# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name B.K.Nicholson C.J.Clark S.G.Telfer T.Groutso _publ_contact_author_name 'Brian Nicholson' _publ_contact_author_email chem0021@waikato.ac.nz data_btmam_sq _database_code_depnum_ccdc_archive 'CCDC 866857' #TrackingRef '- btmam_sq_May.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H88 Ba Co O28 Sb12, 5(H2 O)' _chemical_formula_sum 'C84 H98 Ba Co O33 Sb12' _chemical_formula_weight 3292.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -1.0456 8.4617 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.782(3) _cell_length_b 26.290(5) _cell_length_c 29.175(6) _cell_angle_alpha 90.00(3) _cell_angle_beta 91.69(3) _cell_angle_gamma 90.00(3) _cell_volume 12866(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 18442 _cell_measurement_theta_min 6.75 _cell_measurement_theta_max 71.23 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6244 _exptl_absorpt_coefficient_mu 23.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rigaku MM007 rotating anode' _diffrn_radiation_monochromator 'Rigaku VariMax-HF Confocal Optical System' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 123841 _diffrn_reflns_av_R_equivalents 0.1827 _diffrn_reflns_av_sigmaI/netI 0.2162 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 6.74 _diffrn_reflns_theta_max 72.12 _reflns_number_total 23872 _reflns_number_gt 6843 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_data_reduction 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Aryl rings were treated as rigid hexagons, and the Sb-C and Cn4-Cn7 distances were restrained to 2.1 and 1.52 A respectively. H atoms were added in calculated positions for the aryl groups but those of the H2O molecules were not included. ; _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^)+(0.1303P)^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 23872 _refine_ls_number_parameters 369 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.2601 _refine_ls_R_factor_gt 0.1278 _refine_ls_wR_factor_ref 0.3666 _refine_ls_wR_factor_gt 0.3147 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _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 Ba1 Ba 0.23177(10) 0.08801(5) 0.24622(5) 0.1397(6) Uani 1 1 d . . . Sb1 Sb 0.35591(10) 0.19112(5) 0.16026(5) 0.1331(6) Uani 1 1 d D . . Sb2 Sb 0.16585(10) 0.19582(5) 0.14141(5) 0.1327(6) Uani 1 1 d D . . Sb3 Sb 0.04763(10) 0.19804(5) 0.22352(6) 0.1355(6) Uani 1 1 d D . . Sb4 Sb 0.11499(10) 0.19703(5) 0.32789(5) 0.1313(6) Uani 1 1 d D . . Sb5 Sb 0.30186(10) 0.19167(5) 0.34624(5) 0.1293(6) Uani 1 1 d D . . Sb6 Sb 0.42163(10) 0.18868(5) 0.26241(5) 0.1292(6) Uani 1 1 d D . . Sb7 Sb 0.27192(10) 0.29664(5) 0.12860(5) 0.1290(6) Uani 1 1 d D . . Sb8 Sb 0.05114(10) 0.30199(5) 0.28266(5) 0.1279(6) Uani 1 1 d D . . Sb9 Sb 0.39925(10) 0.29311(5) 0.31966(5) 0.1257(6) Uani 1 1 d D . . Sb10 Sb 0.16001(9) 0.38252(5) 0.20211(5) 0.1257(6) Uani 1 1 d D . . Sb11 Sb 0.22924(9) 0.38022(5) 0.30533(5) 0.1216(6) Uani 1 1 d D . . Sb12 Sb 0.34826(9) 0.37842(5) 0.22214(5) 0.1244(6) Uani 1 1 d D . . Co1 Co 0.2380(2) 0.26300(12) 0.24319(11) 0.1209(11) Uani 1 1 d . . . O1 O 0.2665(8) 0.1557(5) 0.1338(4) 0.130(4) Uiso 1 1 d . . . O2 O 0.1421(7) 0.1602(5) 0.1987(4) 0.125(4) Uiso 1 1 d . . . O3 O 0.0485(8) 0.1602(5) 0.2812(5) 0.144(5) Uiso 1 1 d . . . O4 O 0.2119(7) 0.1585(5) 0.3141(4) 0.116(4) Uiso 1 1 d . . . O5 O 0.3421(8) 0.1550(5) 0.2188(4) 0.137(5) Uiso 1 1 d . . . O6 O 0.1908(7) 0.2507(4) 0.0981(4) 0.114(4) Uiso 1 1 d . . . O7 O 0.3804(7) 0.1498(5) 0.3145(4) 0.125(4) Uiso 1 1 d . . . O8 O 0.0807(7) 0.2419(4) 0.1686(4) 0.113(4) Uiso 1 1 d . . . O9 O -0.0183(7) 0.2530(4) 0.2444(4) 0.118(4) Uiso 1 1 d . . . O10 O 0.0419(8) 0.2553(5) 0.3361(4) 0.128(4) Uiso 1 1 d . . . O11 O 0.2063(6) 0.2393(4) 0.3611(4) 0.100(4) Uiso 1 1 d . . . O12 O 0.3758(7) 0.2454(5) 0.3698(4) 0.121(4) Uiso 1 1 d . . . O13 O 0.4812(9) 0.2420(5) 0.2978(5) 0.151(5) Uiso 1 1 d . . . O14 O 0.3250(7) 0.2380(4) 0.2855(4) 0.105(4) Uiso 1 1 d . . . O15 O 0.1360(8) 0.2427(5) 0.2662(4) 0.126(4) Uiso 1 1 d . . . O16 O 0.4312(8) 0.2307(5) 0.2055(4) 0.132(4) Uiso 1 1 d . . . O17 O 0.2569(7) 0.2396(4) 0.1798(4) 0.107(4) Uiso 1 1 d . . . O18 O 0.3601(8) 0.2483(5) 0.1171(4) 0.129(4) Uiso 1 1 d . . . O19 O 0.1790(7) 0.3337(5) 0.1550(4) 0.123(4) Uiso 1 1 d . . . O20 O 0.0800(7) 0.3336(5) 0.2238(4) 0.116(4) Uiso 1 1 d . . . O21 O 0.1424(8) 0.3302(5) 0.3172(4) 0.124(4) Uiso 1 1 d . . . O22 O 0.3026(7) 0.3287(5) 0.3355(4) 0.121(4) Uiso 1 1 d . . . O23 O 0.4117(8) 0.3264(5) 0.2600(4) 0.124(4) Uiso 1 1 d . . . O24 O 0.2471(6) 0.3345(4) 0.2431(3) 0.083(3) Uiso 1 1 d . . . O25 O 0.3558(8) 0.3254(5) 0.1739(4) 0.129(4) Uiso 1 1 d . . . O26 O 0.2646(8) 0.4184(5) 0.1895(5) 0.144(5) Uiso 1 1 d . . . O27 O 0.1591(8) 0.4178(5) 0.2626(4) 0.132(5) Uiso 1 1 d . . . O28 O 0.3263(8) 0.4136(5) 0.2795(4) 0.129(4) Uiso 1 1 d . . . OW1 O 0.1314(9) 0.0122(6) 0.2026(5) 0.164(5) Uiso 1 1 d . . . OW2 O 0.2174(9) 0.0168(6) 0.3215(5) 0.156(5) Uiso 1 1 d . . . OW3 O 0.3619(10) 0.0168(7) 0.2346(6) 0.184(6) Uiso 1 1 d . . . OW4 O 0.2637(11) 0.0593(7) 0.1534(6) 0.198(7) Uiso 1 1 d . . . OW5 O 0.0634(14) 0.0604(9) 0.2858(8) 0.260(9) Uiso 1 1 d . . . C11 C 0.4394(10) 0.1440(8) 0.1286(8) 0.2156(17) Uiso 1 1 d GD . . C12 C 0.4612(12) 0.0971(9) 0.1469(5) 0.2156(17) Uiso 1 1 d G . . H12 H 0.4419 0.0868 0.1757 0.259 Uiso 1 1 calc R . . C13 C 0.5112(13) 0.0651(6) 0.1229(8) 0.2156(17) Uiso 1 1 d G . . H13 H 0.5262 0.0330 0.1354 0.259 Uiso 1 1 calc R . . C14 C 0.5394(10) 0.0802(8) 0.0807(8) 0.2156(17) Uiso 1 1 d GD . . C15 C 0.5176(12) 0.1271(10) 0.0624(5) 0.2156(17) Uiso 1 1 d G . . H15 H 0.5369 0.1374 0.0336 0.259 Uiso 1 1 calc R . . C16 C 0.4676(12) 0.1591(6) 0.0863(8) 0.2156(17) Uiso 1 1 d G . . H16 H 0.4526 0.1912 0.0738 0.259 Uiso 1 1 calc R . . C17 C 0.5865(19) 0.0436(11) 0.0531(10) 0.275(5) Uiso 1 1 d D . . H17A H 0.6428 0.0535 0.0544 0.413 Uiso 1 1 calc R . . H17B H 0.5666 0.0440 0.0212 0.413 Uiso 1 1 calc R . . H17C H 0.5810 0.0092 0.0657 0.413 Uiso 1 1 calc R . . C21 C 0.0863(11) 0.1532(10) 0.1004(6) 0.2156(17) Uiso 1 1 d GD . . C22 C 0.0915(10) 0.1006(9) 0.0967(6) 0.2156(17) Uiso 1 1 d G . . H22 H 0.1277 0.0823 0.1162 0.259 Uiso 1 1 calc R . . C23 C 0.0439(14) 0.0748(6) 0.0646(8) 0.2156(17) Uiso 1 1 d G . . H23 H 0.0475 0.0388 0.0622 0.259 Uiso 1 1 calc R . . C24 C -0.0090(11) 0.1016(10) 0.0361(6) 0.2156(17) Uiso 1 1 d GD . . C25 C -0.0143(11) 0.1542(9) 0.0398(6) 0.2156(17) Uiso 1 1 d G . . H25 H -0.0504 0.1725 0.0203 0.259 Uiso 1 1 calc R . . C26 C 0.0334(14) 0.1800(6) 0.0719(8) 0.2156(17) Uiso 1 1 d G . . H26 H 0.0298 0.2159 0.0743 0.259 Uiso 1 1 calc R . . C27 C -0.0666(18) 0.0703(12) 0.0066(11) 0.275(5) Uiso 1 1 d D . . H27A H -0.0712 0.0361 0.0195 0.413 Uiso 1 1 calc R . . H27B H -0.0468 0.0680 -0.0246 0.413 Uiso 1 1 calc R . . H27C H -0.1191 0.0867 0.0057 0.413 Uiso 1 1 calc R . . C31 C -0.0437(11) 0.1570(10) 0.1890(6) 0.2156(17) Uiso 1 1 d GD . . C32 C -0.0406(10) 0.1048(9) 0.1820(6) 0.2156(17) Uiso 1 1 d G . . H32 H 0.0019 0.0854 0.1954 0.259 Uiso 1 1 calc R . . C33 C -0.0997(15) 0.0808(6) 0.1555(7) 0.2156(17) Uiso 1 1 d G . . H33 H -0.0976 0.0451 0.1508 0.259 Uiso 1 1 calc R . . C34 C -0.1618(11) 0.1091(10) 0.1360(6) 0.2156(17) Uiso 1 1 d GD . . C35 C -0.1649(11) 0.1614(10) 0.1429(6) 0.2156(17) Uiso 1 1 d G . . H35 H -0.2073 0.1808 0.1295 0.259 Uiso 1 1 calc R . . C36 C -0.1058(15) 0.1854(6) 0.1694(7) 0.2156(17) Uiso 1 1 d G . . H36 H -0.1079 0.2211 0.1742 0.259 Uiso 1 1 calc R . . C37 C -0.2290(16) 0.0845(12) 0.1092(10) 0.275(5) Uiso 1 1 d D . . H37A H -0.2781 0.1041 0.1132 0.413 Uiso 1 1 calc R . . H37B H -0.2365 0.0497 0.1202 0.413 Uiso 1 1 calc R . . H37C H -0.2163 0.0838 0.0766 0.413 Uiso 1 1 calc R . . C41 C 0.0865(11) 0.1552(9) 0.3858(6) 0.2156(17) Uiso 1 1 d GD . . C42 C 0.0609(12) 0.1824(6) 0.4235(9) 0.2156(17) Uiso 1 1 d G . . H42 H 0.0555 0.2184 0.4217 0.259 Uiso 1 1 calc R . . C43 C 0.0433(10) 0.1571(10) 0.4638(6) 0.2156(17) Uiso 1 1 d G . . H43 H 0.0259 0.1758 0.4895 0.259 Uiso 1 1 calc R . . C44 C 0.0513(11) 0.1046(10) 0.4664(6) 0.2156(17) Uiso 1 1 d GD . . C45 C 0.0769(12) 0.0773(6) 0.4287(9) 0.2156(17) Uiso 1 1 d G . . H45 H 0.0823 0.0414 0.4305 0.259 Uiso 1 1 calc R . . C46 C 0.0945(10) 0.1026(9) 0.3884(6) 0.2156(17) Uiso 1 1 d G . . H46 H 0.1119 0.0840 0.3627 0.259 Uiso 1 1 calc R . . C47 C 0.050(2) 0.0784(13) 0.5139(8) 0.275(5) Uiso 1 1 d D . . H47A H 0.0379 0.1036 0.5374 0.413 Uiso 1 1 calc R . . H47B H 0.1030 0.0635 0.5209 0.413 Uiso 1 1 calc R . . H47C H 0.0100 0.0515 0.5135 0.413 Uiso 1 1 calc R . . C51 C 0.2950(12) 0.1481(9) 0.4056(6) 0.2156(17) Uiso 1 1 d GD . . C52 C 0.3163(11) 0.0970(9) 0.4053(6) 0.2156(17) Uiso 1 1 d G . . H52 H 0.3307 0.0812 0.3775 0.259 Uiso 1 1 calc R . . C53 C 0.3165(11) 0.0691(6) 0.4457(9) 0.2156(17) Uiso 1 1 d G . . H53 H 0.3311 0.0342 0.4455 0.259 Uiso 1 1 calc R . . C54 C 0.2954(12) 0.0922(9) 0.4865(6) 0.2156(17) Uiso 1 1 d GD . . C55 C 0.2741(11) 0.1433(9) 0.4868(6) 0.2156(17) Uiso 1 1 d G . . H55 H 0.2597 0.1591 0.5146 0.259 Uiso 1 1 calc R . . C56 C 0.2739(11) 0.1713(6) 0.4463(9) 0.2156(17) Uiso 1 1 d G . . H56 H 0.2593 0.2062 0.4466 0.259 Uiso 1 1 calc R . . C57 C 0.280(2) 0.0642(12) 0.5318(9) 0.275(5) Uiso 1 1 d D . . H57A H 0.3230 0.0397 0.5381 0.413 Uiso 1 1 calc R . . H57B H 0.2290 0.0461 0.5292 0.413 Uiso 1 1 calc R . . H57C H 0.2782 0.0889 0.5569 0.413 Uiso 1 1 calc R . . C61 C 0.5175(10) 0.1402(9) 0.2536(7) 0.2156(17) Uiso 1 1 d GD . . C62 C 0.5238(11) 0.0912(9) 0.2711(6) 0.2156(17) Uiso 1 1 d G . . H62 H 0.4796 0.0760 0.2854 0.259 Uiso 1 1 calc R . . C63 C 0.5948(15) 0.0644(6) 0.2678(6) 0.2156(17) Uiso 1 1 d G . . H63 H 0.5990 0.0309 0.2798 0.259 Uiso 1 1 calc R . . C64 C 0.6595(10) 0.0866(9) 0.2469(7) 0.2156(17) Uiso 1 1 d GD . . C65 C 0.6532(11) 0.1356(9) 0.2293(6) 0.2156(17) Uiso 1 1 d G . . H65 H 0.6974 0.1508 0.2150 0.259 Uiso 1 1 calc R . . C66 C 0.5822(16) 0.1624(6) 0.2327(6) 0.2156(17) Uiso 1 1 d G . . H66 H 0.5779 0.1960 0.2207 0.259 Uiso 1 1 calc R . . C67 C 0.7263(17) 0.0476(12) 0.2464(10) 0.275(5) Uiso 1 1 d D . . H67A H 0.7776 0.0647 0.2521 0.413 Uiso 1 1 calc R . . H67B H 0.7265 0.0308 0.2164 0.413 Uiso 1 1 calc R . . H67C H 0.7181 0.0222 0.2703 0.413 Uiso 1 1 calc R . . C71 C 0.2992(12) 0.3425(9) 0.0734(6) 0.2156(17) Uiso 1 1 d GD . . C72 C 0.2791(11) 0.3938(10) 0.0743(6) 0.2156(17) Uiso 1 1 d G . . H72 H 0.2605 0.4086 0.1017 0.259 Uiso 1 1 calc R . . C73 C 0.2861(12) 0.4234(6) 0.0352(9) 0.2156(17) Uiso 1 1 d G . . H73 H 0.2723 0.4584 0.0358 0.259 Uiso 1 1 calc R . . C74 C 0.3133(12) 0.4017(9) -0.0049(6) 0.2156(17) Uiso 1 1 d GD . . C75 C 0.3334(10) 0.3504(10) -0.0058(6) 0.2156(17) Uiso 1 1 d G . . H75 H 0.3520 0.3356 -0.0332 0.259 Uiso 1 1 calc R . . C76 C 0.3264(11) 0.3209(6) 0.0333(9) 0.2156(17) Uiso 1 1 d G . . H76 H 0.3402 0.2858 0.0327 0.259 Uiso 1 1 calc R . . C77 C 0.330(2) 0.4333(12) -0.0479(9) 0.275(5) Uiso 1 1 d D . . H77A H 0.3786 0.4206 -0.0620 0.413 Uiso 1 1 calc R . . H77B H 0.3376 0.4691 -0.0393 0.413 Uiso 1 1 calc R . . H77C H 0.2850 0.4304 -0.0699 0.413 Uiso 1 1 calc R . . C81 C -0.0348(11) 0.3533(8) 0.3019(7) 0.2156(17) Uiso 1 1 d GD . . C82 C -0.0340(11) 0.4037(10) 0.2875(6) 0.2156(17) Uiso 1 1 d G . . H82 H 0.0085 0.4158 0.2696 0.259 Uiso 1 1 calc R . . C83 C -0.0953(15) 0.4363(6) 0.2992(7) 0.2156(17) Uiso 1 1 d G . . H83 H -0.0947 0.4708 0.2893 0.259 Uiso 1 1 calc R . . C84 C -0.1574(11) 0.4186(9) 0.3253(7) 0.2156(17) Uiso 1 1 d GD . . C85 C -0.1583(11) 0.3682(10) 0.3397(5) 0.2156(17) Uiso 1 1 d G . . H85 H -0.2007 0.3561 0.3575 0.259 Uiso 1 1 calc R . . C86 C -0.0970(15) 0.3355(6) 0.3280(7) 0.2156(17) Uiso 1 1 d G . . H86 H -0.0976 0.3011 0.3378 0.259 Uiso 1 1 calc R . . C87 C -0.2149(18) 0.4527(12) 0.3508(10) 0.275(5) Uiso 1 1 d D . . H87A H -0.2392 0.4772 0.3293 0.413 Uiso 1 1 calc R . . H87B H -0.1857 0.4710 0.3752 0.413 Uiso 1 1 calc R . . H87C H -0.2566 0.4318 0.3641 0.413 Uiso 1 1 calc R . . C91 C 0.4831(11) 