1 1 d . . . C33 C 0.6012(3) 0.2311(4) 0.0761(2) 0.225(7) Uani 1 1 d . . . H33 H 0.6249 0.2365 0.0837 0.270 Uiso 1 1 calc R . . C34 C 0.5646(4) 0.2076(3) 0.0478(2) 0.194(5) Uiso 1 1 d . . . H34 H 0.5613 0.1961 0.0326 0.232 Uiso 1 1 calc R . . C35 C 0.2772(2) 0.2489(2) 0.04268(16) 0.072(2) Uani 1 1 d . . . C36 C 0.3147(3) 0.2538(2) 0.05569(15) 0.079(2) Uani 1 1 d . . . C37 C 0.3470(3) 0.2361(4) 0.04788(17) 0.198(6) Uani 1 1 d . . . H37 H 0.3458 0.2199 0.0343 0.238 Uiso 1 1 calc R . . C38 C 0.3819(3) 0.2414(4) 0.0595(2) 0.184(5) Uani 1 1 d . . . H38 H 0.4032 0.2275 0.0535 0.220 Uiso 1 1 calc R . . C39 C 0.3884(2) 0.2639(3) 0.07820(15) 0.095(3) Uani 1 1 d . . . C40 C 0.3562(4) 0.2811(4) 0.0843(2) 0.243(8) Uani 1 1 d . . . H40 H 0.3574 0.2984 0.0973 0.292 Uiso 1 1 calc R . . C41 C 0.3201(3) 0.2763(4) 0.0734(2) 0.244(8) Uani 1 1 d . . . H41 H 0.2988 0.2903 0.0794 0.292 Uiso 1 1 calc R . . C42 C 0.4271(2) 0.2689(3) 0.08917(16) 0.097(3) Uani 1 1 d . . . C43 C 0.4607(3) 0.2520(2) 0.08018(14) 0.109(3) Uani 1 1 d . . . H43 H 0.4580 0.2349 0.0671 0.131 Uiso 1 1 calc R . . C44 C 0.4982(2) 0.2581(2) 0.08883(15) 0.098(3) Uani 1 1 d . . . C45 C 0.5005(3) 0.2816(3) 0.10989(17) 0.113(3) Uani 1 1 d . . . H45 H 0.5250 0.2864 0.1166 0.135 Uiso 1 1 calc R . . C46 C 0.4681(3) 0.2978(2) 0.12096(15) 0.095(3) Uani 1 1 d . . . C47 C 0.4322(3) 0.2918(2) 0.11032(17) 0.106(3) Uani 1 1 d . . . H47 H 0.4103 0.3034 0.1173 0.128 Uiso 1 1 calc R . . C48 C 0.5330(3) 0.2414(3) 0.07822(15) 0.108(3) Uani 1 1 d . . . C49 C 0.5313(3) 0.2197(4) 0.0596(2) 0.269(9) Uani 1 1 d . . . H49 H 0.5070 0.2119 0.0537 0.323 Uiso 1 1 calc R . . C50 C 0.5673(3) 0.2450(3) 0.08650(19) 0.209(6) Uani 1 1 d . . . H50 H 0.5700 0.2585 0.1011 0.251 Uiso 1 1 calc R . . C51 C 0.4712(3) 0.3235(3) 0.14190(16) 0.104(3) Uani 1 1 d . . . C52 C 0.5048(3) 0.3304(4) 0.1531(2) 0.236(7) Uani 1 1 d . . . H52 H 0.5264 0.3166 0.1475 0.283 Uiso 1 1 calc R . . C53 C 0.5111(3) 0.3556(4) 0.1723(2) 0.233(7) Uani 1 1 d . . . H53 H 0.5364 0.3599 0.1779 0.280 Uiso 1 1 calc R . . C54 C 0.4807(3) 0.3742(2) 0.18271(14) 0.083(2) Uani 1 1 d . . . C55 C 0.4471(3) 0.3688(4) 0.1708(2) 0.201(6) Uani 1 1 d . . . H55 H 0.4256 0.3845 0.1745 0.241 Uiso 1 1 calc R . . C56 C 0.4435(3) 0.3393(4) 0.1524(2) 0.216(7) Uani 1 1 d . . . H56 H 0.4184 0.3314 0.1481 0.259 Uiso 1 1 calc R . . C57 C 0.4833(3) 0.4017(2) 0.20347(14) 0.079(2) 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 0.0677(9) 0.0652(9) 0.0674(9) 0.000 0.000 -0.0164(7) Co2 0.0587(9) 0.0677(9) 0.0644(9) 0.000 0.000 -0.0115(7) Co3 0.0885(7) 0.0921(8) 0.0411(6) 0.0015(5) 0.0007(5) -0.0063(6) Co4 0.0602(7) 0.0636(7) 0.0756(7) -0.0043(5) -0.0041(5) -0.0076(5) S1 0.069(2) 0.058(2) 0.0624(18) 0.000 0.000 -0.0018(16) S2 0.075(2) 0.068(2) 0.079(2) 0.000 0.000 0.0121(19) S3 0.0832(16) 0.0734(14) 0.0593(13) 0.0003(11) 0.0038(12) 0.0027(12) S4 0.1059(19) 0.1001(18) 0.0694(16) 0.0108(13) -0.0095(14) 0.0097(14) O1 0.065(3) 0.077(3) 0.076(3) 0.008(2) 0.003(3) -0.008(3) O2 0.058(3) 0.063(3) 0.064(3) -0.007(2) 0.010(2) 0.002(2) O3 0.112(4) 0.099(4) 0.030(3) 0.000(3) -0.012(3) -0.003(3) O4 0.093(5) 0.053(4) 0.063(4) 0.000 0.000 -0.022(4) O5 0.078(5) 0.086(5) 0.094(5) 0.000 0.000 0.021(4) O6 0.071(3) 0.075(3) 0.078(3) -0.011(2) -0.010(3) 0.000(3) O7 0.110(4) 0.099(4) 0.056(3) 0.006(3) 0.018(3) 0.005(3) O8 0.047(4) 0.072(4) 0.075(4) 0.000 0.000 0.002(4) O9 0.073(4) 0.062(5) 0.083(5) 0.000 0.000 0.000(4) O10 0.086(4) 0.126(5) 0.076(4) -0.031(3) 0.008(3) 0.021(3) O11 0.067(4) 0.111(4) 0.105(4) -0.014(3) 0.011(3) -0.001(3) O12 0.068(4) 0.096(4) 0.099(4) -0.014(3) -0.019(3) -0.007(3) O13 0.072(4) 0.113(4) 0.071(4) -0.016(3) -0.016(3) -0.005(3) O14 0.097(4) 0.118(4) 0.070(3) -0.027(3) 0.002(3) -0.011(3) O15 0.111(4) 0.104(4) 0.058(3) 0.005(3) -0.005(3) 0.020(3) O16 0.115(4) 0.121(4) 0.099(4) 0.009(3) -0.020(3) 0.033(4) O17 0.114(5) 0.107(4) 0.075(4) -0.030(3) 0.000(3) 0.016(4) O18 0.074(4) 0.074(4) 0.063(5) 0.000 0.000 0.000 O19 0.064(4) 0.058(4) 0.078(4) 0.000 0.000 -0.014(3) C1 0.086(7) 0.046(5) 0.059(6) -0.011(4) -0.002(5) 0.002(5) C2 0.069(6) 0.059(5) 0.080(6) -0.001(5) -0.010(5) -0.002(4) C3 0.055(6) 0.128(8) 0.154(8) 0.028(6) 0.024(7) 0.009(6) C4 0.037(6) 0.187(9) 0.143(8) 0.074(7) 0.032(6) 0.008(6) C9 0.039(5) 0.084(7) 0.057(5) 0.017(5) -0.004(4) -0.007(4) C10 0.076(5) 0.055(5) 0.069(5) -0.006(5) 0.019(4) -0.001(5) C11 0.098(6) 0.101(7) 0.084(6) 0.015(5) 0.037(5) -0.034(5) C12 0.128(7) 0.062(7) 0.131(8) 0.036(6) 0.044(6) -0.052(5) C13 0.102(6) 0.050(6) 0.115(6) 0.006(6) 0.033(5) -0.019(5) C14 0.063(5) 0.052(6) 0.076(6) 0.011(4) 0.001(4) -0.001(4) C19 0.064(6) 0.064(5) 0.085(5) -0.002(4) 0.002(5) 0.007(5) C20 0.057(6) 0.145(8) 0.094(7) 0.031(6) 0.021(5) 0.004(5) C21 0.109(7) 0.083(7) 0.041(5) -0.007(6) 0.012(5) -0.013(6) C22 0.097(6) 0.090(7) 0.048(5) 0.009(5) -0.017(5) -0.007(5) C23 0.174(9) 0.128(9) 0.063(7) 0.011(6) -0.035(7) -0.016(7) C24 0.167(9) 0.167(11) 0.062(6) 0.027(8) -0.084(6) 0.007(8) C25 0.154(8) 0.123(9) 0.066(6) -0.008(6) -0.036(6) 0.002(6) C30 0.112(6) 0.107(8) 0.044(5) 0.008(5) -0.021(5) 0.012(5) C31 0.061(6) 0.079(6) 0.090(7) 0.019(5) 0.035(6) 0.014(6) C32 0.059(6) 0.104(6) 0.103(6) -0.035(5) -0.010(5) 0.017(5) C33 0.074(8) 0.354(16) 0.245(12) -0.249(13) -0.034(8) 0.035(8) C35 0.055(7) 0.084(6) 0.077(6) -0.005(5) 0.001(6) 0.008(5) C36 0.062(7) 0.102(7) 0.073(6) -0.022(5) -0.006(6) -0.009(5) C37 0.067(7) 0.363(16) 0.165(10) -0.190(10) -0.027(7) 0.037(9) C38 0.046(7) 0.332(15) 0.174(10) -0.138(11) -0.024(7) 0.025(7) C39 0.048(7) 0.162(8) 0.076(6) -0.070(5) -0.013(5) 0.016(6) C40 0.089(9) 0.411(19) 0.230(13) -0.239(13) -0.038(9) 0.053(11) C41 0.053(7) 0.385(18) 0.293(14) -0.247(15) -0.104(8) 0.077(8) C42 0.043(7) 0.144(8) 0.103(7) -0.043(6) -0.001(6) 0.008(6) C43 0.042(6) 0.157(8) 0.128(7) -0.074(6) -0.007(6) 0.020(6) C44 0.042(7) 0.151(8) 0.101(7) -0.061(6) -0.014(5) 0.024(5) C45 0.075(7) 0.162(8) 0.101(7) -0.063(6) -0.027(6) 0.009(6) C46 0.044(6) 0.151(8) 0.090(6) -0.067(6) -0.008(6) 0.018(6) C47 0.069(7) 0.138(7) 0.112(7) -0.074(6) 0.003(6) -0.002(5) C48 0.045(7) 0.198(10) 0.081(6) -0.062(6) -0.012(6) 0.018(6) C49 0.053(7) 0.53(2) 0.230(13) -0.260(16) 0.001(8) 0.037(9) C50 0.050(7) 0.360(16) 