0.3392(9) 0.3569(7) 0.2156(17) Uiso 1 1 d GD . . C92 C 0.4860(11) 0.3918(10) 0.3524(6) 0.2156(17) Uiso 1 1 d G . . H92 H 0.4526 0.4084 0.3303 0.259 Uiso 1 1 calc R . . C93 C 0.5379(14) 0.4200(6) 0.3804(8) 0.2156(17) Uiso 1 1 d G . . H93 H 0.5398 0.4560 0.3773 0.259 Uiso 1 1 calc R . . C94 C 0.5868(11) 0.3957(9) 0.4128(6) 0.2156(17) Uiso 1 1 d GD . . C95 C 0.5839(11) 0.3431(10) 0.4172(6) 0.2156(17) Uiso 1 1 d G . . H95 H 0.6174 0.3265 0.4394 0.259 Uiso 1 1 calc R . . C96 C 0.5321(14) 0.3148(6) 0.3893(8) 0.2156(17) Uiso 1 1 d G . . H96 H 0.5301 0.2789 0.3923 0.259 Uiso 1 1 calc R . . C97 C 0.6427(19) 0.4309(12) 0.4396(11) 0.275(5) Uiso 1 1 d D . . H97A H 0.6837 0.4437 0.4193 0.413 Uiso 1 1 calc R . . H97B H 0.6682 0.4121 0.4651 0.413 Uiso 1 1 calc R . . H97C H 0.6124 0.4595 0.4517 0.413 Uiso 1 1 calc R . . C101 C 0.0746(13) 0.4284(8) 0.1659(6) 0.2156(17) Uiso 1 1 d GD . . C102 C 0.0997(9) 0.4730(10) 0.1452(7) 0.2156(17) Uiso 1 1 d G . . H102 H 0.1550 0.4796 0.1425 0.259 Uiso 1 1 calc R . . C103 C 0.0439(16) 0.5079(6) 0.1284(6) 0.2156(17) Uiso 1 1 d G . . H103 H 0.0610 0.5383 0.1143 0.259 Uiso 1 1 calc R . . C104 C -0.0371(13) 0.4982(8) 0.1324(6) 0.2156(17) Uiso 1 1 d GD . . C105 C -0.0622(9) 0.4536(10) 0.1531(7) 0.2156(17) Uiso 1 1 d G . . H105 H -0.1175 0.4469 0.1558 0.259 Uiso 1 1 calc R . . C106 C -0.0063(16) 0.4187(6) 0.1699(6) 0.2156(17) Uiso 1 1 d G . . H106 H -0.0235 0.3882 0.1840 0.259 Uiso 1 1 calc R . . C107 C -0.0945(18) 0.5362(11) 0.1063(10) 0.275(5) Uiso 1 1 d D . . H10A H -0.0872 0.5704 0.1190 0.413 Uiso 1 1 calc R . . H10B H -0.1498 0.5254 0.1099 0.413 Uiso 1 1 calc R . . H10C H -0.0823 0.5365 0.0736 0.413 Uiso 1 1 calc R . . C111 C 0.2153(16) 0.4275(6) 0.3626(5) 0.2156(17) Uiso 1 1 d GD . . C112 C 0.1414(12) 0.4456(8) 0.3755(7) 0.2156(17) Uiso 1 1 d G . . H112 H 0.0946 0.4364 0.3583 0.259 Uiso 1 1 calc R . . C113 C 0.1359(11) 0.4770(8) 0.4135(8) 0.2156(17) Uiso 1 1 d G . . H113 H 0.0854 0.4894 0.4224 0.259 Uiso 1 1 calc R . . C114 C 0.2043(17) 0.4905(6) 0.4387(5) 0.2156(17) Uiso 1 1 d GD . . C115 C 0.2782(12) 0.4724(8) 0.4258(7) 0.2156(17) Uiso 1 1 d G . . H115 H 0.3250 0.4816 0.4430 0.259 Uiso 1 1 calc R . . C116 C 0.2837(11) 0.4409(8) 0.3877(8) 0.2156(17) Uiso 1 1 d G . . H116 H 0.3342 0.4286 0.3789 0.259 Uiso 1 1 calc R . . C117 C 0.192(2) 0.5337(11) 0.4730(10) 0.275(5) Uiso 1 1 d D . . H11A H 0.2198 0.5254 0.5021 0.413 Uiso 1 1 calc R . . H11B H 0.1352 0.5380 0.4781 0.413 Uiso 1 1 calc R . . H11C H 0.2141 0.5653 0.4607 0.413 Uiso 1 1 calc R . . C121 C 0.4451(10) 0.4230(7) 0.2021(9) 0.2156(17) Uiso 1 1 d GD . . C122 C 0.5084(15) 0.4363(8) 0.2315(5) 0.2156(17) Uiso 1 1 d G . . H122 H 0.5065 0.4287 0.2632 0.259 Uiso 1 1 calc R . . C123 C 0.5746(11) 0.4609(8) 0.2143(8) 0.2156(17) Uiso 1 1 d G . . H123 H 0.6179 0.4700 0.2344 0.259 Uiso 1 1 calc R . . C124 C 0.5774(10) 0.4721(7) 0.1679(9) 0.2156(17) Uiso 1 1 d GD . . C125 C 0.5141(15) 0.4587(8) 0.1385(5) 0.2156(17) Uiso 1 1 d G . . H125 H 0.5160 0.4664 0.1067 0.259 Uiso 1 1 calc R . . C126 C 0.4479(11) 0.4342(7) 0.1556(8) 0.2156(17) Uiso 1 1 d G . . H126 H 0.4046 0.4251 0.1356 0.259 Uiso 1 1 calc R . . C127 C 0.6509(16) 0.5022(12) 0.1520(11) 0.275(5) Uiso 1 1 d D . . H12A H 0.6382 0.5386 0.1510 0.413 Uiso 1 1 calc R . . H12B H 0.6652 0.4907 0.1213 0.413 Uiso 1 1 calc R . . H12C H 0.6959 0.4964 0.1735 0.413 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ba1 0.1835(15) 0.0919(10) 0.1427(13) -0.0022(9) -0.0097(10) 0.0015(9) Sb1 0.1688(16) 0.1010(10) 0.1288(13) -0.0068(9) -0.0090(11) 0.0009(10) Sb2 0.1774(16) 0.0885(9) 0.1301(13) -0.0080(9) -0.0321(11) -0.0074(9) Sb3 0.1575(15) 0.0918(10) 0.1556(15) -0.0038(9) -0.0253(11) -0.0150(9) Sb4 0.1665(15) 0.0948(10) 0.1320(13) 0.0022(9) -0.0050(11) -0.0135(9) Sb5 0.1753(16) 0.0904(9) 0.1212(12) 0.0064(9) -0.0127(11) -0.0027(9) Sb6 0.1526(14) 0.0995(10) 0.1348(13) 0.0033(9) -0.0087(10) 0.0060(9) Sb7 0.1716(15) 0.0965(10) 0.1175(12) -0.0026(9) -0.0177(10) -0.0096(9) Sb8 0.1458(14) 0.0940(10) 0.1432(14) -0.0058(9) -0.0095(10) -0.0090(9) Sb9 0.1560(15) 0.0977(10) 0.1219(13) -0.0014(9) -0.0219(10) -0.0045(9) Sb10 0.1588(15) 0.0871(9) 0.1296(13) -0.0028(9) -0.0236(10) -0.0090(9) Sb11 0.1551(14) 0.0854(9) 0.1234(12) -0.0046(8) -0.0117(10) -0.0063(9) Sb12 0.1600(14) 0.0903(9) 0.1218(12) -0.0039(8) -0.0123(10) -0.0122(9) Co1 0.137(3) 0.091(2) 0.133(3) -0.002(2) -0.020(2) -0.0061(19) _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 Ba1 O5 2.693(14) . ? Ba1 O4 2.739(12) . ? Ba1 O2 2.769(13) . ? Ba1 OW4 2.876(17) . ? Ba1 OW1 2.880(16) . ? Ba1 OW2 2.902(15) . ? Ba1 OW3 2.904(17) . ? Ba1 OW5 3.17(2) . ? Sb1 O1 1.910(13) . ? Sb1 O18 1.963(13) . ? Sb1 O5 1.975(13) . ? Sb1 O16 2.080(13) . ? Sb1 C11 2.103(12) . ? Sb1 O17 2.184(11) . ? Sb1 Sb6 3.148(2) . ? Sb1 Sb2 3.223(2) . ? Sb1 Sb7 3.234(2) . ? Sb2 O2 1.967(13) . ? Sb2 O6 1.971(12) . ? Sb2 O1 2.008(13) . ? Sb2 O8 2.051(12) . ? Sb2 C21 2.093(13) . ? Sb2 O17 2.194(12) . ? Sb2 Sb3 3.156(3) . ? Sb2 Sb7 3.221(2) . ? Sb3 O9 1.928(12) . ? Sb3 O3 1.953(14) . ? Sb3 O2 2.023(13) . ? Sb3 O8 2.063(12) . ? Sb3 C31 2.106(13) . ? Sb3 O15 2.241(13) . ? Sb3 Sb4 3.217(2) . ? Sb3 Sb8 3.232(2) . ? Sb4 O4 1.968(12) . ? Sb4 O10 1.982(13) . ? Sb4 O3 1.987(14) . ? Sb4 C41 2.084(12) . ? Sb4 O11 2.106(11) . ? Sb4 O15 2.202(13) . ? Sb4 Sb5 3.169(2) . ? Sb4 Sb8 3.228(2) . ? Sb5 O4 1.959(12) . ? Sb5 O7 1.969(12) . ? Sb5 O12 1.990(12) . ? Sb5 C51 2.082(12) . ? Sb5 O11 2.091(11) . ? Sb5 O14 2.194(11) . ? Sb5 Sb6 3.212(2) . ? Sb5 Sb9 3.234(2) . ? Sb6 O7 1.975(12) . ? Sb6 O13 1.991(15) . ? Sb6 O16 2.005(13) . ? Sb6 O5 2.021(14) . ? Sb6 C61 2.074(13) . ? Sb6 O14 2.197(11) . ? Sb6 Sb9 3.241(2) . ? Sb7 O18 1.987(13) . ? Sb7 O6 2.008(12) . ? Sb7 O19 2.010(12) . ? Sb7 O25 2.047(13) . ? Sb7 C71 2.074(13) . ? Sb7 O17 2.137(11) . ? Sb8 O21 1.955(13) . ? Sb8 O20 1.980(12) . ? Sb8 O10 1.994(13) . ? Sb8 O9 2.046(12) . ? Sb8 C81 2.064(12) . ? Sb8 O15 2.174(13) . ? Sb9 O22 1.941(12) . ? Sb9 O23 1.963(13) . ? Sb9 O12 1.976(12) . ? Sb9 O13 2.039(14) . ? Sb9 C91 2.130(13) . ? Sb9 O14 2.140(11) . ? Sb10 O19 1.915(13) . ? Sb10 O20 1.977(12) . ? Sb10 O27 1.994(13) . ? Sb10 O26 2.035(14) . ? Sb10 C101 2.129(12) . ? Sb10 O24 2.249(10) . ? Sb10 Sb11 3.196(2) . ? Sb10 Sb12 3.198(2) . ? Sb11 O27 1.956(13) . ? Sb11 O21 2.001(13) . ? Sb11 O22 2.015(13) . ? Sb11 O28 2.015(13) . ? Sb11 C111 2.101(12) . ? Sb11 O24 2.207(10) . ? Sb11 Sb12 3.189(2) . ? Sb12 O28 1.957(13) . ? Sb12 O26 1.975(14) . ? Sb12 O25 1.987(13) . ? Sb12 O23 2.040(13) . ? Sb12 C121 2.100(12) . ? Sb12 O24 2.157(10) . ? Co1 O24 1.885(11) . ? Co1 O15 1.932(13) . ? Co1 O17 1.983(12) . ? Co1 O14 1.995(12) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C14 C17 1.495(17) . ? C15 C16 1.3900 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C24 C27 1.518(17) . ? C25 C26 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C34 C37 1.500(17) . ? C35 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C44 C47 1.548(17) . ? C45 C46 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C54 C57 1.541(17) . ? C55 C56 1.3900 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C64 C67 1.521(18) . ? C65 C66 1.3900 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C74 C77 1.538(17) . ? C75 C76 1.3900 . ? C81 C82 1.3900 . ? C81 C86 1.3900 . ? C82 C83 1.3900 . ? C83 C84 1.3900 . ? C84 C85 1.3900 . ? C84 C87 1.526(17) . ? C85 C86 1.3900 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C92 C93 1.3900 . ? C93 C94 1.3900 . ? C94 C95 1.3900 . ? C94 C97 1.518(18) . ? C95 C96 1.3900 . ? C101 C102 1.3900 . ? C101 C106 1.3900 . ? C102 C103 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C104 C107 1.570(17) . ? C105 C106 1.3900 . ? C111 C112 1.3900 . ? C111 C116 1.3900 . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C114 C117 1.532(17) . ? C115 C116 1.3900 . ? C121 C122 1.3900 . ? C121 C126 1.3900 . ? C122 C123 1.3900 . ? C123 C124 1.3900 . ? C124 C125 1.3900 . ? C124 C127 1.549(17) . ? C125 C126 1.3900 . ? 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 O5 Ba1 O4 82.6(4) . . ? O5 Ba1 O2 76.8(4) . . ? O4 Ba1 O2 79.8(4) . . ? O5 Ba1 OW4 75.1(5) . . ? O4 Ba1 OW4 152.6(5) . . ? O2 Ba1 OW4 79.8(5) . . ? O5 Ba1 OW1 136.0(4) . . ? O4 Ba1 OW1 134.8(4) . . ? O2 Ba1 OW1 87.2(4) . . ? OW4 Ba1 OW1 61.7(5) . . ? O5 Ba1 OW2 136.0(4) . . ? O4 Ba1 OW2 82.8(4) . . ? O2 Ba1 OW2 139.9(4) . . ? OW4 Ba1 OW2 124.4(4) . . ? OW1 Ba1 OW2 80.1(4) . . ? O5 Ba1 OW3 82.0(4) . . ? O4 Ba1 OW3 128.9(4) . . ? O2 Ba1 OW3 141.5(4) . . ? OW4 Ba1 OW3 63.9(5) . . ? OW1 Ba1 OW3 86.2(5) . . ? OW2 Ba1 OW3 75.6(4) . . ? O5 Ba1 OW5 152.4(5) . . ? O4 Ba1 OW5 76.3(5) . . ? O2 Ba1 OW5 82.1(5) . . ? OW4 Ba1 OW5 118.4(6) . . ? OW1 Ba1 OW5 59.1(5) . . ? OW2 Ba1 OW5 58.8(5) . . ? OW3 Ba1 OW5 125.2(5) . . ? O1 Sb1 O18 99.0(5) . . ? O1 Sb1 O5 90.3(6) . . ? O18 Sb1 O5 158.5(5) . . ? O1 Sb1 O16 163.0(5) . . ? O18 Sb1 O16 89.5(5) . . ? O5 Sb1 O16 77.1(5) . . ? O1 Sb1 C11 93.5(6) . . ? O18 Sb1 C11 97.6(8) . . ? O5 Sb1 C11 101.2(8) . . ? O16 Sb1 C11 100.0(6) . . ? O1 Sb1 O17 78.2(5) . . ? O18 Sb1 O17 76.3(5) . . ? O5 Sb1 O17 86.9(5) . . ? O16 Sb1 O17 89.7(5) . . ? C11 Sb1 O17 168.5(7) . . ? O1 Sb1 Sb6 128.5(4) . . ? O18 Sb1 Sb6 127.2(4) . . ? O5 Sb1 Sb6 38.5(4) . . ? O16 Sb1 Sb6 38.7(4) . . ? C11 Sb1 Sb6 100.7(6) . . ? O17 Sb1 Sb6 90.7(3) . . ? O1 Sb1 Sb2 35.7(4) . . ? O18 Sb1 Sb2 85.1(4) . . ? O5 Sb1 Sb2 91.4(4) . . ? O16 Sb1 Sb2 132.0(4) . . ? C11 Sb1 Sb2 128.0(5) . . ? O17 Sb1 Sb2 42.7(3) . . ? Sb6 Sb1 Sb2 118.66(7) . . ? O1 Sb1 Sb7 88.4(4) . . ? O18 Sb1 Sb7 35.3(4) . . ? O5 Sb1 Sb7 126.8(4) . . ? O16 Sb1 Sb7 90.2(4) . . ? C11 Sb1 Sb7 132.0(8) . . ? O17 Sb1 Sb7 41.0(3) . . ? Sb6 Sb1 Sb7 115.18(6) . . ? Sb2 Sb1 Sb7 59.84(5) . . ? O2 Sb2 O6 161.0(5) . . ? O2 Sb2 O1 92.1(5) . . ? O6 Sb2 O1 96.7(5) . . ? O2 Sb2 O8 77.9(5) . . ? O6 Sb2 O8 88.9(5) . . ? O1 Sb2 O8 161.9(5) . . ? O2 Sb2 C21 95.1(7) . . ? O6 Sb2 C21 99.7(7) . . ? O1 Sb2 C21 100.4(8) . . ? O8 Sb2 C21 95.6(7) . . ? O2 Sb2 O17 88.4(5) . . ? O6 Sb2 O17 77.6(5) . . ? O1 Sb2 O17 75.9(5) . . ? O8 Sb2 O17 88.6(4) . . ? C21 Sb2 O17 175.0(6) . . ? O2 Sb2 Sb3 38.4(4) . . ? O6 Sb2 Sb3 128.6(3) . . ? O1 Sb2 Sb3 130.0(4) . . ? O8 Sb2 Sb3 40.0(3) . . ? C21 Sb2 Sb3 92.3(5) . . ? O17 Sb2 Sb3 92.7(3) . . ? O2 Sb2 Sb7 128.1(4) . . ? O6 Sb2 Sb7 36.4(3) . . ? O1 Sb2 Sb7 87.1(4) . . ? O8 Sb2 Sb7 87.3(3) . . ? C21 Sb2 Sb7 136.0(6) . . ? O17 Sb2 Sb7 41.3(3) . . ? Sb3 Sb2 Sb7 115.78(6) . . ? O2 Sb2 Sb1 93.5(4) . . ? O6 Sb2 Sb1 84.8(3) . . ? O1 Sb2 Sb1 33.7(4) . . ? O8 Sb2 Sb1 130.9(3) . . ? C21 Sb2 Sb1 133.5(7) . . ? O17 Sb2 Sb1 42.5(3) . . ? Sb3 Sb2 Sb1 120.82(6) . . ? Sb7 Sb2 Sb1 60.25(5) . . ? O9 Sb3 O3 95.7(5) . . ? O9 Sb3 O2 160.7(5) . . ? O3 Sb3 O2 94.1(5) . . ? O9 Sb3 O8 89.8(5) . . ? O3 Sb3 O8 163.2(5) . . ? O2 Sb3 O8 76.4(5) . . ? O9 Sb3 C31 96.8(8) . . ? O3 Sb3 C31 98.0(7) . . ? O2 Sb3 C31 98.2(8) . . ? O8 Sb3 C31 97.1(7) . . ? O9 Sb3 O15 78.9(5) . . ? O3 Sb3 O15 78.5(5) . . ? O2 Sb3 O15 86.8(5) . . ? O8 Sb3 O15 87.1(5) . . ? C31 Sb3 O15 174.1(6) . . ? O9 Sb3 Sb2 129.2(4) . . ? O3 Sb3 Sb2 130.9(4) . . ? O2 Sb3 Sb2 37.1(4) . . ? O8 Sb3 Sb2 39.8(3) . . ? C31 Sb3 Sb2 95.3(5) . . ? O15 Sb3 Sb2 90.6(3) . . ? O9 Sb3 Sb4 84.0(4) . . ? O3 Sb3 Sb4 35.6(4) . . ? O2 Sb3 Sb4 94.5(4) . . ? O8 Sb3 Sb4 130.1(3) . . ? C31 Sb3 Sb4 132.8(6) . . ? O15 Sb3 Sb4 43.1(3) . . ? Sb2 Sb3 Sb4 120.48(7) . . ? O9 Sb3 Sb8 36.8(4) . . ? O3 Sb3 Sb8 88.3(4) . . ? O2 Sb3 Sb8 127.2(4) . . ? O8 Sb3 Sb8 86.6(3) . . ? C31 Sb3 Sb8 133.6(7) . . ? O15 Sb3 Sb8 42.1(3) . . ? Sb2 Sb3 Sb8 114.77(6) . . ? Sb4 Sb3 Sb8 60.08(5) . . ? O4 Sb4 O10 160.3(5) . . ? O4 Sb4 O3 93.4(5) . . ? O10 Sb4 O3 97.0(5) . . ? O4 Sb4 C41 96.0(8) . . ? O10 Sb4 C41 98.7(8) . . ? O3 Sb4 C41 99.3(7) . . ? O4 Sb4 O11 76.8(5) . . ? O10 Sb4 O11 88.9(5) . . ? O3 Sb4 O11 163.5(5) . . ? C41 Sb4 O11 94.9(7) . . ? O4 Sb4 O15 87.7(5) . . ? O10 Sb4 O15 78.0(5) . . ? O3 Sb4 O15 78.8(5) . . ? C41 Sb4 O15 175.9(7) . . ? O11 Sb4 O15 87.5(5) . . ? O4 Sb4 Sb5 36.1(4) . . ? O10 Sb4 