0.217(11) -0.210(11) -0.009(8) 0.069(8) C51 0.046(6) 0.164(8) 0.102(7) -0.073(7) -0.020(6) 0.015(6) C52 0.086(9) 0.394(18) 0.229(12) -0.246(13) -0.034(8) 0.061(9) C53 0.071(8) 0.418(19) 0.210(12) -0.238(13) -0.025(7) 0.025(9) C54 0.074(7) 0.118(7) 0.056(5) -0.013(5) -0.010(6) 0.005(6) C55 0.087(8) 0.308(15) 0.207(12) -0.164(11) -0.034(8) 0.051(8) C56 0.096(9) 0.361(17) 0.189(11) -0.223(12) -0.064(8) 0.073(9) C57 0.102(9) 0.095(7) 0.040(6) 0.005(5) -0.009(6) -0.018(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 O10 1.994(5) 4_565 ? Co1 O10 1.994(5) 11_565 ? Co1 O1 2.083(4) 10 ? Co1 O1 2.083(4) . ? Co1 O4 2.109(6) . ? Co1 O19 2.208(5) . ? Co2 O13 2.034(5) 10 ? Co2 O13 2.034(5) . ? Co2 O8 2.109(6) . ? Co2 O2 2.114(4) 10 ? Co2 O2 2.114(4) . ? Co2 O19 2.226(5) . ? Co3 O17 2.014(5) 3_655 ? Co3 O14 2.055(5) . ? Co3 O3 2.081(4) . ? Co3 O3 2.095(4) 4_565 ? Co3 O15 2.110(4) . ? Co3 O18 2.222(2) . ? Co4 O11 2.021(5) 4_565 ? Co4 O12 2.052(5) . ? Co4 O1 2.086(5) . ? Co4 O2 2.104(4) . ? Co4 O6 2.124(4) . ? Co4 O19 2.2099(16) . ? S1 O9 1.423(6) . ? S1 O8 1.442(5) . ? S1 C10 1.764(6) 10 ? S1 C10 1.764(6) . ? S2 O5 1.418(6) . ? S2 O4 1.455(6) . ? S2 C19 1.767(7) . ? S2 C19 1.768(7) 10 ? S3 O7 1.417(4) . ? S3 O6 1.446(4) . ? S3 C2 1.755(7) . ? S3 C14 1.764(6) . ? S4 O16 1.427(5) . ? S4 O15 1.451(4) . ? S4 C22 1.751(7) . ? S4 C30 1.790(8) 4_565 ? O1 C1 1.331(7) . ? O2 C9 1.337(7) . ? O3 C21 1.317(8) . ? O3 Co3 2.095(4) 3_655 ? O10 C31 1.259(9) . ? O10 Co1 1.994(5) 3_655 ? O11 C31 1.241(8) . ? O11 Co4 2.021(5) 3_655 ? O12 C35 1.271(7) . ? O13 C35 1.214(8) . ? O14 C57 1.283(8) . ? O17 C57 1.234(8) . ? O17 Co3 2.014(5) 4_565 ? O18 Co3 2.222(2) 2_665 ? O18 Co3 2.222(2) 3_655 ? O18 Co3 2.222(2) 4_565 ? O18 H18D 0.9500 . ? O19 Co4 2.2100(16) 10 ? O19 H19A 0.9601 . ? C1 C2 1.428(8) . ? C1 C19 1.436(8) . ? C2 C3 1.375(9) . ? C3 C4 1.322(9) . ? C3 H3 0.9300 . ? C4 C20 1.385(9) . ? C4 C5 1.626(14) . ? C5 C8 1.466(14) . ? C5 C6 1.472(15) . ? C5 C7 1.472(15) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.414(8) . ? C9 C14 1.419(8) . ? C10 C11 1.370(8) . ? C11 C12 1.348(9) . ? C11 H11 0.9300 . ? C12 C13 1.383(9) . ? C12 C15 1.573(13) . ? C13 C14 1.338(8) . ? C13 H13 0.9300 . ? C15 C16 1.376(12) . ? C15 C18 1.446(15) . ? C15 C17 1.561(13) . ? 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 C20 1.384(8) . ? C20 H20 0.9300 . ? C21 C22 1.400(9) . ? C21 C30 1.417(9) . ? C22 C23 1.343(10) . ? C23 C24 1.307(10) . ? C23 H23 0.9300 . ? C24 C25 1.404(10) . ? C24 C26 1.692(14) . ? C25 C30 1.403(9) . ? C25 H25 0.9300 . ? C26 C28 1.401(12) . ? C26 C27 1.404(13) . ? C26 C29 1.511(14) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 S4 1.790(8) 3_655 ? C31 C32 1.513(9) . ? C32 C33 1.294(9) . ? C32 C34 1.354(12) . ? C33 C50 1.377(10) . ? C33 H33 0.9300 . ? C34 C49 1.373(13) . ? C34 H34 0.9300 . ? C35 C36 1.475(10) . ? C36 C41 1.254(10) . ? C36 C37 1.329(10) . ? C37 C38 1.367(10) . ? C37 H37 0.9300 . ? C38 C39 1.300(10) . ? C38 H38 0.9300 . ? C39 C40 1.294(10) . ? C39 C42 1.463(9) . ? C40 C41 1.381(11) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.377(8) . ? C42 C47 1.412(9) . ? C43 C44 1.381(9) . ? C43 H43 0.9300 . ? C44 C45 1.411(9) . ? C44 C48 1.441(9) . ? C45 C46 1.378(9) . ? C45 H45 0.9300 . ? C46 C47 1.374(9) . ? C46 C51 1.453(10) . ? C47 H47 0.9300 . ? C48 C50 1.265(9) . ? C48 C49 1.265(10) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C56 1.232(10) . ? C51 C52 1.323(10) . ? C52 C53 1.377(11) . ? C52 H52 0.9300 . ? C53 C54 1.346(10) . ? C53 H53 0.9300 . ? C54 C55 1.334(10) . ? C54 C57 1.481(10) . ? C55 C56 1.431(11) . ? C55 H55 0.9300 . ? C56 H56 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 O10 Co1 O10 82.9(3) 4_565 11_565 ? O10 Co1 O1 175.3(2) 4_565 10 ? O10 Co1 O1 94.44(18) 11_565 10 ? O10 Co1 O1 94.44(18) 4_565 . ? O10 Co1 O1 175.3(2) 11_565 . ? O1 Co1 O1 88.0(2) 10 . ? O10 Co1 O4 87.85(19) 4_565 . ? O10 Co1 O4 87.85(19) 11_565 . ? O1 Co1 O4 88.22(17) 10 . ? O1 Co1 O4 88.22(17) . . ? O10 Co1 O19 102.19(18) 4_565 . ? O10 Co1 O19 102.19(18) 11_565 . ? O1 Co1 O19 82.10(16) 10 . ? O1 Co1 O19 82.10(16) . . ? O4 Co1 O19 166.5(2) . . ? O13 Co2 O13 82.4(3) 10 . ? O13 Co2 O8 90.52(18) 10 . ? O13 Co2 O8 90.52(18) . . ? O13 Co2 O2 94.32(17) 10 10 ? O13 Co2 O2 175.51(19) . 10 ? O8 Co2 O2 86.47(16) . 10 ? O13 Co2 O2 175.50(19) 10 . ? O13 Co2 O2 94.32(17) . . ? O8 Co2 O2 86.47(16) . . ? O2 Co2 O2 88.8(2) 10 . ? O13 Co2 O19 101.34(18) 10 . ? O13 Co2 O19 101.34(18) . . ? O8 Co2 O19 164.2(2) . . ? O2 Co2 O19 82.25(15) 10 . ? O2 Co2 O19 82.25(15) . . ? O17 Co3 O14 83.35(19) 3_655 . ? O17 Co3 O3 94.79(19) 3_655 . ? O14 Co3 O3 175.7(2) . . ? O17 Co3 O3 175.2(2) 3_655 4_565 ? O14 Co3 O3 93.56(18) . 4_565 ? O3 Co3 O3 88.0(2) . 4_565 ? O17 Co3 O15 87.0(2) 3_655 . ? O14 Co3 O15 89.79(19) . . ? O3 Co3 O15 86.27(17) . . ? O3 Co3 O15 89.22(17) 4_565 . ? O17 Co3 O18 101.7(2) 3_655 . ? O14 Co3 O18 101.3(2) . . ? O3 Co3 O18 82.85(19) . . ? O3 Co3 O18 82.54(18) 4_565 . ? O15 Co3 O18 166.5(2) . . ? O11 Co4 O12 84.1(2) 4_565 . ? O11 Co4 O1 93.75(18) 4_565 . ? O12 Co4 O1 177.0(2) . . ? O11 Co4 O2 174.6(2) 4_565 . ? O12 Co4 O2 93.44(17) . . ? O1 Co4 O2 88.49(15) . . ? O11 Co4 O6 88.07(19) 4_565 . ? O12 Co4 O6 89.32(18) . . ? O1 Co4 O6 88.43(17) . . ? O2 Co4 O6 87.05(16) . . ? O11 Co4 O19 102.3(2) 4_565 . ? O12 Co4 O19 100.6(2) . . ? O1 Co4 O19 81.97(18) . . ? O2 Co4 O19 82.86(17) . . ? O6 Co4 O19 166.22(17) . . ? O9 S1 O8 116.6(4) . . ? O9 S1 C10 106.4(3) . 10 ? O8 S1 C10 110.9(3) . 10 ? O9 S1 C10 106.4(3) . . ? O8 S1 C10 110.9(3) . . ? C10 S1 C10 104.7(4) 10 . ? O5 S2 O4 115.4(4) . . ? O5 S2 C19 106.5(3) . . ? O4 S2 C19 110.0(3) . . ? O5 S2 C19 106.5(3) . 10 ? O4 S2 C19 110.0(3) . 10 ? C19 S2 C19 108.0(4) . 10 ? O7 S3 O6 114.6(3) . . ? O7 S3 C2 107.2(4) . . ? O6 S3 C2 111.1(3) . . ? O7 S3 C14 107.6(3) . . ? O6 S3 C14 109.9(3) . . ? C2 S3 C14 106.0(3) . . ? O16 S4 O15 114.7(3) . . ? O16 S4 C22 107.9(4) . . ? O15 S4 C22 108.5(4) . . ? O16 S4 C30 108.5(4) . 4_565 ? O15 S4 C30 110.2(4) . 4_565 ? C22 S4 C30 106.8(3) . 4_565 ? C1 O1 Co1 133.2(4) . . ? C1 O1 Co4 132.3(4) . . ? Co1 O1 Co4 92.21(19) . . ? C9 O2 Co4 134.4(4) . . ? C9 O2 Co2 132.9(4) . . ? Co4 O2 Co2 91.58(19) . . ? C21 O3 Co3 133.0(5) . . ? C21 O3 Co3 133.0(5) . 3_655 ? Co3 O3 Co3 92.28(18) . 3_655 ? S2 O4 Co1 119.4(3) . . ? S3 O6 Co4 119.3(2) . . ? S1 O8 Co2 121.5(3) . . ? C31 O10 Co1 127.3(5) . 3_655 ? C31 O11 Co4 126.7(5) . 3_655 ? C35 O12 Co4 128.5(5) . . ? C35 O13 Co2 129.0(5) . . ? C57 O14 Co3 126.6(5) . . ? S4 O15 Co3 120.1(3) . . ? C57 O17 Co3 128.5(6) . 4_565 ? Co3 O18 Co3 85.28(10) 2_665 3_655 ? Co3 O18 Co3 146.7(4) 2_665 . ? Co3 O18 Co3 85.28(10) 3_655 . ? Co3 O18 Co3 85.28(10) 2_665 4_565 ? Co3 O18 Co3 146.7(4) 3_655 4_565 ? Co3 O18 Co3 85.28(10) . 4_565 ? Co3 O18 H18D 106.7 2_665 . ? Co3 O18 H18D 106.7 3_655 . ? Co3 O18 H18D 106.7 . . ? Co3 O18 H18D 106.7 4_565 . ? Co1 O19 Co4 85.71(14) . . ? Co1 O19 Co4 85.71(14) . 10 ? Co4 O19 Co4 148.7(3) . 10 ? Co1 O19 Co2 148.7(3) . . ? Co4 O19 Co2 85.95(13) . . ? Co4 O19 Co2 85.94(13) 10 . ? Co1 O19 H19A 105.6 . . ? Co4 O19 H19A 105.7 . . ? Co4 O19 H19A 105.7 10 . ? Co2 O19 H19A 105.7 . . ? O1 C1 C2 123.7(7) . . ? O1 C1 C19 122.5(7) . . ? C2 C1 C19 113.9(7) . . ? C3 C2 C1 121.5(7) . . ? C3 C2 S3 116.3(7) . . ? C1 C2 S3 122.2(7) . . ? C4 C3 C2 123.6(8) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C4 C20 118.1(7) . . ? C3 C4 C5 121.0(10) . . ? C20 C4 C5 120.8(9) . . ? C8 C5 C6 119.8(13) . . ? C8 C5 C7 109.5(13) . . ? C6 C5 C7 104.9(13) . . ? C8 C5 C4 110.8(11) . . ? C6 C5 C4 104.8(11) . . ? C7 C5 C4 106.1(11) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C10 123.8(7) . . ? O2 C9 C14 120.2(7) . . ? C10 C9 C14 116.0(6) . . ? C11 C10 C9 122.7(6) . . ? C11 C10 S1 115.2(7) . . ? C9 C10 S1 122.1(6) . . ? C12 C11 C10 119.7(7) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 118.4(6) . . ? C11 C12 C15 120.1(10) . . ? C13 C12 C15 121.4(10) . . ? C14 C13 C12 124.2(7) . . ? C14 C13 H13 117.9 . . ? C12 C13 H13 117.9 . . ? C13 C14 C9 118.9(6) . . ? C13 C14 S3 115.9(7) . . ? C9 C14 S3 125.2(7) . . ? C16 C15 C18 125.3(14) . . ? C16 C15 C17 87.8(11) . . ? C18 C15 C17 96.5(11) . . ? C16 C15 C12 116.6(12) . . ? C18 C15 C12 114.9(12) . . ? C17 C15 C12 104.2(11) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C1 121.4(7) . . ? C20 C19 S2 116.1(7) . . ? C1 C19 S2 122.5(6) . . ? C19 C20 C4 121.4(7) . . ? C19 C20 H20 119.3 . . ? C4 C20 H20 119.3 . . ? O3 C21 C22 124.2(8) . . ? O3 C21 C30 122.4(8) . . ? C22 C21 C30 113.3(7) . . ? C23 C22 C21 120.9(7) . . ? C23 C22 S4 116.7(8) . . ? C21 C22 S4 122.3(7) . . ? C24 C23 C22 126.7(9) . . ? C24 C23 H23 116.6 . . ? C22 C23 H23 116.6 . . ? C23 C24 C25 117.3(8) . . ? C23 C24 C26 130.9(12) . . ? C25 C24 C26 111.6(11) . . ? C24 C25 C30 117.7(8) . . ? C24 C25 H25 121.2 . . ? C30 C25 H25 121.2 . . ? C28 C26 C27 139.6(15) . . ? C28 C26 C29 95.4(11) . . ? C27 C26 C29 100.1(12) . . ? C28 C26 C24 101.1(11) . . ? C27 C26 C24 111.9(12) . . ? C29 C26 C24 101.3(10) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 C21 124.0(7) . . ? C25 C30 S4 111.9(8) . 3_655 ? C21 C30 S4 124.1(7) . 3_655 ? O11 C31 O10 127.1(7) . . ? O11 C31 C32 115.1(8) . . ? O10 C31 C32 117.8(8) . . ? C33 C32 C34 108.6(9) . . ? C33 C32 C31 127.1(8) . . ? C34 C32 C31 124.3(10) . . ? C32 C33 C50 123.2(8) . . ? C32 C33 H33 118.4 . . ? C50 C33 H33 118.4 . . ? C32 C34 C49 126.2(11) . . ? C32 C34 H34 116.9 . . ? C49 C34 H34 116.9 . . ? O13 C35 O12 124.6(8) . . ? O13 C35 C36 121.6(7) . . ? O12 C35 C36 113.8(8) . . ? C41 C36 C37 114.0(8) . . ? C41 C36 C35 125.0(9) . . ? C37 C36 C35 120.8(9) . . ? C36 C37 C38 120.9(8) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C39 C38 C37 126.7(9) . . ? C39 C38 H38 116.7 . . ? C37 C38 H38 116.7 . . ? C40 C39 C38 109.1(8) . . ? C40 C39 C42 127.6(9) . . ? C38 C39 C42 123.2(9) . . ? C39 C40 C41 126.4(9) . . ? C39 C40 H40 116.8 . . ? C41 C40 H40 116.8 . . ? C36 C41 C40 122.8(9) . . ? C36 C41 H41 118.6 . . ? C40 C41 H41 118.6 . . ? C43 C42 C47 115.2(7) . . ? C43 C42 C39 123.8(9) . . ? C47 C42 C39 121.0(8) . . ? C42 C43 C44 125.9(7) . . ? C42 C43 H43 117.1 . . ? C44 C43 H43 117.1 . . ? C43 C44 C45 114.8(7) . . ? C43 C44 C48 124.4(8) . . ? C45 C44 C48 120.7(8) . . ? C46 C45 C44 123.0(7) . . ? C46 C45 H45 118.5 . . ? C44 C45 H45 118.5 . . ? C47 C46 C45 118.1(7) . . ? C47 C46 C51 119.3(8) . . ? C45 C46 C51 122.3(8) . . ? C46 C47 C42 122.7(7) . . ? C46 C47 H47 118.6 . . ? C42 C47 H47 118.6 . . ? C50 C48 C49 113.0(9) . . ? C50 C48 C44 125.5(9) . . ? C49 C48 C44 121.4(9) . . ? C48 C49 C34 121.4(10) . . ? C48 C49 H49 119.3 . . ? C34 C49 H49 119.3 . . ? C48 C50 C33 126.6(9) . . ? C48 C50 H50 116.7 . . ? C33 C50 H50 116.7 . . ? C56 C51 C52 111.7(9) . . ? C56 C51 C46 125.6(9) . . ? C52 C51 C46 122.6(9) . . ? C51 C52 C53 127.1(9) . . ? C51 C52 H52 116.5 . . ? C53 C52 H52 116.5 . . ? C54 C53 C52 119.9(8) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C55 C54 C53 113.0(8) . . ? C55 C54 C57 121.1(9) . . ? C53 C54 C57 125.5(9) . . ? C54 C55 C56 121.1(9) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C51 C56 C55 125.0(9) . . ? C51 C56 H56 117.5 . . ? C55 C56 H56 117.5 . . ? O17 C57 O14 125.8(8) . . ? O17 C57 C54 120.6(8) . . ? O14 C57 C54 113.7(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 18.88 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.533 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.040 # 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 0.000 0.000 0.000 1226 337 ' ' 2 0.449 -0.003 -0.002 45169 15966 ' ' 3 0.500 0.500 0.500 1225 337 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_THETM01 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4553 RESPONSE: It is due to disorder of the solvents and the counter cations, which could not be defined from the DF maps. ; _vrf_PLAT023 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 18.88 Deg RESPONSE: It is due to disorder of the solvents and the counter cations, which could not be defined from the DF maps. ; _vrf_PLAT201 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 13. RESPONSE: Tert-butyl groups are refined isotropically. ; _vrf_PLAT213 ; PROBLEM: Atom C41 has ADP max/min Ratio ..... 6.9 prola Atom C12 has ADP max/min Ratio ..... 4.2 oblat Atom C24 has ADP max/min Ratio ..... 4.5 oblat Atom C50 has ADP max/min Ratio ..... 