Sb5 128.8(4) . . ? O3 Sb4 Sb5 128.8(4) . . ? C41 Sb4 Sb5 95.1(5) . . ? O11 Sb4 Sb5 40.8(3) . . ? O15 Sb4 Sb5 88.9(3) . . ? O4 Sb4 Sb3 94.6(4) . . ? O10 Sb4 Sb3 84.6(4) . . ? O3 Sb4 Sb3 34.9(4) . . ? C41 Sb4 Sb3 133.6(6) . . ? O11 Sb4 Sb3 131.5(3) . . ? O15 Sb4 Sb3 44.1(3) . . ? Sb5 Sb4 Sb3 118.60(7) . . ? O4 Sb4 Sb8 128.5(4) . . ? O10 Sb4 Sb8 35.8(4) . . ? O3 Sb4 Sb8 87.9(4) . . ? C41 Sb4 Sb8 134.5(7) . . ? O11 Sb4 Sb8 88.0(3) . . ? O15 Sb4 Sb8 42.1(3) . . ? Sb5 Sb4 Sb8 114.96(6) . . ? Sb3 Sb4 Sb8 60.19(5) . . ? O4 Sb5 O7 92.5(5) . . ? O4 Sb5 O12 161.0(5) . . ? O7 Sb5 O12 98.1(5) . . ? O4 Sb5 C51 95.3(7) . . ? O7 Sb5 C51 97.9(8) . . ? O12 Sb5 C51 98.7(7) . . ? O4 Sb5 O11 77.4(5) . . ? O7 Sb5 O11 163.9(5) . . ? O12 Sb5 O11 88.7(5) . . ? C51 Sb5 O11 95.4(8) . . ? O4 Sb5 O14 90.7(5) . . ? O7 Sb5 O14 78.1(5) . . ? O12 Sb5 O14 76.2(5) . . ? C51 Sb5 O14 172.9(6) . . ? O11 Sb5 O14 89.5(4) . . ? O4 Sb5 Sb4 36.3(4) . . ? O7 Sb5 Sb4 128.2(4) . . ? O12 Sb5 Sb4 129.1(4) . . ? C51 Sb5 Sb4 94.9(6) . . ? O11 Sb5 Sb4 41.2(3) . . ? O14 Sb5 Sb4 92.1(3) . . ? O4 Sb5 Sb6 96.6(3) . . ? O7 Sb5 Sb6 35.5(4) . . ? O12 Sb5 Sb6 83.3(4) . . ? C51 Sb5 Sb6 132.2(7) . . ? O11 Sb5 Sb6 132.4(3) . . ? O14 Sb5 Sb6 43.0(3) . . ? Sb4 Sb5 Sb6 120.71(6) . . ? O4 Sb5 Sb9 129.8(4) . . ? O7 Sb5 Sb9 89.9(4) . . ? O12 Sb5 Sb9 35.2(4) . . ? C51 Sb5 Sb9 133.9(6) . . ? O11 Sb5 Sb9 87.3(3) . . ? O14 Sb5 Sb9 41.1(3) . . ? Sb4 Sb5 Sb9 115.30(6) . . ? Sb6 Sb5 Sb9 60.37(5) . . ? O7 Sb6 O13 98.5(6) . . ? O7 Sb6 O16 164.1(5) . . ? O13 Sb6 O16 89.4(6) . . ? O7 Sb6 O5 91.0(5) . . ? O13 Sb6 O5 161.2(6) . . ? O16 Sb6 O5 77.8(5) . . ? O7 Sb6 C61 93.9(8) . . ? O13 Sb6 C61 96.7(7) . . ? O16 Sb6 C61 98.9(8) . . ? O5 Sb6 C61 98.8(7) . . ? O7 Sb6 O14 77.9(5) . . ? O13 Sb6 O14 77.9(5) . . ? O16 Sb6 O14 90.4(5) . . ? O5 Sb6 O14 88.4(5) . . ? C61 Sb6 O14 169.3(6) . . ? O7 Sb6 Sb1 128.2(4) . . ? O13 Sb6 Sb1 129.2(4) . . ? O16 Sb6 Sb1 40.5(4) . . ? O5 Sb6 Sb1 37.5(4) . . ? C61 Sb6 Sb1 98.4(5) . . ? O14 Sb6 Sb1 92.1(3) . . ? O7 Sb6 Sb5 35.4(4) . . ? O13 Sb6 Sb5 84.5(4) . . ? O16 Sb6 Sb5 133.2(4) . . ? O5 Sb6 Sb5 94.2(4) . . ? C61 Sb6 Sb5 127.9(7) . . ? O14 Sb6 Sb5 42.9(3) . . ? Sb1 Sb6 Sb5 120.72(7) . . ? O7 Sb6 Sb9 89.6(4) . . ? O13 Sb6 Sb9 37.0(4) . . ? O16 Sb6 Sb9 88.5(4) . . ? O5 Sb6 Sb9 127.7(4) . . ? C61 Sb6 Sb9 133.3(6) . . ? O14 Sb6 Sb9 41.0(3) . . ? Sb1 Sb6 Sb9 115.34(6) . . ? Sb5 Sb6 Sb9 60.15(5) . . ? O18 Sb7 O6 92.2(5) . . ? O18 Sb7 O19 164.6(5) . . ? O6 Sb7 O19 86.4(5) . . ? O18 Sb7 O25 81.1(5) . . ? O6 Sb7 O25 162.3(5) . . ? O19 Sb7 O25 95.7(5) . . ? O18 Sb7 C71 93.3(8) . . ? O6 Sb7 C71 99.7(7) . . ? O19 Sb7 C71 102.0(8) . . ? O25 Sb7 C71 97.0(7) . . ? O18 Sb7 O17 76.9(5) . . ? O6 Sb7 O17 78.2(5) . . ? O19 Sb7 O17 87.9(5) . . ? O25 Sb7 O17 84.4(5) . . ? C71 Sb7 O17 169.8(8) . . ? O18 Sb7 Sb2 84.8(4) . . ? O6 Sb7 Sb2 35.6(3) . . ? O19 Sb7 Sb2 85.2(4) . . ? O25 Sb7 Sb2 127.0(4) . . ? C71 Sb7 Sb2 134.8(6) . . ? O17 Sb7 Sb2 42.6(3) . . ? O18 Sb7 Sb1 34.8(4) . . ? O6 Sb7 Sb1 83.9(3) . . ? O19 Sb7 Sb1 130.0(4) . . ? O25 Sb7 Sb1 81.2(4) . . ? C71 Sb7 Sb1 128.0(7) . . ? O17 Sb7 Sb1 42.1(3) . . ? Sb2 Sb7 Sb1 59.91(5) . . ? O21 Sb8 O20 94.6(5) . . ? O21 Sb8 O10 84.7(5) . . ? O20 Sb8 O10 164.4(5) . . ? O21 Sb8 O9 160.9(5) . . ? O20 Sb8 O9 86.6(5) . . ? O10 Sb8 O9 89.0(5) . . ? O21 Sb8 C81 99.0(7) . . ? O20 Sb8 C81 98.7(8) . . ? O10 Sb8 C81 96.8(8) . . ? O9 Sb8 C81 99.7(7) . . ? O21 Sb8 O15 82.9(5) . . ? O20 Sb8 O15 86.0(5) . . ? O10 Sb8 O15 78.4(5) . . ? O9 Sb8 O15 78.1(5) . . ? C81 Sb8 O15 174.7(8) . . ? O21 Sb8 Sb4 82.4(4) . . ? O20 Sb8 Sb4 128.8(4) . . ? O10 Sb8 Sb4 35.6(4) . . ? O9 Sb8 Sb4 82.0(3) . . ? C81 Sb8 Sb4 132.4(7) . . ? O15 Sb8 Sb4 42.8(3) . . ? O21 Sb8 Sb3 126.7(4) . . ? O20 Sb8 Sb3 83.9(4) . . ? O10 Sb8 Sb3 84.1(4) . . ? O9 Sb8 Sb3 34.4(3) . . ? C81 Sb8 Sb3 134.1(6) . . ? O15 Sb8 Sb3 43.8(3) . . ? Sb4 Sb8 Sb3 59.73(5) . . ? O22 Sb9 O23 96.2(5) . . ? O22 Sb9 O12 86.7(5) . . ? O23 Sb9 O12 165.4(5) . . ? O22 Sb9 O13 165.6(5) . . ? O23 Sb9 O13 85.7(5) . . ? O12 Sb9 O13 88.0(5) . . ? O22 Sb9 C91 98.6(7) . . ? O23 Sb9 C91 96.5(7) . . ? O12 Sb9 C91 97.2(8) . . ? O13 Sb9 C91 95.3(8) . . ? O22 Sb9 O14 87.6(5) . . ? O23 Sb9 O14 88.0(5) . . ? O12 Sb9 O14 77.8(5) . . ? O13 Sb9 O14 78.2(5) . . ? C91 Sb9 O14 171.9(8) . . ? O22 Sb9 Sb5 84.7(4) . . ? O23 Sb9 Sb5 130.3(4) . . ? O12 Sb9 Sb5 35.5(4) . . ? O13 Sb9 Sb5 83.2(4) . . ? C91 Sb9 Sb5 132.7(7) . . ? O14 Sb9 Sb5 42.4(3) . . ? O22 Sb9 Sb6 129.9(4) . . ? O23 Sb9 Sb6 84.5(4) . . ? O12 Sb9 Sb6 82.7(3) . . ? O13 Sb9 Sb6 35.9(4) . . ? C91 Sb9 Sb6 131.3(6) . . ? O14 Sb9 Sb6 42.3(3) . . ? Sb5 Sb9 Sb6 59.48(5) . . ? O19 Sb10 O20 85.6(5) . . ? O19 Sb10 O27 162.4(5) . . ? O20 Sb10 O27 89.7(5) . . ? O19 Sb10 O26 91.1(5) . . ? O20 Sb10 O26 163.1(5) . . ? O27 Sb10 O26 88.5(5) . . ? O19 Sb10 C101 98.5(6) . . ? O20 Sb10 C101 94.2(9) . . ? O27 Sb10 C101 98.8(6) . . ? O26 Sb10 C101 102.7(9) . . ? O19 Sb10 O24 83.4(5) . . ? O20 Sb10 O24 84.3(4) . . ? O27 Sb10 O24 79.2(5) . . ? O26 Sb10 O24 78.8(5) . . ? C101 Sb10 O24 177.5(6) . . ? O19 Sb10 Sb11 126.9(4) . . ? O20 Sb10 Sb11 85.3(4) . . ? O27 Sb10 Sb11 35.6(4) . . ? O26 Sb10 Sb11 83.5(4) . . ? C101 Sb10 Sb11 134.3(5) . . ? O24 Sb10 Sb11 43.6(2) . . ? O19 Sb10 Sb12 85.6(4) . . ? O20 Sb10 Sb12 126.6(4) . . ? O27 Sb10 Sb12 83.5(4) . . ? O26 Sb10 Sb12 36.5(4) . . ? C101 Sb10 Sb12 139.2(8) . . ? O24 Sb10 Sb12 42.3(3) . . ? Sb11 Sb10 Sb12 59.83(5) . . ? O27 Sb11 O21 90.8(5) . . ? O27 Sb11 O22 165.0(5) . . ? O21 Sb11 O22 85.4(5) . . ? O27 Sb11 O28 91.2(5) . . ? O21 Sb11 O28 162.1(5) . . ? O22 Sb11 O28 88.0(5) . . ? O27 Sb11 C111 97.4(8) . . ? O21 Sb11 C111 98.8(7) . . ? O22 Sb11 C111 97.6(7) . . ? O28 Sb11 C111 98.6(8) . . ? O27 Sb11 O24 81.0(5) . . ? O21 Sb11 O24 84.4(4) . . ? O22 Sb11 O24 84.1(4) . . ? O28 Sb11 O24 78.4(5) . . ? C111 Sb11 O24 176.6(6) . . ? O27 Sb11 Sb12 84.3(4) . . ? O21 Sb11 Sb12 126.7(4) . . ? O22 Sb11 Sb12 86.2(3) . . ? O28 Sb11 Sb12 36.0(4) . . ? C111 Sb11 Sb12 134.5(7) . . ? O24 Sb11 Sb12 42.4(3) . . ? O27 Sb11 Sb10 36.4(4) . . ? O21 Sb11 Sb10 86.0(4) . . ? O22 Sb11 Sb10 128.6(4) . . ? O28 Sb11 Sb10 85.1(4) . . ? C111 Sb11 Sb10 133.8(6) . . ? O24 Sb11 Sb10 44.7(3) . . ? Sb12 Sb11 Sb10 60.11(5) . . ? O28 Sb12 O26 90.7(6) . . ? O28 Sb12 O25 162.7(5) . . ? O26 Sb12 O25 95.2(6) . . ? O28 Sb12 O23 87.8(5) . . ? O26 Sb12 O23 166.0(5) . . ? O25 Sb12 O23 82.6(5) . . ? O28 Sb12 C121 98.1(7) . . ? O26 Sb12 C121 96.6(8) . . ? O25 Sb12 C121 97.4(7) . . ? O23 Sb12 C121 97.4(7) . . ? O28 Sb12 O24 80.9(5) . . ? O26 Sb12 O24 82.4(5) . . ? O25 Sb12 O24 83.8(5) . . ? O23 Sb12 O24 83.7(5) . . ? C121 Sb12 O24 178.5(6) . . ? O28 Sb12 Sb11 37.2(4) . . ? O26 Sb12 Sb11 84.6(4) . . ? O25 Sb12 Sb11 127.2(4) . . ? O23 Sb12 Sb11 85.8(4) . . ? C121 Sb12 Sb11 135.3(6) . . ? O24 Sb12 Sb11 43.7(3) . . ? O28 Sb12 Sb10 86.0(4) . . ? O26 Sb12 Sb10 37.8(4) . . ? O25 Sb12 Sb10 88.7(4) . . ? O23 Sb12 Sb10 128.2(4) . . ? C121 Sb12 Sb10 134.3(6) . . ? O24 Sb12 Sb10 44.6(3) . . ? Sb11 Sb12 Sb10 60.06(5) . . ? O24 Co1 O15 110.4(5) . . ? O24 Co1 O17 107.0(5) . . ? O15 Co1 O17 113.9(5) . . ? O24 Co1 O14 105.8(5) . . ? O15 Co1 O14 109.5(5) . . ? O17 Co1 O14 109.9(5) . . ? Sb1 O1 Sb2 110.7(6) . . ? Sb2 O2 Sb3 104.5(6) . . ? Sb2 O2 Ba1 129.1(6) . . ? Sb3 O2 Ba1 125.3(5) . . ? Sb3 O3 Sb4 109.4(7) . . ? Sb5 O4 Sb4 107.6(6) . . ? Sb5 O4 Ba1 122.6(5) . . ? Sb4 O4 Ba1 128.0(6) . . ? Sb1 O5 Sb6 104.0(6) . . ? Sb1 O5 Ba1 132.1(6) . . ? Sb6 O5 Ba1 123.2(6) . . ? Sb2 O6 Sb7 108.1(6) . . ? Sb5 O7 Sb6 109.1(6) . . ? Sb2 O8 Sb3 100.2(5) . . ? Sb3 O9 Sb8 108.8(6) . . ? Sb4 O10 Sb8 108.5(6) . . ? Sb5 O11 Sb4 98.1(4) . . ? Sb9 O12 Sb5 109.3(6) . . ? Sb6 O13 Sb9 107.1(7) . . ? Co1 O14 Sb9 118.0(5) . . ? Co1 O14 Sb5 122.7(5) . . ? Sb9 O14 Sb5 96.5(4) . . ? Co1 O14 Sb6 122.5(5) . . ? Sb9 O14 Sb6 96.7(4) . . ? Sb5 O14 Sb6 94.0(4) . . ? Co1 O15 Sb8 118.2(6) . . ? Co1 O15 Sb4 126.8(6) . . ? Sb8 O15 Sb4 95.1(5) . . ? Co1 O15 Sb3 122.0(6) . . ? Sb8 O15 Sb3 94.1(5) . . ? Sb4 O15 Sb3 92.8(5) . . ? Sb6 O16 Sb1 100.8(6) . . ? Co1 O17 Sb7 117.4(6) . . ? Co1 O17 Sb1 124.6(6) . . ? Sb7 O17 Sb1 96.9(5) . . ? Co1 O17 Sb2 120.7(5) . . ? Sb7 O17 Sb2 96.1(5) . . ? Sb1 O17 Sb2 94.8(4) . . ? Sb1 O18 Sb7 109.9(6) . . ? Sb10 O19 Sb7 138.3(7) . . ? Sb10 O20 Sb8 137.4(7) . . ? Sb8 O21 Sb11 136.3(7) . . ? Sb9 O22 Sb11 136.4(7) . . ? Sb9 O23 Sb12 135.4(7) . . ? Co1 O24 Sb12 126.8(5) . . ? Co1 O24 Sb11 121.9(5) . . ? Sb12 O24 Sb11 93.9(4) . . ? Co1 O24 Sb10 120.6(5) . . ? Sb12 O24 Sb10 93.0(4) . . ? Sb11 O24 Sb10 91.7(4) . . ? Sb12 O25 Sb7 131.3(7) . . ? Sb12 O26 Sb10 105.8(6) . . ? Sb11 O27 Sb10 108.0(6) . . ? Sb12 O28 Sb11 106.8(6) . . ? C12 C11 C16 120.0 . . ? C12 C11 Sb1 121.7(16) . . ? C16 C11 Sb1 118.1(16) . . ? C11 C12 C13 120.0 . . ? C14 C13 C12 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 C17 120(2) . . ? C13 C14 C17 120(2) . . ? C14 C15 C16 120.0 . . ? C15 C16 C11 120.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 Sb2 122.4(17) . . ? C26 C21 Sb2 117.1(17) . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 C27 123(2) . . ? C23 C24 C27 117(2) . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 Sb3 123.1(17) . . ? C36 C31 Sb3 116.7(17) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 C37 118(2) . . ? C33 C34 C37 122(2) . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 Sb4 116.9(17) . . ? C46 C41 Sb4 123.0(17) . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 C47 119(2) . . ? C43 C44 C47 119(2) . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 Sb5 120.4(16) . . ? C56 C51 Sb5 119.5(16) . . ? C53 C52 C51 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 C57 125(2) . . ? C55 C54 C57 114(2) . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 Sb6 125.1(16) . . ? C66 C61 Sb6 114.5(16) . . ? C63 C62 C61 120.0 . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C65 C64 C67 132(2) . . ? C63 C64 C67 108(2) . . ? C64 C65 C66 120.0 . . ? C65 C66 C61 120.0 . . ? C72 C71 C76 120.0 . . ? C72 C71 Sb7 119.3(16) . . ? C76 C71 Sb7 120.0(16) . . ? C73 C72 C71 120.0 . . ? C72 C73 C74 120.0 . . ? C75 C74 C73 120.0 . . ? C75 C74 C77 117(2) . . ? C73 C74 C77 122(2) . . ? C74 C75 C76 120.0 . . ? C75 C76 C71 120.0 . . ? C82 C81 C86 120.0 . . ? C82 C81 Sb8 121.8(16) . . ? C86 C81 Sb8 118.1(16) . . ? C83 C82 C81 120.0 . . ? C84 C83 C82 120.0 . . ? C83 C84 C85 120.0 . . ? C83 C84 C87 124(2) . . ? C85 C84 C87 114(2) . . ? C84 C85 C86 120.0 . . ? C85 C86 C81 120.0 . . ? C92 C91 C96 120.0 . . ? C92 C91 Sb9 122.8(17) . . ? C96 C91 Sb9 117.0(17) . . ? C91 C92 C93 120.0 . . ? C92 C93 C94 120.0 . . ? C95 C94 C93 120.0 . . ? C95 C94 C97 125(2) . . ? C93 C94 C97 114(2) . . ? C94 C95 C96 120.0 . . ? C95 C96 C91 120.0 . . ? C102 C101 C106 120.0 . . ? C102 C101 Sb10 119.0(17) . . ? C106 C101 Sb10 120.0(17) . . ? C103 C102 C101 120.0 . . ? C102 C103 C104 120.0 . . ? C105 C104 C103 120.0 . . ? C105 C104 C107 124(2) . . ? C103 C104 C107 115(2) . . ? C104 C105 C106 120.0 . . ? C105 C106 C101 120.0 . . ? C112 C111 C116 120.0 . . ? C112 C111 Sb11 122.6(16) . . ? C116 C111 Sb11 117.4(17) . . ? C111 C112 C113 120.0 . . ? C114 C113 C112 120.0 . . ? C113 C114 C115 120.0 . . ? C113 C114 C117 114(2) . . ? C115 C114 C117 124(2) . . ? C114 C115 C116 120.0 . . ? C115 C116 C111 120.0 . . ? C122 C121 C126 120.0 . . ? C122 C121 Sb12 123.6(16) . . ? C126 C121 Sb12 116.0(16) . . ? C121 C122 C123 120.0 . . ? C124 C123 C122 120.0 . . ? C125 C124 C123 120.0 . . ? C125 C124 C127 123(2) . . ? C123 C124 C127 117(2) . . ? C124 C125 C126 120.0 . . ? C125 C126 C121 120.0 . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 72.12 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.992 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.161 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.499 -0.001 0.499 4413.6 143.9 2 0.129 0.019 0.813 5.7 0.5 3 0.629 0.481 0.313 6.2 0.3 4 0.371 0.519 0.687 5.7 0.5 5 0.871 0.981 0.187 6.2 0.4 _platon_squeeze_details ; ; # Attachment '- csco_sq_may.cif' data_csco_sq _database_code_depnum_ccdc_archive 'CCDC 866858' #TrackingRef '- csco_sq_may.