5.2 prola RESPONSE: It is due to disorder. ; _vrf_PLAT241 ; PROBLEM: Check High Ueq as Compared to Neighbors for C33 Check High Ueq as Compared to Neighbors for C37 Check High Ueq as Compared to Neighbors for C40 Check High Ueq as Compared to Neighbors for C41 Check High Ueq as Compared to Neighbors for C49 Check High Ueq as Compared to Neighbors for C52 Check High Ueq as Compared to Neighbors for C53 Check High Ueq as Compared to Neighbors for C55 Check High Ueq as Compared to Neighbors for C56 Check High Ueq as Compared to Neighbors for C38 Check High Ueq as Compared to Neighbors for C50 RESPONSE: It is due to disorder. ; _vrf_PLAT412 ; PROBLEM: Short Intra XH3 .. XHn H16C .. H17A .. 1.56 Ang. Short Intra XH3 .. XHn H17B .. H18C .. 1.67 Ang. RESPONSE: It is due to disorder. ; _vrf_PLAT220 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.7 Ratio RESPONSE: It is due to disorder. ; _vrf_PLAT242 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C15 Check Low Ueq as Compared to Neighbors for C26 Check Low Ueq as Compared to Neighbors for C32 Check Low Ueq as Compared to Neighbors for C36 Check Low Ueq as Compared to Neighbors for C39 Check Low Ueq as Compared to Neighbors for C48 Check Low Ueq as Compared to Neighbors for C51 Check Low Ueq as Compared to Neighbors for C54 RESPONSE: It is due to disorder. ; _vrf_PLAT420_dsc120105sq ; PROBLEM: D-H Without Acceptor O18 - H18D ... ? D-H Without Acceptor O19 - H19A ... ? RESPONSE: Unidentified solvents or cations may form hydrogen bonds with these hydrogens. ; #END # Attachment '- CCDC869990-revised.cif' data_3-Co-BTE _database_code_depnum_ccdc_archive 'CCDC 869990' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co24(OH)6(C40H44S4O12)6(C33H15O6)8) _chemical_melting_point ? _chemical_formula_moiety 'C504 H390 Co24 O126 S24' _chemical_formula_sum 'C504 H390 Co24 O126 S24' # Unidentified solvents and cations are not included in the calculation. _chemical_formula_weight 10645.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz '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, -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' _cell_length_a 37.232(13) _cell_length_b 37.232(13) _cell_length_c 60.29(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 83575(59) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9144 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 14.01 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.94 _exptl_crystal_size_mid 0.84 _exptl_crystal_size_min 0.65 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.423 # Unidentified solvents and cations are not included in the calculation. _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10908 _exptl_absorpt_coefficient_mu 0.285 # Unidentified solvents and cations are not included in the calculation. _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8613 _exptl_absorpt_correction_T_max 0.8706 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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_reflns_number 322869 _diffrn_reflns_av_R_equivalents 0.1398 _diffrn_reflns_av_sigmaI/netI 0.2306 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 15.93 _reflns_number_total 10252 _reflns_number_gt 4023 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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. Since the data resolution is low due to the disordered solvents and cations, the constraints and restraints are applied to make the bond lengths, bond angles, and atomic displacements more meaningful. DANG 2.45 0.01 C46 C41 C46 C43 DANG 2.45 0.01 C55 C43 C55 C45 DFIX 1.54 0.01 C7 C8 C7 C9 C7 C10 C17 C18 C17 C19 C17 C20 DFIX 1.54 0.01 C27 C28 C27 C29 C27 C30 DFIX 1.48 0.01 C4 C7 C14 C17 C24 C27 C31 C32 C51 C54 C60 C63 DFIX 1.44 0.01 C35 C38 C39 C40 C42 C46 C47 C48 C44 C55 C56 C57 DFIX 1.18 001 C38 C39 C46 C47 C55 C56 DFIX 1.24 0.01 C31 O14 C31 O15 C54 O16 C54 O17 C63 O18 C63 O19 EADP C1 > C7 EADP C11 > C17 EADP C21 > C27 EADP C31 > C38 EADP C39 > C46 C55 EADP C47 > C54 EADP C56 > C63 ISOR 0.003 0.006 C8 > C10 C18 > C20 C28 > C30 C11 C31 C39 C47 C56 ISOR 0.003 0.006 O1 > O19 SIMU 0.01 0.02 C7 C8 C9 C10 SIMU 0.01 0.02 C17 C18 C19 C20 SIMU 0.01 0.02 C27 C28 C29 C30 SIMU 0.01 0.02 C55 C56 DELU 0.01 0.01 Co1 O1 DELU 0.01 0.01 Co4 O2 ; _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^)+(0.0320P)^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 10252 _refine_ls_number_parameters 412 _refine_ls_number_restraints 294 _refine_ls_R_factor_all 0.1660 _refine_ls_R_factor_gt 0.1084 _refine_ls_wR_factor_ref 0.2421 _refine_ls_wR_factor_gt 0.2273 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.075 _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 0.24129(6) 0.34704(6) -0.03484(4) 0.0825(8) Uani 1 1 d U . . Co2 Co 0.19676(9) 0.38090(9) 0.0000 0.0857(12) Uani 1 2 d S . . Co3 Co 0.28511(9) 0.31297(8) 0.0000 0.0833(12) Uani 1 2 d S . . Co4 Co 0.03479(7) 0.04401(7) 0.26327(4) 0.1091(10) Uani 1 1 d U . . S1 S 0.28220(13) 0.39991(14) -0.06503(9) 0.0791(16) Uani 1 1 d . . . S2 S 0.19822(18) 0.46336(19) 0.0000 0.081(2) Uani 1 2 d S . . S3 S 0.36538(18) 0.33512(17) 0.0000 0.071(2) Uani 1 2 d S . . S4 S 0.06675(16) 0.08124(17) 0.30442(10) 0.122(2) Uani 1 1 d . . . O1 O 0.2328(3) 0.3365(3) 0.0000 0.067(4) Uani 1 2 d SU . . H1O H 0.2195 0.3189 0.0000 0.100 Uiso 1 2 d SR . . O2 O 0.0000 0.0000 0.2552(3) 0.092(4) Uani 1 4 d SU . . H2O H 0.0000 0.0000 0.2416 0.138 Uiso 1 4 d SR . . O3 O 0.2330(2) 0.3969(3) -0.02324(15) 0.083(3) Uani 1 1 d U . . O4 O 0.2923(2) 0.3511(2) -0.02299(15) 0.072(3) Uani 1 1 d U . . O5 O 0.2580(3) 0.3686(3) -0.06455(18) 0.106(4) Uani 1 1 d U . . O6 O 0.2915(3) 0.4128(3) -0.08556(19) 0.080(4) Uani 1 1 d U . . O7 O 0.1748(4) 0.4318(4) 0.0000 0.094(5) Uani 1 2 d SU . . O8 O 0.1820(4) 0.4967(4) 0.0000 0.088(5) Uani 1 2 d SU . . O9 O 0.3413(4) 0.3055(4) 0.0000 0.080(5) Uani 1 2 d SU . . O10 O 0.4030(4) 0.3266(3) 0.0000 0.073(5) Uani 1 2 d SU . . O11 O -0.0057(3) 0.0531(3) 0.28488(17) 0.106(4) Uani 1 1 d U . . O12 O 0.0673(3) 0.0797(3) 0.2813(2) 0.125(5) Uani 1 1 d U . . O13 O 0.0889(3) 0.1073(4) 0.3133(2) 0.134(5) Uani 1 1 d U . . O14 O 0.1590(3) 0.3677(3) 0.02194(17) 0.092(4) Uani 1 1 d DU . . O15 O 0.1920(3) 0.3422(3) 0.04852(17) 0.102(4) Uani 1 1 d DU . . O16 O 0.0203(3) 