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H84 Co O28 Sb12, 4(Co H6 O3), 6(H2O), 2 Cl' _chemical_formula_sum 'C84 H120 Cl2 Co5 O46 Sb12' _chemical_formula_weight 3692.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 n 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y, x, -z' 'y, -x, -z' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' _cell_length_a 16.5969(7) _cell_length_b 16.5969(7) _cell_length_c 24.2315(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6674.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 139(2) _cell_measurement_reflns_used 7631 _cell_measurement_theta_min 6.65 _cell_measurement_theta_max 72.0 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.837 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3546 _exptl_absorpt_coefficient_mu 24.603 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.36 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 139(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Rigaku MM007 rotating anode' _diffrn_radiation_monochromator 'Rigaku VariMax-HF Confocal Optical System' _diffrn_measurement_device_type 'Rigaku Spider' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57610 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 6.65 _diffrn_reflns_theta_max 72.12 _reflns_number_total 6530 _reflns_number_gt 5645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2005)' _computing_cell_refinement 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_data_reduction 'FSProcess in Process-Auto (Rigaku, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms for the aryl rings were placed in calculated positions, but those for the H2O molecules were not included. ; _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^)+(0.0650P)^2^+16.4759P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.067(12) _refine_ls_number_reflns 6530 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1310 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Sb1 Sb 0.65458(4) 0.64587(4) 0.95441(3) 0.05017(16) Uani 1 1 d . . . Sb2 Sb 0.47265(4) 0.71189(4) 0.95564(3) 0.05081(17) Uani 1 1 d . . . Sb3 Sb 0.53035(3) 0.58744(4) 0.86224(3) 0.04954(16) Uani 1 1 d . . . Co1 Co 0.5000 0.5000 1.0000 0.0453(6) Uani 1 4 d S . . Co2 Co 0.68403(9) 0.43336(10) 0.90618(6) 0.0502(4) Uani 1 1 d . . . O1 O 0.5341(3) 0.5945(3) 0.9508(2) 0.0471(14) Uani 1 1 d . . . O2 O 0.6327(4) 0.3519(3) 0.9625(2) 0.0484(15) Uani 1 1 d . . . O3 O 0.4695(4) 0.6948(4) 1.0381(3) 0.0549(16) Uani 1 1 d . . . O4 O 0.6393(4) 0.6297(4) 0.8749(3) 0.0551(16) Uani 1 1 d . . . O5 O 0.4730(4) 0.6889(4) 0.8770(3) 0.0564(17) Uani 1 1 d . . . O6 O 0.5860(4) 0.7428(4) 0.9600(3) 0.0553(16) Uani 1 1 d . . . O7 O 0.4281(4) 0.5262(4) 0.8706(3) 0.0509(15) Uani 1 1 d . . . O8 O 0.6832(4) 0.3391(4) 0.8467(3) 0.0624(18) Uani 1 1 d . . . O9 O 0.7976(4) 0.3900(5) 0.9338(3) 0.0630(18) Uani 1 1 d . . . O10 O 0.7429(5) 0.5054(5) 0.8452(3) 0.076(2) Uani 1 1 d . . . C11 C 0.7655(6) 0.7058(6) 0.9485(5) 0.061(3) Uani 1 1 d . . . C12 C 0.7944(7) 0.7536(6) 0.9915(5) 0.064(3) Uani 1 1 d . . . H12 H 0.7621 0.7615 1.0234 0.077 Uiso 1 1 calc R . . C13 C 0.8677(7) 0.7889(7) 0.9884(6) 0.075(3) Uani 1 1 d . . . H13 H 0.8830 0.8248 1.0170 0.090 Uiso 1 1 calc R . . C14 C 0.9212(8) 0.7757(9) 0.9462(6) 0.086(4) Uani 1 1 d . . . C15 C 0.8889(8) 0.7274(9) 0.9014(5) 0.089(4) Uani 1 1 d . . . H15 H 0.9209 0.7187 0.8695 0.107 Uiso 1 1 calc R . . C16 C 0.8159(7) 0.6951(7) 0.9039(5) 0.072(3) Uani 1 1 d . . . H16 H 0.7977 0.6633 0.8738 0.086 Uiso 1 1 calc R . . C17 C 1.0002(10) 0.8135(11) 0.9415(7) 0.117(6) Uani 1 1 d . . . H17A H 0.9987 0.8546 0.9125 0.175 Uiso 1 1 calc R . . H17B H 1.0405 0.7726 0.9321 0.175 Uiso 1 1 calc R . . H17C H 1.0145 0.8387 0.9767 0.175 Uiso 1 1 calc R . . C21 C 0.4273(6) 0.8308(6) 0.9480(5) 0.057(2) Uani 1 1 d . . . C22 C 0.3915(9) 0.8568(7) 0.9027(6) 0.090(4) Uani 1 1 d . . . H22 H 0.3843 0.8217 0.8722 0.108 Uiso 1 1 calc R . . C23 C 0.3646(11) 0.9349(8) 0.9000(7) 0.104(5) Uani 1 1 d . . . H23 H 0.3389 0.9513 0.8669 0.124 Uiso 1 1 calc R . . C24 C 0.3714(9) 0.9880(7) 0.9387(6) 0.076(3) Uani 1 1 d . . . C25 C 0.4047(7) 0.9617(8) 0.9849(9) 0.101(6) Uani 1 1 d . . . H25 H 0.4086 0.9987 1.0147 0.121 Uiso 1 1 calc R . . C26 C 0.4351(6) 0.8823(7) 0.9938(6) 0.073(3) Uani 1 1 d . . . H26 H 0.4586 0.8657 1.0277 0.087 Uiso 1 1 calc R . . C27 C 0.3414(12) 1.0733(8) 0.9395(10) 0.142(8) Uani 1 1 d . . . H27A H 0.3375 1.0920 0.9778 0.213 Uiso 1 1 calc R . . H27B H 0.2881 1.0757 0.9222 0.213 Uiso 1 1 calc R . . H27C H 0.3789 1.1078 0.9191 0.213 Uiso 1 1 calc R . . C31 C 0.5293(6) 0.6011(6) 0.7749(4) 0.054(2) Uani 1 1 d . . . C32 C 0.4565(7) 0.5970(8) 0.7489(5) 0.074(3) Uani 1 1 d . . . H32 H 0.4088 0.5877 0.7696 0.088 Uiso 1 1 calc R . . C33 C 0.4523(7) 0.6067(7) 0.6911(5) 0.068(3) Uani 1 1 d . . . H33 H 0.4023 0.6030 0.6722 0.082 Uiso 1 1 calc R . . C34 C 0.5208(7) 0.6213(7) 0.6637(4) 0.065(3) Uani 1 1 d . . . C35 C 0.5913(9) 0.6277(10) 0.6902(5) 0.094(5) Uani 1 1 d . . . H35 H 0.6391 0.6396 0.6702 0.113 Uiso 1 1 calc R . . C36 C 0.5947(8) 0.6170(9) 0.7467(6) 0.089(4) Uani 1 1 d . . . H36 H 0.6450 0.6212 0.7653 0.107 Uiso 1 1 calc R . . C37 C 0.5169(10) 0.6279(10) 0.5971(5) 0.102(5) Uani 1 1 d . . . H37A H 0.4791 0.5876 0.5828 0.152 Uiso 1 1 calc R . . H37B H 0.5706 0.6182 0.5817 0.152 Uiso 1 1 calc R . . H37C H 0.4985 0.6819 0.5866 0.152 Uiso 1 1 calc R . . OW1 O 0.9230(6) 0.4655(6) 0.8674(5) 0.105(3) Uiso 1 1 d . . . OW2 O 0.8178(12) 0.2375(12) 0.8620(8) 0.097(5) Uiso 0.50 1 d P . . Cl1A Cl 0.8431(8) 0.6569(8) 0.7500 0.109(5) Uiso 0.33 2 d SP . . Cl1B Cl 0.9490(8) 0.2821(8) 0.7781(5) 0.104(3) Uiso 0.33 1 d P . . 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 Sb1 0.0454(3) 0.0483(3) 0.0568(3) 0.0022(3) -0.0004(3) -0.0038(2) Sb2 0.0500(4) 0.0450(3) 0.0575(4) 0.0033(3) 0.0012(3) 0.0009(2) Sb3 0.0450(3) 0.0504(3) 0.0533(3) 0.0031(3) 0.0000(3) 0.0004(2) Co1 0.0427(9) 0.0427(9) 0.0507(16) 0.000 0.000 0.000 Co2 0.0416(8) 0.0523(9) 0.0565(9) -0.0014(7) 0.0002(7) 0.0026(6) O1 0.049(4) 0.041(3) 0.051(3) -0.003(3) 0.002(3) 0.002(2) O2 0.063(4) 0.026(3) 0.057(3) 0.000(3) -0.018(3) 0.005(2) O3 0.058(4) 0.052(4) 0.055(4) 0.004(3) 0.000(3) 0.005(3) O4 0.046(4) 0.053(4) 0.066(4) 0.009(3) 0.007(3) -0.004(3) O5 0.055(4) 0.048(4) 0.067(4) 0.012(3) 0.003(3) 0.002(3) O6 0.065(4) 0.046(3) 0.054(4) -0.002(3) -0.002(3) 0.005(3) O7 0.047(3) 0.052(4) 0.054(4) -0.002(3) -0.005(3) 0.006(3) O8 0.053(4) 0.068(5) 0.066(4) -0.007(3) 0.000(3) 0.002(3) O9 0.055(4) 0.069(5) 0.065(4) -0.002(4) -0.008(3) 0.007(4) O10 0.072(5) 0.075(5) 0.082(5) -0.002(4) 0.008(4) -0.003(4) C11 0.059(6) 0.056(6) 0.068(6) 0.003(5) -0.001(5) -0.005(5) C12 0.064(7) 0.052(6) 0.077(7) 0.000(5) -0.009(5) -0.001(5) C13 0.069(7) 0.063(7) 0.092(8) 0.000(6) -0.016(7) -0.016(6) C14 0.073(8) 0.097(10) 0.089(9) 0.011(8) -0.002(7) -0.030(7) C15 0.071(8) 0.117(12) 0.078(8) -0.008(8) 0.006(7) -0.033(8) C16 0.059(7) 0.073(8) 0.084(8) -0.002(6) 0.009(6) -0.023(6) C17 0.124(13) 0.129(13) 0.097(10) -0.001(9) 0.007(9) -0.072(12) C21 0.050(5) 0.039(5) 0.082(7) -0.002(5) 0.000(5) 0.006(4) C22 0.132(12) 0.041(6) 0.096(9) 0.007(6) -0.030(9) 0.013(7) C23 0.144(14) 0.056(8) 0.110(11) -0.005(8) -0.030(10) 0.029(8) C24 0.086(9) 0.048(6) 0.094(9) 0.002(6) -0.018(7) 0.000(6) C25 0.058(8) 0.051(7) 0.194(17) -0.041(9) -0.007(9) -0.012(6) C26 0.045(6) 0.049(6) 0.123(11) 0.001(6) -0.013(6) -0.005(4) C27 0.147(17) 0.050(8) 0.23(2) 0.002(11) -0.025(15) 0.009(9) C31 0.049(6) 0.055(6) 0.060(6) 0.000(5) -0.002(4) 0.001(4) C32 0.055(6) 0.087(9) 0.079(7) -0.008(6) 0.012(5) 0.010(6) C33 0.072(7) 0.074(7) 0.059(6) -0.007(5) -0.010(5) 0.022(6) C34 0.068(7) 0.069(7) 0.059(6) 0.009(5) -0.001(5) -0.004(6) C35 0.085(9) 0.147(14) 0.050(6) 0.023(7) -0.006(6) -0.004(9) C36 0.060(7) 0.125(12) 0.083(8) 0.015(8) 0.003(6) 0.008(7) C37 0.110(12) 0.125(12) 0.069(8) 0.019(8) -0.021(8) 0.000(9) _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 Sb1 O4 1.963(7) . ? Sb1 O6 1.975(6) . ? Sb1 O2 2.028(6) 5_657 ? Sb1 O3 2.035(7) 6_567 ? Sb1 C11 2.098(10) . ? Sb1 O1 2.176(6) . ? Sb1 Sb2 3.0862(9) 6_567 ? Sb1 Sb3 3.1906(9) . ? Sb1 Sb2 3.2122(9) . ? Sb2 O5 1.943(7) . ? Sb2 O6 1.953(7) . ? Sb2 O3 2.019(6) . ? Sb2 O2 2.050(7) 2_665 ? Sb2 C21 2.120(9) . ? Sb2 O1 2.202(6) . ? Sb2 Sb1 3.0861(9) 5_657 ? Sb2 Sb3 3.2103(9) . ? Sb3 O4 1.963(6) . ? Sb3 O5 1.967(7) . ? Sb3 O7 1.989(6) . ? Sb3 O7 2.018(6) 2_665 ? Sb3 C31 2.130(10) . ? Sb3 O1 2.150(6) . ? Sb3 Sb3 3.0723(12) 2_665 ? Co1 O1 2.050(6) 2_665 ? Co1 O1 2.050(6) 5_657 ? Co1 O1 2.050(6) 6_567 ? Co1 O1 2.050(6) . ? Co2 O2 2.102(7) . ? Co2 O3 2.111(7) 6_567 ? Co2 O9 2.126(7) . ? Co2 O8 2.127(7) . ? Co2 O10 2.138(8) . ? Co2 O7 2.158(6) 2_665 ? O2 Sb1 2.028(6) 6_567 ? O2 Sb2 2.050(7) 2_665 ? O3 Sb1 2.035(7) 5_657 ? O3 Co2 2.111(7) 5_657 ? O7 Sb3 2.018(6) 2_665 ? O7 Co2 2.158(6) 2_665 ? C11 C16 1.378(15) . ? C11 C12 1.395(15) . ? C12 C13 1.352(15) . ? C13 C14 1.371(18) . ? C14 C15 1.452(18) . ? C14 C17 1.459(18) . ? C15 C16 1.325(15) . ? C21 C22 1.322(16) . ? C21 C26 1.407(17) . ? C22 C23 1.372(16) . ? C23 C24 1.292(18) . ? C24 C25 1.32(2) . ? C24 C27 1.500(18) . ? C25 C26 1.427(17) . ? C31 C36 1.310(15) . ? C31 C32 1.363(15) . ? C32 C33 1.412(16) . ? C33 C34 1.338(16) . ? C34 C35 1.341(16) . ? C34 C37 1.618(16) . ? C35 C36 1.381(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Sb1 O6 96.0(3) . . ? O4 Sb1 O2 162.4(2) . 5_657 ? O6 Sb1 O2 89.4(3) . 5_657 ? O4 Sb1 O3 90.1(3) . 6_567 ? O6 Sb1 O3 161.6(3) . 6_567 ? O2 Sb1 O3 80.1(3) 5_657 6_567 ? O4 Sb1 C11 96.4(4) . . ? O6 Sb1 C11 97.2(4) . . ? O2 Sb1 C11 99.5(4) 5_657 . ? O3 Sb1 C11 99.4(4) 6_567 . ? O4 Sb1 O1 77.7(2) . . ? O6 Sb1 O1 78.0(2) . . ? O2 Sb1 O1 87.1(2) 5_657 . ? O3 Sb1 O1 86.4(2) 6_567 . ? C11 Sb1 O1 171.8(3) . . ? O4 Sb1 Sb2 130.3(2) . 6_567 ? O6 Sb1 Sb2 130.40(19) . 6_567 ? O2 Sb1 Sb2 41.10(19) 5_657 6_567 ? O3 Sb1 Sb2 40.23(18) 6_567 6_567 ? C11 Sb1 Sb2 94.6(3) . 6_567 ? O1 Sb1 Sb2 93.57(16) . 6_567 ? O4 Sb1 Sb3 35.64(18) . . ? O6 Sb1 Sb3 85.60(19) . . ? O2 Sb1 Sb3 128.91(16) 5_657 . ? O3 Sb1 Sb3 89.33(18) 6_567 . ? C11 Sb1 Sb3 131.6(3) . . ? O1 Sb1 Sb3 42.16(16) . . ? Sb2 Sb1 Sb3 119.99(2) 6_567 . ? O4 Sb1 Sb2 86.2(2) . . ? O6 Sb1 Sb2 34.90(19) . . ? O2 Sb1 Sb2 88.74(16) 5_657 . ? O3 Sb1 Sb2 128.91(19) 6_567 . ? C11 Sb1 Sb2 131.6(3) . . ? O1 Sb1 Sb2 43.10(15) . . ? Sb2 Sb1 Sb2 120.04(2) 6_567 . ? Sb3 Sb1 Sb2 60.182(18) . . ? O5 Sb2 O6 95.9(3) . . ? O5 Sb2 O3 160.5(3) . . ? O6 Sb2 O3 90.5(3) . . ? O5 Sb2 O2 88.9(3) . 2_665 ? O6 Sb2 O2 162.3(3) . 2_665 ? O3 Sb2 O2 79.9(3) . 2_665 ? O5 Sb2 C21 95.6(4) . . ? O6 Sb2 C21 95.9(3) . . ? O3 Sb2 C21 102.0(4) . . ? O2 Sb2 C21 100.6(3) 2_665 . ? O5 Sb2 O1 76.9(3) . . ? O6 Sb2 O1 77.8(2) . . ? O3 Sb2 O1 86.6(2) . . ? O2 Sb2 O1 86.7(2) 2_665 . ? C21 Sb2 O1 169.5(3) . . ? O5 Sb2 Sb1 129.3(2) . 5_657 ? O6 Sb2 Sb1 131.04(19) . 5_657 ? O3 Sb2 Sb1 40.63(19) . 5_657 ? O2 Sb2 Sb1 40.55(17) 2_665 5_657 ? C21 Sb2 Sb1 97.0(3) . 5_657 ? O1 Sb2 Sb1 93.44(16) . 5_657 ? O5 Sb2 Sb3 35.07(19) . . ? O6 Sb2 Sb3 85.40(19) . . ? O3 Sb2 Sb3 127.95(19) . . ? O2 Sb2 Sb3 88.83(15) 2_665 . ? C21 Sb2 Sb3 130.0(3) . . ? O1 Sb2 Sb3 41.84(16) . . ? Sb1 Sb2 Sb3 119.32(2) 5_657 . ? O5 Sb2 Sb1 85.49(19) . . ? O6 Sb2 Sb1 35.37(19) . . ? O3 Sb2 Sb1 89.18(18) . . ? O2 Sb2 Sb1 128.77(15) 2_665 . ? C21 Sb2 Sb1 130.6(3) . . ? O1 Sb2 Sb1 42.49(15) . . ? Sb1 Sb2 Sb1 120.03(3) 5_657 . ? Sb3 Sb2 Sb1 59.575(19) . . ? O4 Sb3 O5 96.4(3) . . ? O4 Sb3 O7 162.3(3) . . ? O5 Sb3 O7 90.3(3) . . ? O4 Sb3 O7 90.2(3) . 2_665 ? O5 Sb3 O7 161.3(3) . 2_665 ? O7 Sb3 O7 78.7(3) . 2_665 ? O4 Sb3 C31 97.2(3) . . ? O5 Sb3 C31 94.9(3) . . ? O7 Sb3 C31 98.5(3) . . ? O7 Sb3 C31 101.7(3) 2_665 . ? O4 Sb3 O1 78.4(2) . . ? O5 Sb3 O1 77.6(2) . . ? O7 Sb3 O1 87.2(2) . . ? O7 Sb3 O1 86.6(2) 2_665 . ? C31 Sb3 O1 170.7(3) . . ? O4 Sb3 Sb3 129.7(2) . 2_665 ? O5 Sb3 Sb3 130.53(19) . 2_665 ? O7 Sb3 Sb3 40.28(17) . 