0.0854(3) 0.24243(19) 0.117(4) Uani 1 1 d DU . . O17 O -0.0389(3) 0.0754(3) 0.2420(2) 0.127(5) Uani 1 1 d DU . . O18 O -0.2983(3) 0.2495(3) 0.04857(16) 0.095(4) Uani 1 1 d DU . . O19 O -0.2724(3) 0.2808(3) 0.02192(17) 0.095(4) Uani 1 1 d DU . . C1 C 0.2402(3) 0.4310(2) -0.0337(2) 0.090(2) Uani 1 1 d G . . C2 C 0.2621(3) 0.4341(3) -0.0522(2) 0.090(2) Uani 1 1 d G . . C3 C 0.2706(2) 0.4679(4) -0.06054(14) 0.090(2) Uani 1 1 d G . . H3 H 0.2856 0.4700 -0.0732 0.108 Uiso 1 1 calc R . . C4 C 0.2573(3) 0.4985(2) -0.05028(19) 0.090(2) Uani 1 1 d GD . . C5 C 0.2354(3) 0.4954(3) -0.03170(18) 0.090(2) Uani 1 1 d G . . H5 H 0.2262 0.5163 -0.0247 0.108 Uiso 1 1 calc R . . C6 C 0.2268(2) 0.4616(4) -0.02340(13) 0.090(2) Uani 1 1 d G . . C7 C 0.2652(4) 0.5352(3) -0.0591(2) 0.090(2) Uani 1 1 d DU . . C8 C 0.2883(4) 0.5577(4) -0.0435(3) 0.150(7) Uani 1 1 d DU . . H8A H 0.2930 0.5811 -0.0502 0.224 Uiso 1 1 calc R . . H8B H 0.3110 0.5453 -0.0407 0.224 Uiso 1 1 calc R . . H8C H 0.2755 0.5611 -0.0294 0.224 Uiso 1 1 calc R . . C9 C 0.2849(5) 0.5347(5) -0.0811(3) 0.148(7) Uani 1 1 d DU . . H9A H 0.2890 0.5594 -0.0861 0.223 Uiso 1 1 calc R . . H9B H 0.2705 0.5218 -0.0921 0.223 Uiso 1 1 calc R . . H9C H 0.3081 0.5225 -0.0792 0.223 Uiso 1 1 calc R . . C10 C 0.2316(4) 0.5559(5) -0.0666(3) 0.163(7) Uani 1 1 d DU . . H10A H 0.2388 0.5791 -0.0729 0.245 Uiso 1 1 calc R . . H10B H 0.2158 0.5599 -0.0539 0.245 Uiso 1 1 calc R . . H10C H 0.2189 0.5419 -0.0779 0.245 Uiso 1 1 calc R . . C11 C 0.3239(3) 0.3664(3) -0.0324(2) 0.087(2) Uani 1 1 d GU . . C12 C 0.3210(2) 0.3897(3) -0.05037(19) 0.087(2) Uani 1 1 d G . . C13 C 0.3513(4) 0.4072(2) -0.05841(13) 0.087(2) Uani 1 1 d G . . H13 H 0.3493 0.4231 -0.0707 0.105 Uiso 1 1 calc R . . C14 C 0.3845(3) 0.4014(3) -0.04852(18) 0.087(2) Uani 1 1 d GD . . C15 C 0.3874(2) 0.3781(3) -0.03059(18) 0.087(2) Uani 1 1 d G . . H15 H 0.4101 0.3742 -0.0238 0.105 Uiso 1 1 calc R . . C16 C 0.3571(4) 0.3606(2) -0.02256(13) 0.087(2) Uani 1 1 d G . . C17 C 0.4171(3) 0.4185(4) -0.0574(2) 0.087(2) Uani 1 1 d DU . . C18 C 0.4256(4) 0.4446(4) -0.0388(3) 0.144(7) Uani 1 1 d DU . . H18A H 0.4477 0.4578 -0.0424 0.216 Uiso 1 1 calc R . . H18B H 0.4290 0.4313 -0.0249 0.216 Uiso 1 1 calc R . . H18C H 0.4057 0.4616 -0.0371 0.216 Uiso 1 1 calc R . . C19 C 0.4122(4) 0.4516(4) -0.0715(2) 0.119(6) Uani 1 1 d DU . . H19A H 0.4357 0.4622 -0.0748 0.179 Uiso 1 1 calc R . . H19B H 0.3974 0.4691 -0.0636 0.179 Uiso 1 1 calc R . . H19C H 0.4003 0.4450 -0.0855 0.179 Uiso 1 1 calc R . . C20 C 0.4510(4) 0.3965(4) -0.0566(3) 0.125(6) Uani 1 1 d DU . . H20A H 0.4714 0.4115 -0.0610 0.187 Uiso 1 1 calc R . . H20B H 0.4488 0.3762 -0.0669 0.187 Uiso 1 1 calc R . . H20C H 0.4547 0.3875 -0.0415 0.187 Uiso 1 1 calc R . . C21 C -0.0073(5) 0.0743(3) 0.30428(16) 0.128(3) Uani 1 1 d G . . C22 C 0.0239(3) 0.0878(4) 0.3138(2) 0.128(3) Uani 1 1 d G . . C23 C 0.0219(3) 0.1089(3) 0.3328(2) 0.128(3) Uani 1 1 d G . . H23 H 0.0433 0.1181 0.3393 0.154 Uiso 1 1 calc R . . C24 C -0.0112(5) 0.1167(3) 0.34217(16) 0.128(3) Uani 1 1 d GD . . C25 C -0.0425(3) 0.1032(4) 0.3326(2) 0.128(3) Uani 1 1 d G . . H25 H -0.0651 0.1085 0.3391 0.154 Uiso 1 1 calc R . . C26 C -0.0405(4) 0.0821(3) 0.3137(2) 0.128(3) Uani 1 1 d G . . C27 C -0.0082(5) 0.1382(4) 0.3631(2) 0.128(3) Uani 1 1 d DU . . C28 C 0.0105(5) 0.1191(5) 0.3825(3) 0.183(8) Uani 1 1 d DU . . H28A H 0.0115 0.1352 0.3953 0.274 Uiso 1 1 calc R . . H28B H 0.0350 0.1125 0.3781 0.274 Uiso 1 1 calc R . . H28C H -0.0030 0.0974 0.3864 0.274 Uiso 1 1 calc R . . C29 C 0.0091(5) 0.1757(4) 0.3619(3) 0.183(8) Uani 1 1 d DU . . H29A H 0.0086 0.1868 0.3766 0.275 Uiso 1 1 calc R . . H29B H -0.0044 0.1907 0.3514 0.275 Uiso 1 1 calc R . . H29C H 0.0340 0.1734 0.3569 0.275 Uiso 1 1 calc R . . C30 C -0.0452(4) 0.1456(5) 0.3732(3) 0.166(7) Uani 1 1 d DU . . H30A H -0.0425 0.1604 0.3865 0.248 Uiso 1 1 calc R . . H30B H -0.0567 0.1228 0.3771 0.248 Uiso 1 1 calc R . . H30C H -0.0601 0.1583 0.3623 0.248 Uiso 1 1 calc R . . C31 C 0.1636(3) 0.3488(5) 0.0387(2) 0.134(3) Uani 1 1 d DU . . C32 C 0.1310(3) 0.3410(3) 0.0526(2) 0.134(3) Uani 1 1 d GD . . C33 C 0.1346(3) 0.3228(3) 0.0725(2) 0.134(3) Uani 1 1 d G . . H33 H 0.1579 0.3177 0.0782 0.161 Uiso 1 1 calc R . . C34 C 0.1043(4) 0.3119(3) 0.08422(14) 0.134(3) Uani 1 1 d G . . H34 H 0.1068 0.2995 0.0979 0.161 Uiso 1 1 calc R . . C35 C 0.0703(3) 0.3194(3) 0.0759(2) 0.134(3) Uani 1 1 d GD . . C36 C 0.0666(3) 0.3376(3) 0.0559(2) 0.134(3) Uani 1 1 d G . . H36 H 0.0434 0.3427 0.0502 0.161 Uiso 1 1 calc R . . C37 C 0.0969(4) 0.3485(3) 0.04425(14) 0.134(3) Uani 1 1 d G . . H37 H 0.0944 0.3609 0.0306 0.161 Uiso 1 1 calc R . . C38 C 0.0392(4) 0.3054(5) 0.0872(3) 0.134(3) Uani 1 1 d D . . C39 C 0.0151(4) 0.2966(6) 0.0959(3) 0.167(3) Uani 1 1 d DU . . C40 C -0.0157(3) 0.2812(3) 0.1067(2) 0.167(3) Uani 1 1 d GD . . C41 C -0.0097(2) 0.2620(3) 0.1262(2) 0.167(3) Uani 1 1 d GD . . H41 H 0.0137 0.2610 0.1324 0.200 Uiso 1 1 calc R . . C42 C -0.0380(3) 0.2444(3) 0.13654(16) 0.167(3) Uani 1 1 d GD . . C43 C -0.0723(2) 0.2459(3) 0.12747(17) 0.167(3) Uani 1 1 d GD . . H43 H -0.0916 0.2338 0.1346 0.200 Uiso 1 1 calc R . . C44 C -0.0783(3) 0.2650(3) 0.10802(18) 0.167(3) Uani 1 1 d GD . . C45 C -0.0500(3) 0.2826(3) 0.09765(17) 0.167(3) Uani 1 1 d GD . . H45 H -0.0541 0.2957 0.0844 0.200 Uiso 1 1 calc R . . C46 C -0.0308(4) 0.2212(5) 0.1553(3) 0.167(3) Uani 1 1 d D . . C47 C -0.0289(5) 0.1962(5) 0.1699(3) 0.146(3) Uani 1 1 d DU . . C48 C -0.0238(5) 0.1714(3) 0.18790(17) 0.146(3) Uani 1 1 d GD . . C49 C 0.0102(3) 0.1639(3) 0.1963(2) 0.146(3) Uani 1 1 d G . . H49 H 0.0306 0.1764 0.1907 0.175 Uiso 1 1 calc R . . C50 C 0.0144(3) 0.1382(4) 0.2127(2) 0.146(3) Uani 1 1 d G . . H50 H 0.0376 0.1330 0.2184 0.175 Uiso 1 1 calc R . . C51 C -0.0154(5) 0.1199(3) 0.22085(17) 0.146(3) Uani 1 1 d GD . . C52 C -0.0494(3) 0.1274(3) 0.2125(2) 0.146(3) Uani 1 1 d G . . H52 H -0.0697 0.1149 0.2180 0.175 Uiso 1 1 calc R . . C53 C -0.0535(3) 0.1532(4) 0.1960(2) 0.146(3) Uani 1 1 d G . . H53 H -0.0768 0.1583 0.1903 0.175 Uiso 1 1 calc R . . C54 C -0.0105(4) 0.0885(4) 0.2351(3) 0.146(3) Uani 1 1 d D . . C55 C -0.1133(4) 0.2637(6) 0.0977(3) 0.167(3) Uani 1 1 d DU . . C56 C -0.1412(4) 0.2645(5) 0.0890(3) 