2_665 ? O7 Sb3 Sb3 39.59(18) 2_665 2_665 ? C31 Sb3 Sb3 95.6(3) . 2_665 ? O1 Sb3 Sb3 93.50(16) . 2_665 ? O4 Sb3 Sb1 35.64(19) . . ? O5 Sb3 Sb1 85.7(2) . . ? O7 Sb3 Sb1 129.46(18) . . ? O7 Sb3 Sb1 89.59(18) 2_665 . ? C31 Sb3 Sb1 132.0(3) . . ? O1 Sb3 Sb1 42.80(16) . . ? Sb3 Sb3 Sb1 119.94(2) 2_665 . ? O4 Sb3 Sb2 86.3(2) . . ? O5 Sb3 Sb2 34.58(19) . . ? O7 Sb3 Sb2 90.15(17) . . ? O7 Sb3 Sb2 129.22(18) 2_665 . ? C31 Sb3 Sb2 129.0(3) . . ? O1 Sb3 Sb2 43.08(15) . . ? Sb3 Sb3 Sb2 120.66(2) 2_665 . ? Sb1 Sb3 Sb2 60.24(2) . . ? O1 Co1 O1 109.78(17) 2_665 5_657 ? O1 Co1 O1 109.78(16) 2_665 6_567 ? O1 Co1 O1 108.9(3) 5_657 6_567 ? O1 Co1 O1 108.9(3) 2_665 . ? O1 Co1 O1 109.78(16) 5_657 . ? O1 Co1 O1 109.78(17) 6_567 . ? O2 Co2 O3 96.3(2) . 6_567 ? O2 Co2 O9 86.4(3) . . ? O3 Co2 O9 89.0(3) 6_567 . ? O2 Co2 O8 87.9(3) . . ? O3 Co2 O8 174.8(3) 6_567 . ? O9 Co2 O8 88.3(3) . . ? O2 Co2 O10 173.8(3) . . ? O3 Co2 O10 88.7(3) 6_567 . ? O9 Co2 O10 90.1(3) . . ? O8 Co2 O10 86.9(3) . . ? O2 Co2 O7 96.3(2) . 2_665 ? O3 Co2 O7 95.2(3) 6_567 2_665 ? O9 Co2 O7 174.7(3) . 2_665 ? O8 Co2 O7 87.3(3) . 2_665 ? O10 Co2 O7 86.8(3) . 2_665 ? Co1 O1 Sb3 122.1(3) . . ? Co1 O1 Sb1 122.0(3) . . ? Sb3 O1 Sb1 95.0(2) . . ? Co1 O1 Sb2 121.2(3) . . ? Sb3 O1 Sb2 95.1(2) . . ? Sb1 O1 Sb2 94.4(2) . . ? Sb1 O2 Sb2 98.4(3) 6_567 2_665 ? Sb1 O2 Co2 129.4(3) 6_567 . ? Sb2 O2 Co2 128.7(3) 2_665 . ? Sb2 O3 Sb1 99.1(3) . 5_657 ? Sb2 O3 Co2 128.7(3) . 5_657 ? Sb1 O3 Co2 129.3(3) 5_657 5_657 ? Sb3 O4 Sb1 108.7(3) . . ? Sb2 O5 Sb3 110.3(3) . . ? Sb2 O6 Sb1 109.7(3) . . ? Sb3 O7 Sb3 100.1(3) . 2_665 ? Sb3 O7 Co2 128.1(3) . 2_665 ? Sb3 O7 Co2 128.7(3) 2_665 2_665 ? C16 C11 C12 116.8(10) . . ? C16 C11 Sb1 121.7(8) . . ? C12 C11 Sb1 121.4(8) . . ? C13 C12 C11 120.9(11) . . ? C12 C13 C14 123.7(12) . . ? C13 C14 C15 114.0(11) . . ? C13 C14 C17 124.9(13) . . ? C15 C14 C17 120.7(13) . . ? C16 C15 C14 121.7(13) . . ? C15 C16 C11 122.6(12) . . ? C22 C21 C26 119.8(10) . . ? C22 C21 Sb2 122.5(9) . . ? C26 C21 Sb2 117.7(8) . . ? C21 C22 C23 119.7(13) . . ? C24 C23 C22 125.6(15) . . ? C23 C24 C25 115.1(13) . . ? C23 C24 C27 128.6(15) . . ? C25 C24 C27 116.1(14) . . ? C24 C25 C26 125.5(14) . . ? C21 C26 C25 114.2(13) . . ? C36 C31 C32 120.3(12) . . ? C36 C31 Sb3 122.1(9) . . ? C32 C31 Sb3 117.4(8) . . ? C31 C32 C33 119.7(11) . . ? C34 C33 C32 118.1(11) . . ? C33 C34 C35 121.2(11) . . ? C33 C34 C37 118.2(11) . . ? C35 C34 C37 120.6(12) . . ? C34 C35 C36 120.1(13) . . ? C31 C36 C35 120.5(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 72.12 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.080 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.119 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.000 0.000 0.000 7.3 0.1 2 0.000 0.500 0.250 490.3 11.5 3 0.000 0.500 0.750 28.3 4.9 4 0.500 1.000 0.750 490.3 13.1 5 0.500 0.000 0.250 28.3 3.5 6 0.500 0.500 0.500 7.3 -0.6 _platon_squeeze_details ; ; __exptl_crystal_density_method 'not measured' data_p_cl4_sq _database_code_depnum_ccdc_archive 'CCDC 866859' #TrackingRef '- p_cl4_sq.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; '2(C10 H16 N), C72 H48 Br1.40 Cl14.46 O28 Sb12 Sr0.14 Zn4.86, 7(C2 H3 N), H2 O' ; _chemical_formula_sum 'C108 H106 Br1.40 Cl14.46 N10 O29 Sb12 Sr0.14 Zn4.86' _chemical_formula_weight 4423.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 15.2930(2) _cell_length_b 25.0465(4) _cell_length_c 19.1113(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.5970(10) _cell_angle_gamma 90.00 _cell_volume 7312.80(19) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 9531 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4228 _exptl_absorpt_coefficient_mu 3.720 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 170500 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 27.98 _reflns_number_total 17961 _reflns_number_gt 13560 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. (i) The Zn(3) and Zn(4) and attached halide were refined with sof (1-x) to account for the x fractions of Sr2+ (0.1 and 0.04 respectively) arising from substitutional disorder (ii) four restraints limit the Zn-Cl/Zn-Br distances (twice) for the overlapping halide positions (iii) the data have been SQUEEZED to account for the void volume (153 3) which presumably contains 2-3 extra MeCN and/or H2O. Details are appended below (iv) H atoms were not included for the H2O molecule, (v) Residual electron density consisted of 7 peaks 2.2-3.4 e -3 in each case ca 0.7 away from each of the unique Sb atoms, all in the same direction. This was treated as some small disorder relating to the Sb12 polyhedron. This refined to ca 3% of an alternative orientation. Similarly there were four partial O atoms around the Zn atom corresponding to an inverted tetrahedral orientation and these also refined to ca 3%. None of the other atoms that would follow the alternative arrangement could be resolved. Extra void volume was dealt with using SQUEEZE (see below). ; _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^)+(0.0728P)^2^+36.2801P] 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 17961 _refine_ls_number_parameters 931 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Sb1 Sb 0.98738(4) 0.2500 0.50338(4) 0.02541(13) Uani 0.97 2 d SP . 1 Sb2 Sb 0.83398(4) 0.2500 0.38969(4) 0.02469(13) Uani 0.97 2 d SP . 1 Sb3 Sb 1.16318(3) 0.313693(16) 0.47738(3) 0.02421(10) Uani 0.97 1 d P . 1 Sb4 Sb 1.18141(3) 0.375183(15) 0.33737(3) 0.02330(10) Uani 0.97 1 d P . 1 Sb5 Sb 1.20468(3) 0.312120(16) 0.19507(3) 0.02528(10) Uani 0.97 1 d P . 1 Sb6 Sb 1.02708(3) 0.375786(16) 0.22001(3) 0.02495(10) Uani 0.97 1 d P . 1 Sb7 Sb 0.85479(3) 0.313541(16) 0.24630(3) 0.02519(10) Uani 0.97 1 d P . 1 Zn1 Zn 1.05673(6) 0.2500 0.32057(5) 0.02351(19) Uani 1 2 d S . 1 Zn2 Zn 0.96423(4) 0.36943(3) 0.39929(4) 0.02778(16) Uani 1 1 d D . 1 Zn3 Zn 1.29615(6) 0.2500 0.35109(5) 0.0247(2) Uani 0.96 2 d SPD . 1 Zn4 Zn 1.00596(7) 0.2500 0.13228(6) 0.0314(2) Uani 0.90 2 d SPD . 1 Cl1 Cl 0.7387(5) 0.2500 0.7743(3) 0.160(3) Uani 1 2 d S A 1 Cl2 Cl 0.5156(3) 0.2500 0.6120(3) 0.1095(17) Uani 1 2 d S B 1 Cl3 Cl 1.40778(15) 0.48784(9) 0.65585(13) 0.0645(6) Uani 1 1 d . . 1 Cl4 Cl 1.41606(19) 0.57503(10) 0.46626(18) 0.0889(9) Uani 1 1 d . . 1 Cl5 Cl 1.48382(18) 0.36611(12) -0.04608(14) 0.0789(8) Uani 1 1 d . . 1 Cl6 Cl 0.8490(3) 0.57187(14) 0.03223(19) 0.1242(14) Uani 1 1 d . . 1 Cl7 Cl 0.60926(16) 0.49510(10) 0.08156(12) 0.0695(7) Uani 1 1 d . . 1 Cl21 Cl 0.9117(19) 0.4440(8) 0.4439(13) 0.0482(13) Uani 0.56 1 d PD . 1 Br21 Br 0.9032(9) 0.4400(4) 0.4554(6) 0.0482(13) Uani 0.44 1 d PD . 1 Cl31 Cl 1.4410(16) 0.2500 0.366(4) 0.049(3) Uani 0.56 2 d SPD . 1 Br31 Br 1.4438(9) 0.2500 0.375(2) 0.049(3) Uani 0.40 2 d SPD . 1 Cl41 Cl 1.0079(2) 0.2500 0.0166(2) 0.0452(8) Uani 0.78 2 d SPD . 1 Br41 Br 0.9755(7) 0.2500 0.0156(7) 0.0452(8) Uani 0.12 2 d SPD . 1 O1 O 0.7888(3) 0.30846(16) 0.3307(2) 0.0314(9) Uani 1 1 d . . 1 O2 O 0.9195(3) 0.30063(16) 0.4385(2) 0.0287(9) Uani 1 1 d . . 1 O3 O 1.0631(3) 0.30866(16) 0.5361(2) 0.0298(9) Uani 1 1 d . . 1 O4 O 0.9251(4) 0.2500 0.3030(3) 0.0206(11) Uani 0.95 2 d SP . 1 O5 O 1.0859(3) 0.2500 0.4249(3) 0.0223(11) Uani 0.96 2 d SP . 1 O6 O 1.2247(4) 0.2500 0.5120(3) 0.0295(13) Uani 1 2 d S . 1 O7 O 0.8060(4) 0.2500 0.1996(3) 0.0324(13) Uani 1 2 d S . 1 O8 O 1.0956(3) 0.36456(15) 0.4128(2) 0.0269(8) Uani 1 1 d . . 1 O9 O 0.9398(3) 0.36435(16) 0.2946(2) 0.0278(9) Uani 1 1 d . . 1 O10 O 1.2347(3) 0.31341(15) 0.3911(2) 0.0242(8) Uani 1 1 d . . 1 O11 O 0.9557(3) 0.31366(16) 0.1807(2) 0.0308(9) Uani 1 1 d . . 1 O12 O 1.1073(2) 0.31559(15) 0.2769(2) 0.0202(8) Uani 0.97 1 d P . 1 O13 O 1.0974(3) 0.42009(15) 0.2847(2) 0.0300(9) Uani 1 1 d . . 1 O14 O 1.1364(4) 0.2500 0.1553(3) 0.0315(13) Uani 1 2 d S . 1 O15 O 1.2584(4) 0.2500 0.2492(3) 0.0284(12) Uani 1 2 d S . 1 O16 O 1.2602(3) 0.36201(16) 0.2614(2) 0.0293(9) Uani 1 1 d . . 1 O17 O 1.1176(3) 0.36150(17) 0.1539(2) 0.0305(9) Uani 1 1 d . . 1 C11 C 0.9062(7) 0.2500 0.5889(6) 0.044(2) Uani 1 2 d S . . C12 C 0.9021(13) 0.2890(8) 0.6324(10) 0.055(4) Uani 0.50 1 d P . -2 C12A C 0.8564(11) 0.3003(6) 0.6002(9) 0.043(3) Uani 0.50 1 d P . -3 C13 C 0.8483(17) 0.2890(11) 0.6901(13) 0.078(7) Uani 0.50 1 d P . -2 C13A C 0.8027(14) 0.3023(8) 0.6561(12) 0.059(5) Uani 0.50 1 d P . -3 C14 C 0.8030(12) 0.2500 0.7018(8) 0.091(5) Uani 1 2 d S . . C21 C 0.7340(6) 0.2500 0.4622(5) 0.035(2) Uani 1 2 d S . . C22 C 0.7278(10) 0.2959(6) 0.5063(8) 0.043(3) Uani 0.50 1 d P . -2 C22A C 0.6764(12) 0.2907(7) 0.4649(10) 0.054(4) Uani 0.50 1 d P . -3 C23 C 0.6609(12) 0.2963(7) 0.5537(10) 0.055(4) Uani 0.50 1 d P . -2 C23A C 0.6076(14) 0.2871(7) 0.5111(12) 0.066(5) Uani 0.50 1 d P . -3 C24 C 0.6017(8) 0.2500 0.5544(8) 0.068(4) Uani 1 2 d S . . C31 C 1.2392(4) 0.3689(2) 0.5360(4) 0.0332(14) Uani 1 1 d . . 1 C32 C 1.2094(4) 0.4207(3) 0.5467(4) 0.0375(15) Uani 1 1 d . . 1 H32 H 1.1533 0.4312 0.5281 0.045 Uiso 1 1 calc R . 1 C33 C 1.2617(5) 0.4571(3) 0.5846(4) 0.0401(15) Uani 1 1 d . . 1 H33 H 1.2417 0.4925 0.5915 0.048 Uiso 1 1 calc R . 1 C34 C 1.3415(5) 0.4416(3) 0.6116(4) 0.0443(17) Uani 1 1 d . . 1 C35 C 1.3727(5) 0.3901(3) 0.6025(4) 0.0444(17) Uani 1 1 d . . 1 H35 H 1.4287 0.3801 0.6216 0.053 Uiso 1 1 calc R . 1 C36 C 1.3210(4) 0.3531(3) 0.5648(4) 0.0364(14) Uani 1 1 d . . 1 H36 H 1.3410 0.3175 0.5589 0.044 Uiso 1 1 calc R . 1 C41 C 1.2555(4) 0.4380(2) 0.3821(4) 0.0354(14) Uani 1 1 d . . 1 C42 C 1.2159(4) 0.4871(3) 0.3936(4) 0.0391(15) Uani 1 1 d . . 1 H42 H 1.1550 0.4916 0.3836 0.047 Uiso 1 1 calc R . 1 C43 C 1.2658(5) 0.5289(3) 0.4195(4) 0.0465(17) Uani 1 1 d . . 1 H43 H 1.2396 0.5627 0.4270 0.056 Uiso 1 1 calc R . 1 C44 C 1.3531(5) 0.5215(3) 0.4345(5) 0.0502(19) Uani 1 1 d . . 1 C45 C 1.3923(5) 0.4729(3) 0.4273(5) 0.055(2) Uani 1 1 d . . 1 H45 H 1.4524 0.4683 0.4407 0.066 Uiso 1 1 calc R . 1 C46 C 1.3440(4) 0.4307(3) 0.4005(4) 0.0423(16) Uani 1 1 d . . 1 H46 H 1.3706 0.3969 0.3945 0.051 Uiso 1 1 calc R . 1 C51 C 1.2961(4) 0.3227(3) 0.1176(3) 0.0344(14) Uani 1 1 d . . 1 C52 C 1.3796(5) 0.3392(3) 0.1379(4) 0.0474(18) Uani 1 1 d . . 1 H52 H 1.3971 0.3412 0.1861 0.057 Uiso 1 1 calc R . 1 C53 C 1.4380(5) 0.3528(4) 0.0871(4) 0.053(2) Uani 1 1 d . . 1 H53 H 1.4951 0.3653 0.1002 0.064 Uiso 1 1 calc R . 1 C54 C 1.4120(6) 0.3480(4) 0.0183(4) 0.057(2) Uani 1 1 d . . 1 C55 C 1.3285(6) 0.3310(4) -0.0035(4) 0.059(2) Uani 1 1 d . . 1 H55 H 1.3120 0.3278 -0.0518 0.071 Uiso 1 1 calc R . 1 C56 C 1.2711(5) 0.3192(3) 0.0473(4) 0.0496(18) Uani 1 1 d . . 1 H56 H 1.2131 0.3084 0.0340 0.059 Uiso 1 1 calc R . 1 C61 C 0.9675(4) 0.4385(3) 0.1620(4) 0.0344(14) Uani 1 1 d . . 1 C62 C 0.9408(7) 0.4299(4) 0.0929(4) 0.063(2) Uani 1 1 d . . 1 H62 H 0.9476 0.3956 0.0726 0.076 Uiso 1 1 calc R . 1 C63 C 0.9041(8) 0.4711(4) 0.0529(5) 0.084(4) Uani 1 1 d . . 1 H63 H 0.8853 0.4652 0.0055 0.101 Uiso 1 1 calc R . 1 C64 C 0.8954(6) 0.5200(4) 0.0822(5) 0.070(3) Uani 1 1 d . . 1 C65 C 0.9239(8) 0.5300(4) 0.1503(6) 0.083(3) Uani 1 1 d . . 1 H65 H 0.9183 0.5646 0.1699 0.099 Uiso 1 1 calc R . 1 C66 C 0.9608(7) 0.4889(3) 0.1897(5) 0.063(2) Uani 1 1 d . . 1 H66 H 0.9817 0.4956 0.2365 0.076 Uiso 1 1 calc R . 1 C71 C 0.7747(4) 0.3710(3) 0.1942(3) 0.0317(13) Uani 1 1 d . . 1 C72 C 0.7619(6) 0.4198(3) 0.2248(4) 0.060(2) Uani 1 1 d . . 1 H72 H 0.7881 0.4272 0.2698 0.073 Uiso 1 1 calc R . 1 C73 C 0.7111(7) 0.4581(4) 0.1905(5) 0.071(3) Uani 1 1 d . . 1 H73 H 0.7027 0.4920 0.2115 0.085 Uiso 1 1 calc R . 1 C74 C 0.6723(5) 0.4465(3) 0.1247(4) 0.0483(19) Uani 1 1 d . . 1 C75 C 0.6875(5) 0.3992(4) 0.0939(4) 0.054(2) Uani 1 1 d . . 1 H75 H 0.6633 0.3922 0.0481 0.065 Uiso 1 1 calc R . 1 C76 C 0.7382(5) 0.3607(3) 0.1286(4) 0.052(2) Uani 1 1 d . . 1 H76 H 0.7477 0.3272 0.1070 0.062 Uiso 1 1 calc R . 