0.139(3) Uani 1 1 d DU . . C57 C -0.1751(3) 0.2656(3) 0.0778(2) 0.139(3) Uani 1 1 d GD . . C58 C -0.2058(4) 0.2507(3) 0.08705(15) 0.139(3) Uani 1 1 d G . . H58 H -0.2051 0.2409 0.1016 0.167 Uiso 1 1 calc R . . C59 C -0.2377(3) 0.2500(3) 0.0750(2) 0.139(3) Uani 1 1 d G . . H59 H -0.2587 0.2397 0.0813 0.167 Uiso 1 1 calc R . . C60 C -0.2387(3) 0.2643(3) 0.0537(2) 0.139(3) Uani 1 1 d GD . . C61 C -0.2079(4) 0.2792(3) 0.04447(15) 0.139(3) Uani 1 1 d G . . H61 H -0.2087 0.2890 0.0299 0.167 Uiso 1 1 calc R . . C62 C -0.1761(3) 0.2799(3) 0.0565(3) 0.139(3) Uani 1 1 d G . . H62 H -0.1551 0.2901 0.0502 0.167 Uiso 1 1 calc R . . C63 C -0.2716(3) 0.2633(5) 0.0394(2) 0.139(3) Uani 1 1 d 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 0.0725(19) 0.0644(19) 0.111(2) -0.0079(17) -0.0125(17) -0.0109(15) Co2 0.075(3) 0.085(3) 0.097(3) 0.000 0.000 -0.032(2) Co3 0.100(3) 0.058(3) 0.091(3) 0.000 0.000 -0.021(2) Co4 0.129(3) 0.136(3) 0.0623(19) 0.0011(19) 0.0021(19) 0.0045(19) S1 0.076(4) 0.083(4) 0.079(4) 0.019(4) 0.014(3) 0.019(3) S2 0.094(6) 0.049(6) 0.099(6) 0.000 0.000 0.011(5) S3 0.069(6) 0.064(5) 0.080(6) 0.000 0.000 -0.004(5) S4 0.144(6) 0.136(6) 0.086(5) -0.021(4) -0.003(4) -0.017(4) O1 0.064(5) 0.067(5) 0.069(5) 0.000 0.000 0.003(3) O2 0.092(4) 0.092(4) 0.091(5) 0.000 0.000 0.000 O3 0.080(4) 0.086(4) 0.083(4) -0.006(3) 0.000(3) 0.001(3) O4 0.074(4) 0.068(4) 0.073(4) -0.004(3) -0.007(3) 0.006(3) O5 0.106(5) 0.106(5) 0.107(5) 0.001(3) -0.002(3) 0.004(3) O6 0.074(6) 0.082(6) 0.084(6) 0.001(5) 0.000(5) 0.008(4) O7 0.095(6) 0.094(6) 0.093(6) 0.000 0.000 -0.001(3) O8 0.085(7) 0.091(7) 0.089(7) 0.000 0.000 -0.007(5) O9 0.081(6) 0.080(6) 0.080(6) 0.000 0.000 0.002(3) O10 0.070(7) 0.072(7) 0.077(7) 0.000 0.000 0.005(5) O11 0.105(5) 0.108(5) 0.106(5) 0.005(3) 0.001(3) -0.002(3) O12 0.124(5) 0.126(5) 0.123(5) 0.001(3) 0.000(3) 0.000(3) O13 0.135(7) 0.138(7) 0.130(7) -0.003(5) -0.006(5) 0.001(5) O14 0.092(4) 0.092(4) 0.092(4) -0.003(3) -0.002(3) -0.003(3) O15 0.104(5) 0.100(5) 0.103(5) 0.000(3) 0.002(3) -0.002(3) O16 0.117(5) 0.118(5) 0.116(5) 0.000(3) 0.002(3) -0.002(3) O17 0.127(5) 0.129(5) 0.126(5) -0.004(3) -0.002(3) 0.002(3) O18 0.097(5) 0.093(4) 0.096(5) 0.001(3) -0.003(3) 0.005(3) O19 0.093(4) 0.095(4) 0.097(4) -0.003(3) 0.001(3) 0.001(3) C1 0.087(5) 0.083(6) 0.100(6) -0.009(5) 0.020(4) 0.004(5) C2 0.087(5) 0.083(6) 0.100(6) -0.009(5) 0.020(4) 0.004(5) C3 0.087(5) 0.083(6) 0.100(6) -0.009(5) 0.020(4) 0.004(5) C4 0.087(5) 0.083(6) 0.100(6) -0.009(5) 0.020(4) 0.004(5) C5 0.087(5) 0.083(6) 0.100(6) -0.009(5) 0.020(4) 0.004(5) C6 0.087(5) 0.083(6) 0.100(6) -0.009(5) 0.020(4) 0.004(5) C7 0.087(5) 0.083(6) 0.100(6) -0.009(5) 0.020(4) 0.004(5) C8 0.154(8) 0.143(8) 0.152(8) 0.001(6) -0.002(6) -0.010(6) C9 0.151(8) 0.144(8) 0.151(8) 0.003(6) 0.013(6) -0.002(6) C10 0.164(8) 0.159(8) 0.167(8) 0.008(6) 0.005(6) -0.001(6) C11 0.087(3) 0.086(3) 0.089(3) 0.009(2) -0.004(3) 0.001(3) C12 0.087(3) 0.086(3) 0.089(3) 0.009(2) -0.004(3) 0.001(3) C13 0.087(3) 0.086(3) 0.089(3) 0.009(2) -0.004(3) 0.001(3) C14 0.087(3) 0.086(3) 0.089(3) 0.009(2) -0.004(3) 0.001(3) C15 0.087(3) 0.086(3) 0.089(3) 0.009(2) -0.004(3) 0.001(3) C16 0.087(3) 0.086(3) 0.089(3) 0.009(2) -0.004(3) 0.001(3) C17 0.087(3) 0.086(3) 0.089(3) 0.009(2) -0.004(3) 0.001(3) C18 0.140(8) 0.144(8) 0.148(8) 0.007(6) 0.001(6) 0.001(6) C19 0.117(8) 0.120(8) 0.121(8) 0.012(5) 0.006(5) -0.010(5) C20 0.118(8) 0.127(8) 0.130(8) 0.005(5) 0.001(5) -0.003(5) C21 0.121(6) 0.146(7) 0.117(7) -0.018(5) 0.012(6) -0.012(6) C22 0.121(6) 0.146(7) 0.117(7) -0.018(5) 0.012(6) -0.012(6) C23 0.121(6) 0.146(7) 0.117(7) -0.018(5) 0.012(6) -0.012(6) C24 0.121(6) 0.146(7) 0.117(7) -0.018(5) 0.012(6) -0.012(6) C25 0.121(6) 0.146(7) 0.117(7) -0.018(5) 0.012(6) -0.012(6) C26 0.121(6) 0.146(7) 0.117(7) -0.018(5) 0.012(6) -0.012(6) C27 0.121(6) 0.146(7) 0.117(7) -0.018(5) 0.012(6) -0.012(6) C28 0.181(9) 0.190(9) 0.178(9) -0.007(6) -0.002(6) 0.000(6) C29 0.184(9) 0.184(9) 0.183(9) -0.011(6) 0.008(6) -0.005(6) C30 0.166(9) 0.166(9) 0.165(9) -0.007(6) 0.005(6) -0.001(6) C31 0.130(4) 0.137(4) 0.135(4) 0.011(3) 0.002(3) -0.004(3) C32 0.130(4) 0.137(4) 0.135(4) 0.011(3) 0.002(3) -0.004(3) C33 0.130(4) 0.137(4) 0.135(4) 0.011(3) 0.002(3) -0.004(3) C34 0.130(4) 0.137(4) 0.135(4) 0.011(3) 0.002(3) -0.004(3) C35 0.130(4) 0.137(4) 0.135(4) 0.011(3) 0.002(3) -0.004(3) C36 0.130(4) 0.137(4) 0.135(4) 0.011(3) 0.002(3) -0.004(3) C37 0.130(4) 0.137(4) 0.135(4) 0.011(3) 0.002(3) -0.004(3) C38 0.130(4) 0.137(4) 0.135(4) 0.011(3) 0.002(3) -0.004(3) C39 0.160(4) 0.173(4) 0.167(4) 0.020(3) -0.004(3) -0.003(3) C40 0.160(4) 0.173(4) 0.167(4) 0.020(3) -0.004(3) -0.003(3) C41 0.160(4) 0.173(4) 0.167(4) 0.020(3) -0.004(3) -0.003(3) C42 0.160(4) 0.173(4) 0.167(4) 0.020(3) -0.004(3) -0.003(3) C43 0.160(4) 0.173(4) 0.167(4) 0.020(3) -0.004(3) -0.003(3) C44 0.160(4) 0.173(4) 0.167(4) 0.020(3) -0.004(3) -0.003(3) C45 0.160(4) 0.173(4) 0.167(4) 0.020(3) -0.004(3) -0.003(3) C46 0.160(4) 0.173(4) 0.167(4) 0.020(3) -0.004(3) -0.003(3) C47 0.141(4) 0.149(4) 0.147(4) 0.014(3) 0.000(3) -0.001(3) C48 0.141(4) 0.149(4) 0.147(4) 0.014(3) 0.000(3) -0.001(3) C49 0.141(4) 0.149(4) 0.147(4) 0.014(3) 0.000(3) -0.001(3) C50 0.141(4) 0.149(4) 0.147(4) 0.014(3) 0.000(3) -0.001(3) C51 0.141(4) 0.149(4) 0.147(4) 0.014(3) 0.000(3) -0.001(3) C52 0.141(4) 0.149(4) 0.147(4) 0.014(3) 0.000(3) -0.001(3) C53 0.141(4) 0.149(4) 0.147(4) 0.014(3) 0.000(3) -0.001(3) C54 0.141(4) 0.149(4) 0.147(4) 0.014(3) 0.000(3) -0.001(3) C55 0.160(4) 0.173(4) 0.167(4) 0.020(3) -0.004(3) -0.003(3) C56 0.133(4) 0.144(4) 0.140(4) 0.014(3) -0.004(3) -0.004(3) C57 0.133(4) 0.144(4) 0.140(4) 0.014(3) -0.004(3) -0.004(3) C58 0.133(4) 0.144(4) 0.140(4) 0.014(3) -0.004(3) -0.004(3) C59 0.133(4) 0.144(4) 0.140(4) 0.014(3) -0.004(3) -0.004(3) C60 0.133(4) 0.144(4) 0.140(4) 0.014(3) -0.004(3) -0.004(3) C61 0.133(4) 0.144(4) 0.140(4) 0.014(3) -0.004(3) -0.004(3) C62 0.133(4) 0.144(4) 0.140(4) 0.014(3) -0.004(3) -0.004(3) C63 0.133(4) 0.144(4) 0.140(4) 0.014(3) -0.004(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.009(10) . ? Co1 O18 2.016(10) 10 ? Co1 O15 2.021(11) 11 ? Co1 O4 2.033(9) . ? Co1 O5 2.060(12) . ? Co1 O1 2.160(4) . ? Co1 Co3 