1 N1 N 0.3094(5) 0.5124(3) 0.1747(5) 0.071(2) Uani 1 1 d . C 1 C1 C 0.3639(9) 0.5119(5) 0.1131(6) 0.094(4) Uani 1 1 d . C 1 H1A H 0.3278 0.5211 0.0712 0.142 Uiso 1 1 calc R C 1 H1B H 0.3888 0.4762 0.1075 0.142 Uiso 1 1 calc R C 1 H1C H 0.4113 0.5380 0.1197 0.142 Uiso 1 1 calc R C 1 C2 C 0.3615(8) 0.4861(5) 0.2353(6) 0.095(4) Uani 1 1 d . C 1 H2A H 0.3775 0.4497 0.2221 0.142 Uiso 1 1 calc R C 1 H2B H 0.3257 0.4849 0.2766 0.142 Uiso 1 1 calc R C 1 H2C H 0.4147 0.5069 0.2463 0.142 Uiso 1 1 calc R C 1 C3 C 0.2298(8) 0.4795(5) 0.1625(7) 0.094(4) Uani 1 1 d . C 1 H3A H 0.1984 0.4770 0.2060 0.141 Uiso 1 1 calc R C 1 H3B H 0.2465 0.4436 0.1475 0.141 Uiso 1 1 calc R C 1 H3C H 0.1918 0.4961 0.1260 0.141 Uiso 1 1 calc R C 1 C4 C 0.2909(8) 0.5697(5) 0.2029(6) 0.083(3) Uani 1 1 d . C 1 H4A H 0.2510 0.5672 0.2421 0.099 Uiso 1 1 calc R C 1 H4B H 0.3464 0.5860 0.2209 0.099 Uiso 1 1 calc R C 1 C5 C 0.2500(7) 0.6046(5) 0.1459(5) 0.071(3) Uani 1 1 d . C 1 C6 C 0.3061(8) 0.6389(4) 0.1116(6) 0.078(3) Uani 1 1 d . C 1 H6 H 0.3672 0.6386 0.1231 0.094 Uiso 1 1 calc R C 1 C7 C 0.2694(8) 0.6753(4) 0.0576(6) 0.073(3) Uani 1 1 d . C 1 H7 H 0.3059 0.6991 0.0336 0.088 Uiso 1 1 calc R C 1 C8 C 0.1815(9) 0.6738(6) 0.0432(7) 0.097(4) Uani 1 1 d . C 1 H8 H 0.1583 0.6970 0.0076 0.117 Uiso 1 1 calc R C 1 C9 C 0.1198(9) 0.6394(5) 0.0782(7) 0.095(4) Uani 1 1 d . C 1 H9 H 0.0587 0.6396 0.0669 0.113 Uiso 1 1 calc R C 1 C10 C 0.1586(8) 0.6055(6) 0.1305(7) 0.094(4) Uani 1 1 d . C 1 H10 H 0.1220 0.5827 0.1560 0.113 Uiso 1 1 calc R C 1 N2 N 0.4945(8) 0.3859(7) 0.7776(6) 0.128(5) Uani 1 1 d . D 1 C2A C 0.4210(10) 0.3867(5) 0.7830(6) 0.086(3) Uani 1 1 d . D 1 C2B C 0.3216(9) 0.3834(6) 0.7913(7) 0.108(4) Uani 1 1 d . D 1 H2B1 H 0.2911 0.4006 0.7511 0.162 Uiso 1 1 calc R D 1 H2B2 H 0.3065 0.4017 0.8345 0.162 Uiso 1 1 calc R D 1 H2B3 H 0.3038 0.3459 0.7936 0.162 Uiso 1 1 calc R D 1 N3 N 0.3493(14) 0.2500 0.8233(13) 0.140(7) Uani 1 2 d S E 1 C3A C 0.4334(18) 0.2500 0.8342(15) 0.128(8) Uani 1 2 d S E 1 C3B C 0.5262(13) 0.2500 0.8349(18) 0.151(11) Uani 1 2 d S E 1 H3B1 H 0.5431 0.2795 0.8019 0.226 Uiso 0.50 1 d P F 1 H3B2 H 0.5440 0.2161 0.8116 0.226 Uiso 0.50 1 d P G 1 H3B3 H 0.5503 0.2543 0.8788 0.226 Uiso 0.50 1 d P H 1 N4 N 0.5992(9) 0.2500 0.0584(9) 0.083(4) Uani 1 2 d S I 1 C4A C 0.5877(10) 0.2500 0.1197(11) 0.076(4) Uani 1 2 d S I 1 C4B C 0.5791(10) 0.2500 0.1928(9) 0.083(4) Uani 1 2 d S I 1 H4B1 H 0.5255 0.2309 0.2040 0.125 Uiso 0.50 1 calc PR I 1 H4B2 H 0.5759 0.2869 0.2096 0.125 Uiso 0.50 1 calc PR I 1 H4B3 H 0.6298 0.2322 0.2156 0.125 Uiso 0.50 1 calc PR I 1 N5 N 0.5128(11) 0.4053(10) 0.2424(11) 0.183(11) Uani 1 1 d U J 1 C5A C 0.5471(11) 0.3873(8) 0.2891(15) 0.139(10) Uani 1 1 d U J 1 C5B C 0.5948(10) 0.3640(6) 0.3530(13) 0.161(10) Uani 1 1 d U J 1 H5B1 H 0.5602 0.3349 0.3718 0.241 Uiso 1 1 calc R J 1 H5B2 H 0.6035 0.3918 0.3888 0.241 Uiso 1 1 calc R J 1 H5B3 H 0.6519 0.3503 0.3400 0.241 Uiso 1 1 calc R J 1 N6 N 0.8907(6) 0.4198(4) 0.7078(6) 0.089(3) Uani 1 1 d . K 1 C6A C 0.9516(7) 0.4215(4) 0.6741(6) 0.075(3) Uani 1 1 d . K 1 C6B C 1.0262(9) 0.4240(5) 0.6330(7) 0.099(4) Uani 1 1 d . K 1 H6B1 H 1.0192 0.3989 0.5938 0.148 Uiso 1 1 calc R K 1 H6B2 H 1.0784 0.4146 0.6619 0.148 Uiso 1 1 calc R K 1 H6B3 H 1.0325 0.4603 0.6147 0.148 Uiso 1 1 calc R K 1 OW1 O 0.1796(14) 0.2500 0.6860(11) 0.173(7) Uiso 1 2 d S . . Sr1 Sr 0.9886(6) 0.2500 0.0771(5) 0.038(2) Uiso 0.10 2 d SP L 6 Sr2 Sr 1.368(2) 0.2500 0.3533(17) 0.060(7) Uiso 0.04 2 d SP M 6 Sb1A Sb 0.9807(17) 0.2500 0.4725(15) 0.035(7) Uiso 0.03 2 d SP . 5 Sb2A Sb 0.8310(15) 0.2500 0.3569(14) 0.030(6) Uiso 0.03 2 d SP . 5 Sb3A Sb 1.1629(13) 0.3159(8) 0.4470(12) 0.041(5) Uiso 0.03 1 d P . 5 Sb4A Sb 1.1908(14) 0.3731(8) 0.3058(12) 0.046(6) Uiso 0.03 1 d P . 5 Sb5A Sb 1.2164(13) 0.3111(8) 0.1633(12) 0.044(5) Uiso 0.03 1 d P . 5 Sb6A Sb 1.0386(12) 0.3742(7) 0.1887(11) 0.036(5) Uiso 0.03 1 d P . 5 Sb7A Sb 0.8666(10) 0.3138(6) 0.2141(9) 0.025(3) Uiso 0.03 1 d P . 5 O4A O 1.1839 0.2500 0.3373 0.030 Uiso 0.05 2 d SP N 5 O5A O 1.0303 0.2500 0.2198 0.030 Uiso 0.04 2 d SP O 5 O12A O 1.0055 0.3131 0.3636 0.030 Uiso 0.03 1 d P P 5 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 Sb1 0.0242(3) 0.0219(3) 0.0302(4) 0.000 0.0018(3) 0.000 Sb2 0.0195(3) 0.0197(3) 0.0349(4) 0.000 0.0014(2) 0.000 Sb3 0.0228(2) 0.0188(2) 0.0306(3) -0.00120(18) -0.00313(18) 0.00000(14) Sb4 0.0190(2) 0.01651(19) 0.0342(3) 0.00028(17) -0.00102(17) -0.00065(13) Sb5 0.0211(2) 0.0218(2) 0.0330(3) 0.00234(17) 0.00163(18) -0.00038(14) Sb6 0.0208(2) 0.0204(2) 0.0334(3) 0.00388(17) -0.00112(18) 0.00060(14) Sb7 0.01834(19) 0.0219(2) 0.0350(3) 0.00158(17) -0.00214(18) 0.00117(14) Zn1 0.0177(4) 0.0175(4) 0.0351(5) 0.000 -0.0011(4) 0.000 Zn2 0.0229(3) 0.0202(3) 0.0401(4) -0.0006(3) 0.0002(3) 0.0022(3) Zn3 0.0172(4) 0.0195(4) 0.0373(5) 0.000 -0.0011(4) 0.000 Zn4 0.0267(6) 0.0294(6) 0.0377(6) 0.000 -0.0020(5) 0.000 Cl1 0.166(6) 0.201(7) 0.122(4) 0.000 0.110(5) 0.000 Cl2 0.079(3) 0.152(5) 0.103(3) 0.000 0.060(3) 0.000 Cl3 0.0629(13) 0.0498(11) 0.0783(15) -0.0271(10) -0.0224(11) -0.0081(10) Cl4 0.0813(17) 0.0523(13) 0.130(2) -0.0222(14) -0.0324(17) -0.0286(12) Cl5 0.0736(16) 0.100(2) 0.0658(14) 0.0219(14) 0.0340(12) 0.0014(14) Cl6 0.161(3) 0.092(2) 0.117(3) 0.057(2) -0.019(2) 0.060(2) Cl7 0.0722(14) 0.0720(15) 0.0640(13) 0.0183(11) -0.0014(11) 0.0425(12) Cl21 0.052(3) 0.0307(16) 0.063(4) -0.0034(19) 0.014(2) 0.0121(16) Br21 0.052(3) 0.0307(16) 0.063(4) -0.0034(19) 0.014(2) 0.0121(16) Cl31 0.0217(11) 0.0513(10) 0.073(10) 0.000 -0.0079(19) 0.000 Br31 0.0217(11) 0.0513(10) 0.073(10) 0.000 -0.0079(19) 0.000 Cl41 0.027(2) 0.0664(18) 0.0412(14) 0.000 -0.008(2) 0.000 Br41 0.027(2) 0.0664(18) 0.0412(14) 0.000 -0.008(2) 0.000 O1 0.022(2) 0.025(2) 0.047(3) 0.0028(18) 0.0020(18) 0.0062(16) O2 0.023(2) 0.0213(19) 0.042(2) -0.0025(17) 0.0002(17) -0.0005(16) O3 0.031(2) 0.025(2) 0.034(2) -0.0074(17) 0.0021(17) -0.0001(17) O4 0.020(3) 0.014(2) 0.027(3) 0.000 -0.002(2) 0.000 O5 0.016(3) 0.016(3) 0.035(3) 0.000 -0.003(2) 0.000 O6 0.033(3) 0.018(3) 0.035(3) 0.000 -0.013(3) 0.000 O7 0.027(3) 0.028(3) 0.040(3) 0.000 -0.009(3) 0.000 O8 0.0227(19) 0.0184(18) 0.039(2) 0.0001(17) -0.0010(17) 0.0017(15) O9 0.0223(19) 0.0221(19) 0.039(2) 0.0008(17) -0.0017(17) -0.0029(16) O10 0.025(2) 0.0187(18) 0.029(2) -0.0007(15) -0.0003(16) 0.0010(15) O11 0.022(2) 0.028(2) 0.042(2) -0.0020(18) -0.0013(17) 0.0007(16) O12 0.0169(18) 0.0162(18) 0.027(2) 0.0008(15) 0.0005(15) 0.0002(14) O13 0.026(2) 0.0171(19) 0.046(2) -0.0003(17) -0.0026(18) 0.0012(16) O14 0.021(3) 0.033(3) 0.041(3) 0.000 0.001(2) 0.000 O15 0.027(3) 0.021(3) 0.037(3) 0.000 0.002(2) 0.000 O16 0.021(2) 0.025(2) 0.041(2) 0.0005(18) 0.0011(17) -0.0058(16) O17 0.029(2) 0.027(2) 0.035(2) 0.0062(18) 0.0000(17) 0.0032(17) C11 0.043(6) 0.047(6) 0.044(6) 0.000 0.002(4) 0.000 C12 0.056(11) 0.059(11) 0.052(10) -0.016(8) 0.020(8) -0.009(9) C12A 0.042(9) 0.041(8) 0.047(9) -0.015(7) 0.010(7) -0.006(7) C13 0.080(16) 0.087(17) 0.070(15) -0.024(13) 0.037(12) -0.024(14) C13A 0.058(12) 0.050(10) 0.071(13) -0.015(9) 0.022(10) -0.003(9) C14 0.094(12) 0.130(15) 0.053(8) 0.000 0.056(8) 0.000 C21 0.035(5) 0.026(4) 0.043(5) 0.000 0.005(4) 0.000 C22 0.042(8) 0.040(8) 0.047(8) -0.005(6) 0.007(7) 0.018(6) C22A 0.050(10) 0.042(8) 0.073(12) 0.000(8) 0.025(9) 0.006(7) C23 0.056(10) 0.050(10) 0.061(10) -0.003(8) 0.013(9) 0.021(8) C23A 0.061(12) 0.051(10) 0.090(15) 0.002(10) 0.048(11) 0.004(9) C24 0.036(6) 0.097(11) 0.072(9) 0.000 0.024(6) 0.000 C31 0.026(3) 0.026(3) 0.048(4) -0.004(3) -0.002(3) -0.002(2) C32 0.034(3) 0.029(3) 0.049(4) -0.005(3) -0.005(3) 0.002(3) C33 0.047(4) 0.028(3) 0.045(4) -0.008(3) -0.001(3) -0.002(3) C34 0.050(4) 0.039(4) 0.042(4) -0.015(3) -0.016(3) -0.007(3) C35 0.038(4) 0.043(4) 0.052(4) -0.009(3) -0.010(3) -0.003(3) C36 0.035(3) 0.030(3) 0.043(4) -0.006(3) -0.005(3) -0.001(3) C41 0.030(3) 0.024(3) 0.052(4) -0.002(3) -0.006(3) -0.003(2) C42 0.030(3) 0.023(3) 0.063(4) -0.004(3) -0.003(3) -0.001(3) C43 0.049(4) 0.028(3) 0.063(5) -0.008(3) -0.001(4) 0.000(3) C44 0.047(4) 0.034(4) 0.068(5) -0.005(3) -0.009(4) -0.018(3) C45 0.037(4) 0.041(4) 0.086(6) -0.009(4) -0.011(4) -0.012(3) C46 0.031(3) 0.040(4) 0.055(4) -0.002(3) -0.005(3) -0.002(3) C51 0.034(3) 0.032(3) 0.037(3) 0.008(3) 0.003(3) 0.003(3) C52 0.036(4) 0.062(5) 0.045(4) 0.002(4) 0.007(3) -0.011(3) C53 0.039(4) 0.067(5) 0.055(5) 0.005(4) 0.013(3) -0.008(4) C54 0.062(5) 0.059(5) 0.051(5) 0.012(4) 0.024(4) 0.005(4) C55 0.060(5) 0.079(6) 0.038(4) 0.014(4) 0.007(4) 0.012(5) C56 0.045(4) 0.054(5) 0.051(4) 0.006(4) 0.006(3) 0.005(4) C61 0.028(3) 0.032(3) 0.042(4) 0.014(3) -0.002(3) 0.004(3) C62 0.092(7) 0.048(5) 0.048(5) 0.005(4) -0.013(4) 0.019(5) C63 0.129(10) 0.071(7) 0.051(5) 0.011(5) -0.025(6) 0.034(7) C64 0.067(6) 0.064(6) 0.078(6) 0.043(5) -0.001(5) 0.025(5) C65 0.110(9) 0.043(5) 0.094(8) 0.014(5) -0.011(7) 0.031(5) C66 0.095(7) 0.035(4) 0.057(5) 0.000(4) -0.022(5) 0.019(4) C71 0.025(3) 0.035(3) 0.035(3) 0.004(3) -0.001(2) 0.000(2) C72 0.083(6) 0.048(5) 0.050(5) -0.003(4) -0.010(4) 0.033(4) C73 0.096(7) 0.058(6) 0.058(5) -0.004(4) -0.004(5) 0.044(5) C74 0.037(4) 0.051(4) 0.057(5) 0.018(4) -0.002(3) 0.022(3) C75 0.053(5) 0.064(5) 0.045(4) 0.004(4) -0.013(4) 0.019(4) C76 0.051(5) 0.041(4) 0.063(5) -0.007(4) -0.013(4) 0.014(4) N1 0.061(5) 0.049(4) 0.106(7) 0.029(4) 0.029(4) 0.004(4) C1 0.102(9) 0.102(9) 0.080(8) 0.015(7) 0.012(7) 0.004(8) C2 0.090(8) 0.104(9) 0.088(8) 0.026(7) -0.018(6) -0.017(7) C3 0.085(8) 0.092(8) 0.103(9) 0.032(7) -0.025(7) -0.035(7) C4 0.075(7) 0.091(8) 0.084(7) 0.011(6) 0.025(6) 0.006(6) C5 0.057(6) 0.087(7) 0.069(6) 0.012(5) 0.000(5) -0.004(5) C6 0.085(7) 0.061(6) 0.090(8) 0.004(6) 0.023(6) -0.005(5) C7 0.077(7) 0.064(6) 0.078(7) 0.012(5) 0.010(5) 0.014(5) C8 0.109(10) 0.103(10) 0.078(8) 0.022(7) -0.009(7) 0.020(8) C9 0.100(9) 0.088(8) 0.095(9) 0.020(7) -0.010(7) 0.014(7) C10 0.061(6) 0.122(11) 0.098(9) 0.011(8) -0.007(6) 0.006(7) N2 0.069(7) 0.241(17) 0.072(7) 0.032(8) -0.015(5) -0.006(9) C2A 0.105(10) 0.087(8) 0.067(7) 0.008(6) -0.008(7) -0.001(7) C2B 0.098(10) 0.131(12) 0.096(9) 0.020(8) 0.001(8) 0.018(9) N3 0.103(14) 0.125(16) 0.19(2) 0.000 0.014(14) 0.000 C3A 0.12(2) 0.079(13) 0.18(2) 0.000 -0.021(18) 0.000 C3B 0.054(11) 0.091(14) 0.31(4) 0.000 0.018(16) 0.000 N4 0.069(8) 0.063(8) 0.120(12) 0.000 0.026(8) 0.000 C4A 0.060(9) 0.052(8) 0.117(14) 0.000 0.031(9) 0.000 C4B 0.063(9) 0.105(13) 0.081(11) 0.000 0.007(8) 0.000 N5 0.088(11) 0.27(2) 0.188(18) -0.134(17) 0.011(10) -0.079(13) C5A 0.068(11) 0.123(15) 0.23(3) -0.128(18) 0.032(12) -0.043(10) C5B 0.074(10) 0.096(11) 0.32(3) -0.097(16) 0.067(14) -0.028(9) N6 0.069(6) 0.072(6) 0.129(9) -0.006(6) 0.016(6) 0.003(5) C6A 0.061(6) 0.065(6) 0.097(8) -0.014(6) -0.007(6) 0.006(5) C6B 0.105(10) 0.091(9) 0.102(9) -0.025(7) 0.032(8) -0.019(7) _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 Sb1 O3 1.955(4) . ? Sb1 O3 1.955(4) 4_565 ? Sb1 O2 2.026(4) 4_565 ? Sb1 O2 2.026(4) . ? Sb1 C11 2.097(11) . ? Sb1 O5 2.174(6) . ? Sb1 Sb2 3.1245(10) . ? Sb1 Sb3 3.1844(7) . ? Sb1 Sb3 3.1844(7) 4_565 ? Sb2 O1 1.954(4) 4_565 ? Sb2 O1 1.954(4) . ? Sb2 O2 2.020(4) . ? Sb2 O2 2.020(4) 4_565 ? Sb2 C21 2.109(9) . ? Sb2 O4 2.212(6) . ? Sb2 Sb7 3.1973(9) 4_565 ? Sb2 Sb7 3.1973(9) . ? Sb3 O3 1.943(4) . ? Sb3 O6 1.952(3) . ? Sb3 O10 2.021(4) . ? Sb3 O8 2.025(4) . ? Sb3 C31 2.097(6) . ? Sb3 O5 2.200(4) . ? Sb3 Sb4 3.1108(7) . ? Sb3 Sb3 3.1906(8) 4_565 ? Sb4 O13 1.953(4) . ? Sb4 O16 1.955(4) . ? Sb4 O10 2.009(4) . ? Sb4 O8 2.011(4) . ? Sb4 C41 2.099(6) . ? Sb4 O12 2.175(4) . ? Sb4 Sb5 3.1789(7) . ? Sb4 Sb6 3.1816(6) . ? Sb5 O16 1.948(4) . ? Sb5 O17 1.956(4) . ? Sb5 O14 2.004(4) . ? Sb5 O15 2.023(4) . ? Sb5 C51 2.099(7) . ? Sb5 O12 2.210(4) . ? Sb5 Sb5 3.1118(8) 4_565 ? Sb5 Sb6 3.2038(6) . ? Sb6 O13 1.948(4) . ? Sb6 O17 1.949(4) . ? Sb6 O9 2.017(4) . ? Sb6 O11 2.026(4) . ? Sb6 C61 2.105(6) . ? Sb6 O12 2.200(4) . ? Sb6 Sb7 3.1217(6) . ? Sb7 O1 1.946(5) . ? Sb7 O7 1.956(3) . ? Sb7 O9 2.013(4) . ? Sb7 O11 2.031(4) . ? Sb7 C71 2.109(6) . ? Sb7 O4 2.182(4) . ? Sb7 Sb7 3.1830(8) 4_565 ? Zn1 O12 2.012(4) . ? Zn1 O12 2.012(4) 4_565 ? Zn1 O5 2.023(6) . ? Zn1 O4 2.025(6) . ? Zn2 O2 2.011(4) . ? Zn2 O8 