2.947(3) . ? Co1 Co2 2.958(3) . ? Co2 O14 1.993(10) 11 ? Co2 O14 1.993(10) . ? Co2 O3 2.036(10) . ? Co2 O3 2.036(10) 11 ? Co2 O7 2.063(16) . ? Co2 O1 2.131(12) . ? Co2 Co1 2.958(3) 11 ? Co3 O4 2.002(9) 11 ? Co3 O4 2.002(9) . ? Co3 O19 2.014(10) 10 ? Co3 O19 2.014(10) 4 ? Co3 O9 2.109(15) . ? Co3 O1 2.134(12) . ? Co3 Co1 2.947(3) 11 ? Co4 O17 1.994(12) 4 ? Co4 O11 2.022(11) . ? Co4 O11 2.048(11) 4 ? Co4 O16 2.061(12) . ? Co4 O12 2.101(13) . ? Co4 O2 2.144(5) . ? Co4 Co4 2.954(4) 2 ? Co4 Co4 2.954(4) 4 ? S1 O6 1.372(10) . ? S1 O5 1.472(11) . ? S1 C2 1.667(8) . ? S1 C12 1.735(8) . ? S2 O8 1.381(15) . ? S2 O7 1.463(15) . ? S2 C6 1.769(13) 11 ? S2 C6 1.769(8) . ? S3 O9 1.422(14) . ? S3 O10 1.437(13) . ? S3 C16 1.687(12) 11 ? S3 C16 1.687(8) . ? S4 O13 1.381(12) . ? S4 O12 1.396(12) . ? S4 C22 1.710(10) . ? S4 C26 1.71(4) 4 ? O1 Co1 2.160(4) 11 ? O1 H1O 0.8178 . ? O2 Co4 2.144(5) 3 ? O2 Co4 2.144(5) 4 ? O2 Co4 2.144(5) 2 ? O2 H2O 0.8187 . ? O3 C1 1.440(10) . ? O4 C11 1.427(10) . ? O11 C21 1.412(12) . ? O11 Co4 2.048(11) 2 ? O14 C31 1.242(9) . ? O15 C31 1.238(9) . ? O15 Co1 2.021(11) 11 ? O16 C54 1.237(9) . ? O17 C54 1.233(9) . ? O17 Co4 1.994(12) 2 ? O18 C63 1.250(9) . ? O18 Co1 2.016(10) 12 ? O19 C63 1.240(9) . ? O19 Co3 2.014(10) 2 ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 C7 1.496(9) . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C7 C9 1.515(9) . ? C7 C8 1.526(9) . ? C7 C10 1.536(9) . ? 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 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 C15 1.3900 . ? C14 C17 1.472(8) . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C17 C20 1.503(9) . ? C17 C19 1.511(9) . ? C17 C18 1.518(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 C27 1.501(9) . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 S4 1.714(10) 2 ? C27 C30 1.529(9) . ? C27 C28 1.533(9) . ? C27 C29 1.537(9) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 C32 1.503(9) . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 C36 1.3900 . ? C35 C38 1.443(9) . ? C36 C37 1.3900 . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.087(15) . ? C39 C40 1.440(9) . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 C46 1.447(6) . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 C55 1.447(6) . ? C45 H45 0.9500 . ? C46 C47 1.282(15) . ? C47 C48 1.438(9) . ? C48 C49 1.3900 . ? C48 C53 1.3900 . ? C49 C50 1.3900 . ? C49 H49 0.9500 . ? C50 C51 1.3900 . ? C50 H50 0.9500 . ? C51 C52 1.3900 . ? C51 C54 1.461(9) . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C55 C56 1.162(15) . ? C56 C57 1.432(9) . ? C57 C58 1.3900 . ? C57 C62 1.3900 . ? C58 C59 1.3900 . ? C58 H58 0.9500 . ? C59 C60 1.3900 . ? C59 H59 0.9500 . ? C60 C61 1.3900 . ? C60 C63 1.499(9) . ? C61 C62 1.3900 . ? C61 H61 0.9500 . ? C62 H62 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 O3 Co1 O18 176.1(4) . 10 ? O3 Co1 O15 95.0(4) . 11 ? O18 Co1 O15 83.6(4) 10 11 ? O3 Co1 O4 87.2(4) . . ? O18 Co1 O4 94.0(4) 10 . ? O15 Co1 O4 176.3(4) 11 . ? O3 Co1 O5 89.3(4) . . ? O18 Co1 O5 87.0(4) 10 . ? O15 Co1 O5 87.4(4) 11 . ? O4 Co1 O5 89.7(4) . . ? O3 Co1 O1 78.9(4) . . ? O18 Co1 O1 104.9(4) 10 . ? O15 Co1 O1 104.3(4) 11 . ? O4 Co1 O1 78.9(4) . . ? O5 Co1 O1 163.9(5) . . ? O3 Co1 Co3 103.6(3) . . ? O18 Co1 Co3 79.7(3) 10 . ? O15 Co1 Co3 139.0(3) 11 . ? O4 Co1 Co3 42.7(3) . . ? O5 Co1 Co3 128.3(3) . . ? O1 Co1 Co3 46.3(3) . . ? O3 Co1 Co2 43.4(3) . . ? O18 Co1 Co2 139.4(3) 10 . ? O15 Co1 Co2 79.6(3) 11 . ? O4 Co1 Co2 104.0(3) . . ? O5 Co1 Co2 128.4(3) . . ? O1 Co1 Co2 46.0(3) . . ? Co3 Co1 Co2 89.28(10) . . ? O14 Co2 O14 83.2(6) 11 . ? O14 Co2 O3 94.8(4) 11 . ? O14 Co2 O3 176.1(4) . . ? O14 Co2 O3 176.1(4) 11 11 ? O14 Co2 O3 94.8(4) . 11 ? O3 Co2 O3 87.0(5) . 11 ? O14 Co2 O7 87.0(5) 11 . ? O14 Co2 O7 87.0(5) . . ? O3 Co2 O7 89.6(4) . . ? O3 Co2 O7 89.6(4) 11 . ? O14 Co2 O1 104.7(4) 11 . ? O14 Co2 O1 104.7(4) . . ? O3 Co2 O1 79.1(4) . . ? O3 Co2 O1 79.1(4) 11 . ? O7 Co2 O1 164.3(6) . . ? O14 Co2 Co1 79.6(3) 11 . ? O14 Co2 Co1 139.6(3) . . ? O3 Co2 Co1 42.7(3) . . ? O3 Co2 Co1 104.0(3) 11 . ? O7 Co2 Co1 127.8(2) . . ? O1 Co2 Co1 46.84(10) . . ? O14 Co2 Co1 139.6(3) 11 11 ? O14 Co2 Co1 79.6(3) . 11 ? O3 Co2 Co1 104.0(3) . 11 ? O3 Co2 Co1 42.7(3) 11 11 ? O7 Co2 Co1 127.8(2) . 11 ? O1 Co2 Co1 46.84(10) . 11 ? Co1 Co2 Co1 90.50(13) . 11 ? O4 Co3 O4 87.6(5) 11 . ? O4 Co3 O19 175.6(4) 11 10 ? O4 Co3 O19 95.1(4) . 10 ? O4 Co3 O19 95.1(4) 11 4 ? O4 Co3 O19 175.6(4) . 4 ? O19 Co3 O19 82.0(6) 10 4 ? O4 Co3 O9 87.8(4) 11 . ? O4 Co3 O9 87.8(4) . . ? O19 Co3 O9 88.8(4) 10 . ? O19 Co3 O9 88.8(4) 4 . ? O4 Co3 O1 80.2(4) 11 . ? O4 Co3 O1 80.2(4) . . ? O19 Co3 O1 103.6(4) 10 . ? O19 Co3 O1 103.6(4) 4 . ? O9 Co3 O1 163.4(5) . . ? O4 Co3 Co1 105.2(3) 11 . ? O4 Co3 Co1 43.5(3) . . ? O19 Co3 Co1 79.1(3) 10 . ? O19 Co3 Co1 138.3(3) 4 . ? O9 Co3 Co1 127.3(2) . . ? O1 Co3 Co1 47.05(10) . . ? O4 Co3 Co1 43.5(3) 11 11 ? O4 Co3 Co1 105.2(3) . 11 ? O19 Co3 Co1 138.3(3) 10 11 ? O19 Co3 Co1 79.1(3) 4 11 ? O9 Co3 Co1 127.3(2) . 11 ? O1 Co3 Co1 47.05(10) . 11 ? Co1 Co3 Co1 90.94(13) . 11 ? O17 Co4 O11 175.8(5) 4 . ? O17 Co4 O11 95.2(5) 4 4 ? O11 Co4 O11 87.5(5) . 4 ? O17 Co4 O16 82.9(5) 4 . ? O11 Co4 O16 94.1(4) . . ? O11 Co4 O16 174.6(5) 4 . ? O17 Co4 O12 87.5(5) 4 . ? O11 Co4 O12 89.5(5) . . ? O11 Co4 O12 85.3(5) 4 . ? O16 Co4 O12 89.6(5) . . ? O17 Co4 O2 103.8(5) 4 . ? O11 Co4 O2 79.8(5) . . ? O11 Co4 O2 79.3(5) 4 . ? O16 Co4 O2 106.0(5) . . ? O12 Co4 O2 161.6(6) . . ? O17 Co4 Co4 137.9(3) 4 2 ? O11 Co4 Co4 43.8(3) . 2 ? O11 Co4 Co4 104.5(3) 4 2 ? O16 Co4 Co4 80.1(3) . 2 ? O12 Co4 Co4 130.3(4) . 2 ? O2 Co4 Co4 46.47(11) . 2 ? O17 Co4 Co4 79.4(4) 4 4 ? O11 Co4 Co4 104.7(3) . 4 ? O11 Co4 Co4 43.1(3) 4 4 ? O16 Co4 Co4 140.7(3) . 4 ? O12 Co4 Co4 124.1(3) . 4 ? O2 Co4 Co4 46.47(11) . 4 ? Co4 Co4 Co4 90.0 2 4 ? O6 S1 O5 116.7(8) . . ? O6 S1 C2 105.3(7) . . ? O5 S1 C2 108.7(7) . . ? O6 S1 C12 109.0(7) . . ? O5 S1 C12 109.0(7) . . ? C2 S1 C12 107.7(5) . . ? O8 S2 O7 117.6(10) . . ? O8 S2 C6 107.2(11) . 11 ? O7 S2 C6 109.2(11) . 11 ? O8 S2 C6 107.2(6) . . ? O7 S2 C6 109.2(6) . . ? C6 S2 C6 105.7(11) 11 . ? O9 S3 O10 116.4(9) . . ? O9 S3 C16 108.7(11) . 11 ? O10 S3 C16 107.6(11) . 