2.017(4) . ? Zn2 O9 2.023(4) . ? Zn2 Cl21 2.218(19) . ? Zn2 Br21 2.288(9) . ? Zn3 O15 2.005(6) . ? Zn3 O10 2.013(4) . ? Zn3 O10 2.013(4) 4_565 ? Zn3 Cl31 2.22(2) . ? Zn3 Br31 2.284(13) . ? Zn4 O11 2.014(4) . ? Zn4 O11 2.014(4) 4_565 ? Zn4 O14 2.023(6) . ? Zn4 Cl41 2.212(5) . ? Zn4 Br41 2.257(13) . ? Cl1 C14 1.735(12) . ? Cl2 C24 1.756(12) . ? Cl3 C34 1.733(7) . ? Cl4 C44 1.744(7) . ? Cl5 C54 1.746(8) . ? Cl6 C64 1.745(8) . ? Cl7 C74 1.738(7) . ? O4 Sb7 2.182(4) 4_565 ? O5 Sb3 2.200(4) 4_565 ? O6 Sb3 1.952(3) 4_565 ? O7 Sb7 1.956(3) 4_565 ? O14 Sb5 2.004(4) 4_565 ? O15 Sb5 2.023(4) 4_565 ? C11 C12 1.286(18) . ? C11 C12 1.286(18) 4_565 ? C11 C12A 1.492(17) 4_565 ? C11 C12A 1.492(17) . ? C11 Sb1A 2.55(3) . ? C12 C13 1.41(3) . ? C12A C13A 1.38(2) . ? C13 C14 1.22(2) . ? C13A C14 1.57(2) . ? C14 C13 1.22(2) 4_565 ? C14 C13A 1.57(2) 4_565 ? C21 C22A 1.348(17) 4_565 ? C21 C22A 1.348(17) . ? C21 C22 1.432(16) . ? C21 C22 1.432(16) 4_565 ? C21 Sb2A 2.55(3) . ? C22 C23 1.40(2) . ? C22A C23A 1.41(2) . ? C23 C24 1.47(2) . ? C23A C24 1.25(2) . ? C24 C23A 1.25(2) 4_565 ? C24 C23 1.47(2) 4_565 ? C31 C32 1.393(9) . ? C31 C36 1.401(9) . ? C32 C33 1.395(9) . ? C33 C34 1.359(10) . ? C34 C35 1.391(10) . ? C35 C36 1.396(9) . ? C41 C42 1.391(9) . ? C41 C46 1.394(9) . ? C42 C43 1.375(9) . ? C43 C44 1.365(11) . ? C44 C45 1.366(11) . ? C45 C46 1.376(10) . ? C51 C52 1.380(10) . ? C51 C56 1.384(10) . ? C52 C53 1.391(10) . ? C53 C54 1.361(12) . ? C54 C55 1.391(13) . ? C55 C56 1.371(11) . ? C61 C66 1.376(10) . ? C61 C62 1.382(11) . ? C62 C63 1.388(11) . ? C63 C64 1.355(15) . ? C64 C65 1.377(15) . ? C65 C66 1.380(11) . ? C71 C76 1.372(10) . ? C71 C72 1.374(10) . ? C72 C73 1.381(11) . ? C73 C74 1.397(12) . ? C74 C75 1.347(12) . ? C75 C76 1.387(10) . ? N1 C1 1.472(14) . ? N1 C3 1.480(13) . ? N1 C2 1.525(13) . ? N1 C4 1.562(14) . ? C4 C5 1.510(15) . ? C5 C6 1.398(14) . ? C5 C10 1.415(14) . ? C6 C7 1.469(15) . ? C7 C8 1.361(17) . ? C8 C9 1.462(18) . ? C9 C10 1.420(16) . ? N2 C2A 1.134(16) . ? C2A C2B 1.537(19) . ? N3 C3A 1.29(3) . ? C3A C3B 1.42(3) . ? N4 C4A 1.19(2) . ? C4A C4B 1.41(2) . ? N5 C5A 1.11(3) . ? C5A C5B 1.51(3) . ? N6 C6A 1.156(14) . ? C6A C6B 1.415(16) . ? Sb1A Sb2A 3.11(4) . ? Sb1A Sb3A 3.29(3) . ? Sb1A Sb3A 3.29(3) 4_565 ? Sb2A Sb7A 3.23(3) 4_565 ? Sb2A Sb7A 3.23(3) . ? Sb3A Sb4A 3.10(3) . ? Sb3A Sb3A 3.30(4) 4_565 ? Sb4A Sb6A 3.15(3) . ? Sb4A Sb5A 3.17(3) . ? Sb5A Sb5A 3.06(4) 4_565 ? Sb5A Sb6A 3.20(3) . ? Sb6A Sb7A 3.09(2) . ? Sb7A Sb7A 3.20(3) 4_565 ? 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 Sb1 O3 97.4(2) . 4_565 ? O3 Sb1 O2 160.95(18) . 4_565 ? O3 Sb1 O2 90.26(17) 4_565 4_565 ? O3 Sb1 O2 90.26(17) . . ? O3 Sb1 O2 160.95(18) 4_565 . ? O2 Sb1 O2 77.5(2) 4_565 . ? O3 Sb1 C11 96.5(2) . . ? O3 Sb1 C11 96.5(2) 4_565 . ? O2 Sb1 C11 99.9(3) 4_565 . ? O2 Sb1 C11 99.9(3) . . ? O3 Sb1 O5 78.58(16) . . ? O3 Sb1 O5 78.58(16) 4_565 . ? O2 Sb1 O5 85.96(16) 4_565 . ? O2 Sb1 O5 85.96(16) . . ? C11 Sb1 O5 172.5(3) . . ? O3 Sb1 Sb2 129.58(13) . . ? O3 Sb1 Sb2 129.58(13) 4_565 . ? O2 Sb1 Sb2 39.37(11) 4_565 . ? O2 Sb1 Sb2 39.37(11) . . ? C11 Sb1 Sb2 95.1(3) . . ? O5 Sb1 Sb2 92.40(15) . . ? O3 Sb1 Sb3 35.09(12) . . ? O3 Sb1 Sb3 86.25(12) 4_565 . ? O2 Sb1 Sb3 129.11(12) 4_565 . ? O2 Sb1 Sb3 90.21(11) . . ? C11 Sb1 Sb3 131.0(2) . . ? O5 Sb1 Sb3 43.61(10) . . ? Sb2 Sb1 Sb3 120.27(3) . . ? O3 Sb1 Sb3 86.25(12) . 4_565 ? O3 Sb1 Sb3 35.09(12) 4_565 4_565 ? O2 Sb1 Sb3 90.21(11) 4_565 4_565 ? O2 Sb1 Sb3 129.11(12) . 4_565 ? C11 Sb1 Sb3 131.0(2) . 4_565 ? O5 Sb1 Sb3 43.61(10) . 4_565 ? Sb2 Sb1 Sb3 120.27(3) . 4_565 ? Sb3 Sb1 Sb3 60.129(18) . 4_565 ? O1 Sb2 O1 97.0(3) 4_565 . ? O1 Sb2 O2 160.27(17) 4_565 . ? O1 Sb2 O2 90.04(17) . . ? O1 Sb2 O2 90.04(17) 4_565 4_565 ? O1 Sb2 O2 160.27(17) . 4_565 ? O2 Sb2 O2 77.8(2) . 4_565 ? O1 Sb2 C21 97.5(2) 4_565 . ? O1 Sb2 C21 97.5(2) . . ? O2 Sb2 C21 99.8(2) . . ? O2 Sb2 C21 99.8(2) 4_565 . ? O1 Sb2 O4 77.68(16) 4_565 . ? O1 Sb2 O4 77.68(16) . . ? O2 Sb2 O4 85.94(16) . . ? O2 Sb2 O4 85.94(16) 4_565 . ? C21 Sb2 O4 172.6(3) . . ? O1 Sb2 Sb1 129.46(13) 4_565 . ? O1 Sb2 Sb1 129.46(13) . . ? O2 Sb2 Sb1 39.51(12) . . ? O2 Sb2 Sb1 39.51(12) 4_565 . ? C21 Sb2 Sb1 95.0(3) . . ? O4 Sb2 Sb1 92.40(14) . . ? O1 Sb2 Sb7 34.85(13) 4_565 4_565 ? O1 Sb2 Sb7 85.71(13) . 4_565 ? O2 Sb2 Sb7 128.39(12) . 4_565 ? O2 Sb2 Sb7 89.78(12) 4_565 4_565 ? C21 Sb2 Sb7 131.8(2) . 4_565 ? O4 Sb2 Sb7 42.93(10) . 4_565 ? Sb1 Sb2 Sb7 119.686(19) . 4_565 ? O1 Sb2 Sb7 85.71(13) 4_565 . ? O1 Sb2 Sb7 34.85(13) . . ? O2 Sb2 Sb7 89.78(12) . . ? O2 Sb2 Sb7 128.39(12) 4_565 . ? C21 Sb2 Sb7 131.8(2) . . ? O4 Sb2 Sb7 42.93(10) . . ? Sb1 Sb2 Sb7 119.686(19) . . ? Sb7 Sb2 Sb7 59.70(2) 4_565 . ? O3 Sb3 O6 97.6(2) . . ? O3 Sb3 O10 160.28(17) . . ? O6 Sb3 O10 90.2(2) . . ? O3 Sb3 O8 89.94(17) . . ? O6 Sb3 O8 161.01(19) . . ? O10 Sb3 O8 77.58(16) . . ? O3 Sb3 C31 99.6(2) . . ? O6 Sb3 C31 96.4(2) . . ? O10 Sb3 C31 97.5(2) . . ? O8 Sb3 C31 99.6(2) . . ? O3 Sb3 O5 78.18(19) . . ? O6 Sb3 O5 78.62(17) . . ? O10 Sb3 O5 85.67(19) . . ? O8 Sb3 O5 85.94(15) . . ? C31 Sb3 O5 174.1(2) . . ? O3 Sb3 Sb4 129.24(13) . . ? O6 Sb3 Sb4 129.45(19) . . ? O10 Sb3 Sb4 39.33(11) . . ? O8 Sb3 Sb4 39.40(12) . . ? C31 Sb3 Sb4 93.66(19) . . ? O5 Sb3 Sb4 91.94(14) . . ? O3 Sb3 Sb1 35.35(12) . . ? O6 Sb3 Sb1 86.27(16) . . ? O10 Sb3 Sb1 128.16(11) . . ? O8 Sb3 Sb1 89.94(11) . . ? C31 Sb3 Sb1 134.30(19) . . ? O5 Sb3 Sb1 42.96(15) . . ? Sb4 Sb3 Sb1 119.44(2) . . ? O3 Sb3 Sb3 86.28(12) . 4_565 ? O6 Sb3 Sb3 35.19(13) . 4_565 ? O10 Sb3 Sb3 89.80(10) . 4_565 ? O8 Sb3 Sb3 128.99(11) . 4_565 ? C31 Sb3 Sb3 131.23(18) . 4_565 ? O5 Sb3 Sb3 43.53(10) . 4_565 ? Sb4 Sb3 Sb3 119.675(11) . 4_565 ? Sb1 Sb3 Sb3 59.936(9) . 4_565 ? O13 Sb4 O16 97.34(18) . . ? O13 Sb4 O10 161.70(16) . . ? O16 Sb4 O10 89.98(17) . . ? O13 Sb4 O8 90.58(17) . . ? O16 Sb4 O8 162.50(16) . . ? O10 Sb4 O8 78.17(16) . . ? O13 Sb4 C41 96.2(2) . . ? O16 Sb4 C41 95.1(2) . . ? O10 Sb4 C41 99.8(2) . . ? O8 Sb4 C41 99.5(2) . . ? O13 Sb4 O12 78.83(15) . . ? O16 Sb4 O12 79.28(15) . . ? O10 Sb4 O12 86.13(15) . . ? O8 Sb4 O12 87.03(15) . . ? C41 Sb4 O12 171.9(2) . . ? O13 Sb4 Sb3 130.25(13) . . ? O16 Sb4 Sb3 129.57(12) . . ? O10 Sb4 Sb3 39.60(11) . . ? O8 Sb4 Sb3 39.73(11) . . ? C41 Sb4 Sb3 95.08(19) . . ? O12 Sb4 Sb3 92.99(10) . . ? O13 Sb4 Sb5 86.65(13) . . ? O16 Sb4 Sb5 35.39(12) . . ? O10 Sb4 Sb5 89.75(11) . . ? O8 Sb4 Sb5 130.51(11) . . ? C41 Sb4 Sb5 129.9(2) . . ? O12 Sb4 Sb5 43.98(10) . . ? Sb3 Sb4 Sb5 120.515(16) . . ? O13 Sb4 Sb6 35.30(12) . . ? O16 Sb4 Sb6 86.56(12) . . ? O10 Sb4 Sb6 129.40(11) . . ? O8 Sb4 Sb6 91.06(12) . . ? C41 Sb4 Sb6 130.78(18) . . ? O12 Sb4 Sb6 43.66(10) . . ? Sb3 Sb4 Sb6 121.077(17) . . ? Sb5 Sb4 Sb6 60.491(15) . . ? O16 Sb5 O17 97.17(18) . . ? O16 Sb5 O14 161.7(2) . . ? O17 Sb5 O14 90.28(18) . . ? O16 Sb5 O15 90.30(18) . . ? O17 Sb5 O15 161.0(2) . . ? O14 Sb5 O15 77.85(19) . . ? O16 Sb5 C51 95.4(2) . . ? O17 Sb5 C51 95.8(2) . . ? O14 Sb5 C51 100.5(3) . . ? O15 Sb5 C51 100.9(2) . . ? O16 Sb5 O12 78.55(16) . . ? O17 Sb5 O12 77.95(16) . . ? O14 Sb5 O12 86.7(2) . . ? O15 Sb5 O12 86.53(19) . . ? C51 Sb5 O12 170.5(2) . . ? O16 Sb5 Sb5 129.91(12) . 4_565 ? O17 Sb5 Sb5 129.21(13) . 4_565 ? O14 Sb5 Sb5 39.08(13) . 4_565 ? O15 Sb5 Sb5 39.71(13) . 4_565 ? C51 Sb5 Sb5 97.25(18) . 4_565 ? O12 Sb5 Sb5 92.25(10) . 4_565 ? O16 Sb5 Sb4 35.55(12) . . ? O17 Sb5 Sb4 85.94(13) . . ? O14 Sb5 Sb4 129.31(18) . . ? O15 Sb5 Sb4 90.18(15) . . ? C51 Sb5 Sb4 130.14(19) . . ? O12 Sb5 Sb4 43.09(10) . . ? Sb5 Sb5 Sb4 119.793(11) 4_565 . ? O16 Sb5 Sb6 86.05(12) . . ? O17 Sb5 Sb6 34.79(13) . . ? O14 Sb5 Sb6 90.70(14) . . ? O15 Sb5 Sb6 129.38(17) . . ? C51 Sb5 Sb6 129.70(17) . . ? O12 Sb5 Sb6 43.29(10) . . ? Sb5 Sb5 Sb6 119.850(10) 4_565 . ? Sb4 Sb5 Sb6 59.796(14) . . ? O13 Sb6 O17 97.36(18) . . ? O13 Sb6 O9 89.79(17) . . ? O17 Sb6 O9 160.77(17) . . ? O13 Sb6 O11 161.01(18) . . ? O17 Sb6 O11 90.31(18) . . ? O9 Sb6 O11 77.89(17) . . ? O13 Sb6 C61 97.0(2) . . ? O17 Sb6 C61 95.7(2) . . ? O9 Sb6 C61 101.2(2) . . ? O11 Sb6 C61 99.5(2) . . ? O13 Sb6 O12 78.31(15) . . ? O17 Sb6 O12 78.37(16) . . ? O9 Sb6 O12 85.70(15) . . ? O11 Sb6 O12 86.33(15) . . ? C61 Sb6 O12 171.8(2) . . ? O13 Sb6 Sb7 128.90(13) . . ? O17 Sb6 Sb7 129.95(13) . . ? O9 Sb6 Sb7 39.20(11) . . ? O11 Sb6 Sb7 39.76(12) . . ? C61 Sb6 Sb7 96.27(17) . . ? O12 Sb6 Sb7 91.94(10) . . ? O13 Sb6 Sb4 35.40(12) . . ? O17 Sb6 Sb4 85.99(12) . . ? O9 Sb6 Sb4 89.68(12) . . ? O11 Sb6 Sb4 128.89(12) . . ? C61 Sb6 Sb4 131.62(19) . . ? O12 Sb6 Sb4 43.03(10) . . ? Sb7 Sb6 Sb4 119.26(2) . . ? O13 Sb6 Sb5 86.03(12) . . ? O17 Sb6 Sb5 34.95(12) . . ? O9 Sb6 Sb5 128.83(12) . . ? O11 Sb6 Sb5 90.51(12) . . ? C61 Sb6 Sb5 129.96(18) . . ? O12 Sb6 Sb5 43.54(10) . . ? Sb7 Sb6 Sb5 120.184(16) . . ? Sb4 Sb6 Sb5 59.713(14) . . ? O1 Sb7 O7 97.1(2) . . ? O1 Sb7 O9 90.54(18) . . ? O7 Sb7 O9 161.56(19) . . ? O1 Sb7 O11 161.57(17) . . ? O7 Sb7 O11 90.3(2) . . ? O9 Sb7 O11 77.83(17) . . ? O1 Sb7 C71 97.1(2) . . ? O7 Sb7 C71 97.9(2) . . ? O9 Sb7 C71 97.7(2) . . ? O11 Sb7 C71 98.6(2) . . ? O1 Sb7 O4 78.61(19) . . ? O7 Sb7 O4 78.61(17) . . ? O9 Sb7 O4 86.54(15) . . ? O11 Sb7 O4 86.36(19) . . ? C71 Sb7 O4 174.0(2) . . ? O1 Sb7 Sb6 129.75(13) . . ? O7 Sb7 Sb6 129.82(19) . . ? O9 Sb7 Sb6 39.28(12) . . ? O11 Sb7 Sb6 39.63(12) . . ? C71 Sb7 Sb6 93.43(17) . . ? O4 Sb7 Sb6 92.50(13) . . ? O1 Sb7 Sb7 86.25(12) . 4_565 ? O7 Sb7 Sb7 35.55(14) . 4_565 ? O9 Sb7 Sb7 129.20(11) . 4_565 ? O11 Sb7 Sb7 90.08(12) . 4_565 ? C71 Sb7 Sb7 132.98(17) . 4_565 ? O4 Sb7 Sb7 43.16(10) . 4_565 ? Sb6 Sb7 Sb7 119.962(10) . 4_565 ? O1 Sb7 Sb2 35.03(12) . . ? O7 Sb7 Sb2 86.29(17) . . ? O9 Sb7 Sb2 90.51(12) . . ? O11 Sb7 Sb2 129.60(12) . . ? C71 Sb7 Sb2 131.74(17) . . ? O4 Sb7 Sb2 43.69(15) . . ? Sb6 Sb7 Sb2 120.268(19) . . ? Sb7 Sb7 Sb2 60.148(11) 4_565 . ? O12 Zn1 O12 109.4(2) . 4_565 ? O12 Zn1 O5 109.67(14) . . ? O12 Zn1 O5 109.67(14) 4_565 . ? O12 Zn1 O4 109.20(14) . . ? O12 Zn1 O4 109.20(14) 4_565 . ? O5 Zn1 O4 109.6(2) . . ? O2 Zn2 O8 104.71(16) . . ? O2 Zn2 O9 105.33(17) . . ? O8 Zn2 O9 105.12(17) . . ? O2 Zn2 Cl21 116.3(5) . . ? O8 Zn2 Cl21 112.2(8) . . ? O9 Zn2 Cl21 112.3(7) . . ? O2 Zn2 Br21 109.5(2) . . ? O8 Zn2 Br21 114.3(4) . . ? O9 Zn2 Br21 116.8(4) . . ? Cl21 Zn2 Br21 6.9(7) . . ? O15 Zn3 O10 104.47(15) . . ? O15 Zn3 O10 104.47(15) . 4_565 ? O10 Zn3 O10 104.2(2) . 4_565 ? O15 Zn3 Cl31 111(2) . . ? O10 Zn3 Cl31 115.6(10) . . ? O10 Zn3 Cl31 115.6(10) 4_565 . ? O15 Zn3 Br31 115.8(11) . . ? O10 Zn3 Br31 113.4(6) . . ? O10 Zn3 Br31 113.4(6) 4_565 . ? Cl31 Zn3 Br31 4(3) . . ? O11 Zn4 O11 104.7(3) . 4_565 ? O11 Zn4 O14 107.05(16) . . ? O11 Zn4 O14 107.05(16) 4_565 . ? O11 Zn4 Cl41 118.82(14) . . ? O11 Zn4 Cl41 118.82(14) 4_565 . ? O14 Zn4 Cl41 99.2(2) . . ? O11 Zn4 Br41 112.8(2) . . ? O11 Zn4 Br41 112.8(2) 4_565 . ? O14 Zn4 Br41 111.9(3) . . ? Cl41 Zn4 Br41 12.7(3) . . ? Sb7 O1 Sb2 110.12(19) . . ? Zn2 O2 Sb2 126.1(2) . . ? Zn2 O2 Sb1 126.2(2) . . ? Sb2 O2 Sb1 101.12(18) . . ? Sb3 O3 Sb1 109.56(19) . . ? Zn1 O4 Sb7 123.10(17) . 4_565 ? Zn1 O4 Sb7 123.10(17) . . ? Sb7 O4 Sb7 93.7(2) 4_565 . ? Zn1 O4 Sb2 122.1(3) . . ? Sb7 O4 Sb2 93.38(18) 4_565 . ? Sb7 O4 Sb2 93.38(18) . . ? Zn1 O5 Sb1 123.5(3) . . ? Zn1 O5 Sb3 122.64(18) . . ? Sb1 O5 Sb3 93.43(19) . . ? Zn1 O5 Sb3 122.64(18) . 4_565 ? Sb1 O5 Sb3 93.43(19) . 4_565 ? Sb3 O5 Sb3 92.9(2) . 4_565 ? Sb3 O6 Sb3 109.6(3) 4_565 . ? Sb7 O7 Sb7 108.9(3) . 4_565 ? Sb4 O8 Zn2 125.4(2) . . ? Sb4 O8 Sb3 100.86(17) . . ? Zn2 O8 Sb3 126.4(2) . . ? Sb7 O9 Sb6 101.53(19) . . ? Sb7 O9 Zn2 125.4(2) . . ? Sb6 O9 Zn2 126.3(2) . . ? Sb4 O10 Zn3 126.8(2) . . ? Sb4 O10 Sb3 101.06(17) . . ? Zn3 O10 Sb3 126.29(19) . . ? Zn4 O11 Sb6 124.6(2) . . ? Zn4 O11 Sb7 126.8(2) . . ? Sb6 O11 Sb7 100.61(19) . . ? Zn1 O12 Sb4 122.76(19) . . ? Zn1 O12 Sb6 123.26(18) . . ? Sb4 O12 Sb6 93.32(14) . . ? Zn1 O12 Sb5 123.02(18) . . ? Sb4 O12 Sb5 92.93(14) . . ? Sb6 O12 Sb5 93.17(14) . . ? Sb6 O13 Sb4 109.29(19) . . ? Sb5 O14 Sb5 101.8(3) . 