11 ? O9 S3 C16 108.7(6) . . ? O10 S3 C16 107.6(6) . . ? C16 S3 C16 107.4(11) 11 . ? O13 S4 O12 114.1(9) . . ? O13 S4 C22 109.2(9) . . ? O12 S4 C22 110.6(8) . . ? O13 S4 C26 107.2(10) . 4 ? O12 S4 C26 106.5(12) . 4 ? C22 S4 C26 109.2(12) . 4 ? Co2 O1 Co3 153.2(6) . . ? Co2 O1 Co1 87.1(3) . . ? Co3 O1 Co1 86.6(3) . . ? Co2 O1 Co1 87.2(3) . 11 ? Co3 O1 Co1 86.6(3) . 11 ? Co1 O1 Co1 153.0(6) . 11 ? Co2 O1 H1O 103.8 . . ? Co3 O1 H1O 103.0 . . ? Co1 O1 H1O 103.5 . . ? Co1 O1 H1O 103.5 11 . ? Co4 O2 Co4 87.1(2) 3 4 ? Co4 O2 Co4 87.1(2) 3 2 ? Co4 O2 Co4 153.8(10) 4 2 ? Co4 O2 Co4 153.8(10) 3 . ? Co4 O2 Co4 87.1(2) 4 . ? Co4 O2 Co4 87.1(2) 2 . ? Co4 O2 H2O 103.1 3 . ? Co4 O2 H2O 103.1 4 . ? Co4 O2 H2O 103.1 2 . ? Co4 O2 H2O 103.1 . . ? C1 O3 Co1 129.3(9) . . ? C1 O3 Co2 133.0(9) . . ? Co1 O3 Co2 94.0(4) . . ? C11 O4 Co3 132.0(8) . . ? C11 O4 Co1 131.3(9) . . ? Co3 O4 Co1 93.8(4) . . ? S1 O5 Co1 120.7(7) . . ? S2 O7 Co2 120.2(9) . . ? S3 O9 Co3 121.6(9) . . ? C21 O11 Co4 131.2(11) . . ? C21 O11 Co4 133.2(11) . 2 ? Co4 O11 Co4 93.1(5) . 2 ? S4 O12 Co4 122.3(8) . . ? C31 O14 Co2 125.6(9) . . ? C31 O15 Co1 124.2(9) . 11 ? C54 O16 Co4 122.0(10) . . ? C54 O17 Co4 126.7(10) . 2 ? C63 O18 Co1 126.6(9) . 12 ? C63 O19 Co3 128.0(9) . 2 ? C2 C1 C6 120.0 . . ? C2 C1 O3 122.3(11) . . ? C6 C1 O3 117.5(11) . . ? C1 C2 C3 120.0 . . ? C1 C2 S1 124.9(10) . . ? C3 C2 S1 114.9(9) . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 C7 121.4(11) . . ? C5 C4 C7 118.6(11) . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 S2 113.1(9) . . ? C1 C6 S2 126.9(9) . . ? C4 C7 C9 113.2(12) . . ? C4 C7 C8 113.1(12) . . ? C9 C7 C8 105.9(12) . . ? C4 C7 C10 113.8(12) . . ? C9 C7 C10 98.2(12) . . ? C8 C7 C10 111.4(13) . . ? 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 . . ? C12 C11 C16 120.0 . . ? C12 C11 O4 119.7(11) . . ? C16 C11 O4 120.1(11) . . ? C13 C12 C11 120.0 . . ? C13 C12 S1 113.3(9) . . ? C11 C12 S1 126.7(9) . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 C17 119.2(11) . . ? C13 C14 C17 120.8(11) . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 S3 113.4(10) . . ? C11 C16 S3 126.6(10) . . ? C14 C17 C20 116.5(12) . . ? C14 C17 C19 117.2(12) . . ? C20 C17 C19 124.3(11) . . ? C14 C17 C18 100.4(11) . . ? C20 C17 C18 98.7(12) . . ? C19 C17 C18 85.3(11) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 120.0 . . ? C22 C21 O11 120.6(15) . . ? C26 C21 O11 119.4(15) . . ? C21 C22 C23 120.0 . . ? C21 C22 S4 126.3(12) . . ? C23 C22 S4 113.7(12) . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 C27 112.8(14) . . ? C25 C24 C27 127.1(14) . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 S4 114.2(12) . 2 ? C21 C26 S4 125.8(12) . 2 ? C24 C27 C30 111.2(14) . . ? C24 C27 C28 115.2(14) . . ? C30 C27 C28 101.0(14) . . ? C24 C27 C29 118.5(14) . . ? C30 C27 C29 103.5(14) . . ? C28 C27 C29 105.5(14) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O15 C31 O14 128.3(13) . . ? O15 C31 C32 112.6(12) . . ? O14 C31 C32 116.7(13) . . ? C33 C32 C37 120.0 . . ? C33 C32 C31 119.8(13) . . ? C37 C32 C31 119.8(13) . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 C38 119.4(15) . . ? C36 C35 C38 120.4(15) . . ? C37 C36 C35 120.0 . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C32 120.0 . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C39 C38 C35 176(3) . . ? C38 C39 C40 174(3) . . ? C41 C40 C45 120.0 . . ? C41 C40 C39 117.4(13) . . ? C45 C40 C39 122.4(13) . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 C46 119.6(5) . . ? C43 C42 C46 120.0(5) . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 C55 119.4(5) . . ? C45 C44 C55 120.4(5) . . ? C44 C45 C40 120.0 . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? C47 C46 C42 168(2) . . ? C46 C47 C48 172(2) . . ? C49 C48 C53 120.0 . . ? C49 C48 C47 121.6(16) . . ? C53 C48 C47 118.3(16) . . ? C50 C49 C48 120.0 . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.0 . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 120.0 . . ? C52 C51 C54 119.1(14) . . ? C50 C51 C54 120.0(14) . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C48 120.0 . . ? C52 C53 H53 120.0 . . ? C48 C53 H53 120.0 . . ? O17 C54 O16 129.7(14) . . ? O17 C54 C51 114.0(14) . . ? O16 C54 C51 113.5(14) . . ? C56 C55 C44 176(2) . . ? C55 C56 C57 178(2) . . ? C58 C57 C62 120.0 . . ? C58 C57 C56 121.7(15) . . ? C62 C57 C56 118.2(15) . . ? C59 C58 C57 120.0 . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C58 C59 C60 120.0 . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.0 . . ? C61 C60 C59 120.0 . . ? C61 C60 C63 116.9(13) . . ? C59 C60 C63 123.1(13) . . ? C62 C61 C60 120.0 . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C61 C62 C57 120.0 . . ? C61 C62 H62 120.0 . . ? C57 C62 H62 120.0 . . ? O19 C63 O18 125.1(13) . . ? O19 C63 C60 119.7(13) . . ? O18 C63 C60 114.0(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 15.93 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.937 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.061 # 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 0.025 -0.012 -0.002 55011 12172 ' ' 2 0.001 -0.001 0.500 849 403 ' ' 3 0.500 0.500 0.000 883 423 ' ' _platon_squeeze_details ; R factors from the data before SQUEEZE: _refine_ls_R_factor_all 0.4049 _refine_ls_R_factor_gt 0.2966 _refine_ls_wR_factor_ref 0.6278 _refine_ls_wR_factor_gt 0.5931 ; # start Validation Reply Form _vrf_THETM01_dsc120105sq ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.3862 RESPONSE: It is due to disorder of the solvents and the counter cations, which could not be defined from the DF maps. ; _vrf_PLAT150_dsc120105sq ; PROBLEM: Volume as Calculated Differs from that Given ... 8358.00 Ang-3 RESPONSE: The cell volume is 83575(59) Ang-3 reported by SHELXTL. ; _vrf_PLAT026_dsc120105sq ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 39 Perc. RESPONSE: Even a large crystal did not diffract well. It is due to disorder. ; _vrf_PLAT341_dsc120105sq ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0183 Ang RESPONSE: It is due to disorder. ; _vrf_PLAT420_dsc120105sq ; PROBLEM: D-H Without Acceptor O1 - H1O ... ? D-H Without Acceptor O2 - H2O ... ? RESPONSE: Unidentified solvents or cations may form hydrogen bonds with these hydrogens. ; #END