4_565 ? Sb5 O14 Zn4 125.04(16) . . ? Sb5 O14 Zn4 125.04(16) 4_565 . ? Zn3 O15 Sb5 126.09(16) . 4_565 ? Zn3 O15 Sb5 126.09(16) . . ? Sb5 O15 Sb5 100.6(3) 4_565 . ? Sb5 O16 Sb4 109.07(19) . . ? Sb6 O17 Sb5 110.3(2) . . ? C12 C11 C12 98.8(19) . 4_565 ? C12 C11 C12A 120.5(12) . 4_565 ? C12 C11 C12A 39.3(10) 4_565 4_565 ? C12 C11 C12A 39.3(10) . . ? C12 C11 C12A 120.5(12) 4_565 . ? C12A C11 C12A 115.1(14) 4_565 . ? C12 C11 Sb1 123.5(9) . . ? C12 C11 Sb1 123.5(9) 4_565 . ? C12A C11 Sb1 115.9(8) 4_565 . ? C12A C11 Sb1 115.9(8) . . ? C12 C11 Sb1A 127.0(9) . . ? C12 C11 Sb1A 127.0(9) 4_565 . ? C12A C11 Sb1A 112.2(8) 4_565 . ? C12A C11 Sb1A 112.2(8) . . ? Sb1 C11 Sb1A 9.7(6) . . ? C11 C12 C13 123.7(17) . . ? C13A C12A C11 118.0(16) . . ? C14 C13 C12 119.9(19) . . ? C12A C13A C14 114.4(16) . . ? C13 C14 C13 106(3) . 4_565 ? C13 C14 C13A 123.4(13) . 4_565 ? C13 C14 C13A 38.9(14) 4_565 4_565 ? C13 C14 C13A 38.9(14) . . ? C13 C14 C13A 123.4(13) 4_565 . ? C13A C14 C13A 112.6(17) 4_565 . ? C13 C14 Cl1 119.4(12) . . ? C13 C14 Cl1 119.4(12) 4_565 . ? C13A C14 Cl1 117.1(9) 4_565 . ? C13A C14 Cl1 117.1(9) . . ? C22A C21 C22A 98.1(16) 4_565 . ? C22A C21 C22 121.5(11) 4_565 . ? C22A C21 C22 46.4(9) . . ? C22A C21 C22 46.4(9) 4_565 4_565 ? C22A C21 C22 121.5(11) . 4_565 ? C22 C21 C22 106.8(14) . 4_565 ? C22A C21 Sb2 121.3(8) 4_565 . ? C22A C21 Sb2 121.3(8) . . ? C22 C21 Sb2 117.1(7) . . ? C22 C21 Sb2 117.1(7) 4_565 . ? C22A C21 Sb2A 115.7(9) 4_565 . ? C22A C21 Sb2A 115.7(9) . . ? C22 C21 Sb2A 121.4(8) . . ? C22 C21 Sb2A 121.4(8) 4_565 . ? Sb2 C21 Sb2A 10.9(6) . . ? C23 C22 C21 117.2(15) . . ? C21 C22A C23A 118.9(15) . . ? C22 C23 C24 118.0(15) . . ? C24 C23A C22A 122.7(17) . . ? C23A C24 C23A 96(2) 4_565 . ? C23A C24 C23 121.2(13) 4_565 . ? C23A C24 C23 49.2(12) . . ? C23A C24 C23 49.2(12) 4_565 4_565 ? C23A C24 C23 121.2(13) . 4_565 ? C23 C24 C23 104.0(14) . 4_565 ? C23A C24 Cl2 119.6(10) 4_565 . ? C23A C24 Cl2 119.6(10) . . ? C23 C24 Cl2 119.0(9) . . ? C23 C24 Cl2 119.0(9) 4_565 . ? C32 C31 C36 119.8(6) . . ? C32 C31 Sb3 121.0(5) . . ? C36 C31 Sb3 119.2(5) . . ? C31 C32 C33 120.1(6) . . ? C34 C33 C32 119.7(6) . . ? C33 C34 C35 121.6(6) . . ? C33 C34 Cl3 119.4(6) . . ? C35 C34 Cl3 119.0(6) . . ? C34 C35 C36 119.5(7) . . ? C35 C36 C31 119.3(6) . . ? C42 C41 C46 120.0(6) . . ? C42 C41 Sb4 119.7(5) . . ? C46 C41 Sb4 120.3(5) . . ? C43 C42 C41 119.4(6) . . ? C44 C43 C42 119.6(7) . . ? C43 C44 C45 121.9(7) . . ? C43 C44 Cl4 119.3(6) . . ? C45 C44 Cl4 118.8(6) . . ? C44 C45 C46 119.4(7) . . ? C45 C46 C41 119.5(7) . . ? C52 C51 C56 120.2(7) . . ? C52 C51 Sb5 118.5(5) . . ? C56 C51 Sb5 120.9(5) . . ? C51 C52 C53 119.5(7) . . ? C54 C53 C52 118.9(8) . . ? C53 C54 C55 122.7(7) . . ? C53 C54 Cl5 119.5(7) . . ? C55 C54 Cl5 117.8(7) . . ? C56 C55 C54 117.6(8) . . ? C55 C56 C51 121.1(8) . . ? C66 C61 C62 119.1(7) . . ? C66 C61 Sb6 121.3(5) . . ? C62 C61 Sb6 119.3(5) . . ? C61 C62 C63 120.3(8) . . ? C64 C63 C62 119.3(9) . . ? C63 C64 C65 121.5(8) . . ? C63 C64 Cl6 119.4(8) . . ? C65 C64 Cl6 119.1(8) . . ? C64 C65 C66 119.0(9) . . ? C61 C66 C65 120.7(8) . . ? C76 C71 C72 119.7(7) . . ? C76 C71 Sb7 120.5(5) . . ? C72 C71 Sb7 119.8(5) . . ? C71 C72 C73 120.3(8) . . ? C72 C73 C74 119.3(8) . . ? C75 C74 C73 120.1(7) . . ? C75 C74 Cl7 120.7(6) . . ? C73 C74 Cl7 119.0(6) . . ? C74 C75 C76 120.3(7) . . ? C71 C76 C75 120.2(7) . . ? C1 N1 C3 111.1(10) . . ? C1 N1 C2 108.0(9) . . ? C3 N1 C2 106.1(8) . . ? C1 N1 C4 113.7(8) . . ? C3 N1 C4 113.9(9) . . ? C2 N1 C4 103.4(9) . . ? C5 C4 N1 111.1(9) . . ? C6 C5 C10 120.9(11) . . ? C6 C5 C4 116.8(10) . . ? C10 C5 C4 122.2(10) . . ? C5 C6 C7 119.2(11) . . ? C8 C7 C6 117.9(11) . . ? C7 C8 C9 125.1(11) . . ? C10 C9 C8 114.7(12) . . ? C5 C10 C9 122.2(12) . . ? N2 C2A C2B 175.9(16) . . ? N3 C3A C3B 171(3) . . ? N4 C4A C4B 176.9(17) . . ? N5 C5A C5B 178.7(19) . . ? N6 C6A C6B 179.5(13) . . ? C11 Sb1A Sb2A 106.0(10) . . ? C11 Sb1A Sb3A 123.0(9) . . ? Sb2A Sb1A Sb3A 119.7(9) . . ? C11 Sb1A Sb3A 123.0(9) . 4_565 ? Sb2A Sb1A Sb3A 119.7(9) . 4_565 ? Sb3A Sb1A Sb3A 60.1(8) . 4_565 ? C21 Sb2A Sb1A 82.9(9) . . ? C21 Sb2A Sb7A 142.4(6) . 4_565 ? Sb1A Sb2A Sb7A 117.0(8) . 4_565 ? C21 Sb2A Sb7A 142.4(6) . . ? Sb1A Sb2A Sb7A 117.0(8) . . ? Sb7A Sb2A Sb7A 59.3(7) 4_565 . ? Sb4A Sb3A Sb1A 120.7(9) . . ? Sb4A Sb3A Sb3A 117.5(6) . 4_565 ? Sb1A Sb3A Sb3A 59.9(4) . 4_565 ? Sb3A Sb4A Sb6A 119.7(8) . . ? Sb3A Sb4A Sb5A 123.2(9) . . ? Sb6A Sb4A Sb5A 60.8(6) . . ? Sb5A Sb5A Sb4A 119.3(5) 4_565 . ? Sb5A Sb5A Sb6A 119.6(5) 4_565 . ? Sb4A Sb5A Sb6A 59.3(6) . . ? Sb7A Sb6A Sb4A 119.4(8) . . ? Sb7A Sb6A Sb5A 121.1(7) . . ? Sb4A Sb6A Sb5A 59.9(6) . . ? Sb6A Sb7A Sb7A 119.3(4) . 4_565 ? Sb6A Sb7A Sb2A 123.5(7) . . ? Sb7A Sb7A Sb2A 60.4(4) 4_565 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.001 _refine_diff_density_min -1.609 _refine_diff_density_rms 0.188 # 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 -0.080 0.750 0.172 152 35 ' ' 2 0.080 0.250 0.828 152 35 ' ' 3 0.382 0.655 0.308 11 1 ' ' 4 0.382 0.845 0.308 11 1 ' ' 5 0.618 0.155 0.692 11 1 ' ' 6 0.618 0.345 0.692 11 1 ' ' _platon_squeeze_details ; ; # Attachment '- rbcocl_sq.cif' data_rbcocl_sq _database_code_depnum_ccdc_archive 'CCDC 866860' #TrackingRef '- rbcocl_sq.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C72 H72 Cl12 Co5 O40 Sb12, 2Cl, 19(H2 O) ; _chemical_formula_sum 'C72 H116 Cl14 Co5 O62 Sb12' _chemical_formula_weight 4225.60 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R 32' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' _cell_length_a 23.7522(3) _cell_length_b 23.7522(3) _cell_length_c 44.6195(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21800.3(8) _cell_formula_units_Z 6 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 9276 _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description prism _exptl_crystal_colour pink _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12174 _exptl_absorpt_coefficient_mu 3.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 224245 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 27.92 _reflns_number_total 11547 _reflns_number_gt 10919 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms associated with the H2O molecules were not included. Co(1) refined to give a larger than expected Ueq for reasons that are not obvious The Cl- anions are disordered over symmetry equivalent sites, and Cl6/Cl6a is further disordered over two adjacent sites with a amjor/minor contribution. Their site occupancies are tied to give exactly 2.00 Cl- per cation to neutralise charges. ; _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^)+(0.0571P)^2^+58.5323P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 11547 _refine_ls_number_parameters 498 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.009 _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 Sb1 Sb 0.343458(14) 0.748686(13) 0.932505(6) 0.02084(6) Uani 1 1 d . . . Sb2 Sb 0.350665(14) 0.827627(13) 0.989376(6) 0.02161(6) Uani 1 1 d . . . Sb3 Sb 0.422817(14) 0.818842(14) 1.047587(6) 0.02330(7) Uani 1 1 d . . . Sb4 Sb 0.268642(15) 0.755078(15) 1.047743(6) 0.02389(7) Uani 1 1 d . . . Co1 Co 0.3333 0.6667 1.00451(4) 0.0630(5) Uani 1 3 d S . . Co2 Co 0.3333 0.6667 1.09280(2) 0.0238(2) Uani 1 3 d S . . Co3 Co 0.49967(3) 0.81402(3) 0.974444(13) 0.02161(12) Uani 1 1 d . . . Cl1 Cl 0.36460(11) 1.06200(8) 0.90487(5) 0.0748(7) Uani 1 1 d . . . Cl2 Cl 0.39095(13) 0.97392(13) 0.83306(5) 0.0887(8) Uani 1 1 d . . . Cl3 Cl 0.65626(13) 1.04481(11) 1.13131(5) 0.0931(9) Uani 1 1 d . . . Cl4 Cl 0.07071(18) 0.80822(19) 1.13142(8) 0.1309(14) Uani 1 1 d . . . O1 O 0.34279(15) 0.75643(15) 1.02046(7) 0.0226(6) Uani 1 1 d . . . O2 O 0.3333 0.6667 0.95624(13) 0.0244(11) Uani 1 3 d S . . O3 O 0.28444(15) 0.75445(15) 0.96359(6) 0.0221(6) Uani 1 1 d . . . O4 O 0.40745(16) 0.80584(16) 0.96377(6) 0.0239(6) Uani 1 1 d . . . O5 O 0.47907(17) 0.79693(16) 1.02182(7) 0.0256(6) Uani 1 1 d . . . O6 O 0.28145(16) 0.82078(16) 1.01698(7) 0.0256(6) Uani 1 1 d . . . O7 O 0.34820(16) 0.81128(17) 1.07099(7) 0.0280(7) Uani 1 1 d . . . O8 O 0.42491(17) 0.87988(15) 1.01642(7) 0.0251(6) Uani 1 1 d . . . O9 O 0.26109(16) 0.67532(16) 1.06815(7) 0.0258(7) Uani 1 1 d . . . O10 O 0.26703(16) 0.67677(16) 0.91250(7) 0.0255(7) Uani 1 1 d . . . C11 C 0.3566(2) 0.9051(2) 0.96426(10) 0.0273(9) Uani 1 1 d . . . C12 C 0.4109(3) 0.9657(3) 0.96328(12) 0.0346(11) Uani 1 1 d . . . H12 H 0.4477 0.9747 0.9752 0.042 Uiso 1 1 calc R . . C13 C 0.4127(3) 1.0142(3) 0.94498(13) 0.0418(13) Uani 1 1 d . . . H13 H 0.4502 1.0563 0.9447 0.050 Uiso 1 1 calc R . . C14 C 0.3610(3) 1.0010(3) 0.92780(13) 0.0423(13) Uani 1 1 d . . . C15 C 0.3048(3) 0.9397(3) 0.92769(13) 0.0424(13) Uani 1 1 d . . . H15 H 0.2690 0.9314 0.9153 0.051 Uiso 1 1 calc R . . C16 C 0.3024(3) 0.8920(3) 0.94560(11) 0.0339(10) Uani 1 1 d . . . H16 H 0.2646 0.8501 0.9457 0.041 Uiso 1 1 calc R . . C21 C 0.3563(3) 0.8208(2) 0.90127(10) 0.0282(9) Uani 1 1 d . . . C22 C 0.3072(3) 0.8110(3) 0.88111(12) 0.0425(13) Uani 1 1 d . . . H22 H 0.2665 0.7718 0.8818 0.051 Uiso 1 1 calc R . . C23 C 0.3174(4) 0.8576(4) 0.86039(14) 0.0523(16) Uani 1 1 d . . . H23 H 0.2838 0.8514 0.8469 0.063 Uiso 1 1 calc R . . C24 C 0.3781(4) 0.9148(3) 0.85933(13) 0.0484(15) Uani 1 1 d . . . C25 C 0.4258(3) 0.9246(3) 0.87840(16) 0.0509(16) Uani 1 1 d . . . H25 H 0.4667 0.9635 0.8771 0.061 Uiso 1 1 calc R . . C26 C 0.4161(3) 0.8784(3) 0.90017(13) 0.0392(12) Uani 1 1 d . . . H26 H 0.4496 0.8861 0.9140 0.047 Uiso 1 1 calc R . . C31 C 0.4944(3) 0.8921(2) 1.07452(10) 0.0298(10) Uani 1 1 d . . . C32 C 0.4980(3) 0.8811(3) 1.10535(12) 0.0493(15) Uani 1 1 d . . . H32 H 0.4668 0.8412 1.1142 0.059 Uiso 1 1 calc R . . C33 C 0.5469(4) 0.9287(4) 1.12257(13) 0.0566(18) Uani 1 1 d . . . H33 H 0.5486 0.9217 1.1434 0.068 Uiso 1 1 calc R . . C34 C 0.5929(3) 0.9859(3) 1.10992(13) 0.0494(15) Uani 1 1 d . . . C35 C 0.5876(4) 1.0003(3) 1.08047(15) 0.0535(16) Uani 1 1 d . . . H35 H 0.6171 1.0417 1.0723 0.064 Uiso 1 1 calc R . . C36 C 0.5382(3) 0.9530(3) 1.06294(13) 0.0459(14) Uani 1 1 d . . . H36 H 0.5342 0.9625 1.0426 0.055 Uiso 1 1 calc R . . C41 C 0.2034(3) 0.7690(3) 1.07479(12) 0.0356(11) Uani 1 1 d . . . C42 C 0.2166(4) 0.7824(4) 1.10508(13) 0.0515(15) Uani 1 1 d . . . H42 H 0.2540 0.7842 1.1138 0.062 Uiso 1 1 calc R . . C43 C 0.1736(5) 0.7932(4) 1.12258(17) 0.070(2) Uani 1 1 d . . . H43 H 0.1813 0.8017 1.1434 0.084 Uiso 1 1 calc R . . C44 C 0.1204(5) 0.7913(4) 1.1093(2) 0.072(2) Uani 1 1 d . . . C45 C 0.1024(5) 0.7703(6) 1.0805(2) 0.091(3) Uani 1 1 d . . . H45 H 0.0619 0.7625 1.0727 0.110 Uiso 1 1 calc R . . C46 C 0.1465(4) 0.7604(6) 1.06256(18) 0.076(3) Uani 1 1 d . . . H46 H 0.1365 0.7479 1.0422 0.091 Uiso 1 1 calc R . . Cl5 Cl 0.4413(2) 0.7746(2) 1.1667 0.0757(13) Uani 0.65 2 d SP . . Cl6 Cl 0.6793(3) 1.0000 1.0000 0.088(2) Uani 0.51 2 d SPU A 1 Cl6A Cl 0.6556(9) 1.0000 1.0000 0.088(2) Uani 0.17 2 d SPU B 2 OW1 O 0.3389(2) 0.7413(2) 1.12078(8) 0.0424(9) Uani 1 1 d . . . OW2 O 0.52653(19) 0.83661(18) 0.92935(8) 0.0368(8) Uani 1 1 d . . . OW3 O 0.53225(19) 0.91265(19) 0.98241(8) 0.0365(8) Uani 1 1 d . . . OW4 O 0.5947(2) 0.8325(2) 0.98347(9) 0.0407(9) Uani 1 1 d . . . OW5 O 0.2563(4) 0.9308(5) 1.01379(18) 0.104(2) Uani 1 1 d . . . OW6 O 0.7032(12) 0.8528(15) 0.8584(6) 0.207(11) Uiso 0.65 1 d P . . OW6A O 0.7112(19) 0.891(3) 0.8485(11) 0.24(3) Uiso 0.35 1 d P C 6 OW7 O 0.3333 0.6667 0.8533(3) 0.166(8) Uani 1 3 d SU . . OW8 O 0.6634(5) 0.8621(5) 0.9225(2) 0.049(2) Uiso 0.50 1 d P D 3 OW8A O 0.6370(5) 0.8420(5) 0.9108(2) 0.055(2) Uiso 0.50 1 d P E 4 OW9 O 0.2724(11) 1.1112(11) 1.0364(5) 0.123(6) Uiso 0.50 1 d P . . OW9A O 0.2402(10) 1.0755(10) 1.0246(4) 0.115(6) Uiso 0.50 1 d P F 5 OW10 O 0.1855(12) 0.9886(11) 1.1127(3) 0.259(10) Uani 1 1 d U . . OW11 O 0.1870(6) 0.9687(7) 1.0547(3) 0.170(5) Uani 1 1 d U . . OW12 O 0.7347(10) 0.9444(9) 0.9550(3) 0.231(8) Uani 1 1 d U . . 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 Sb1 0.02323(14) 0.02248(14) 0.01686(12) 0.00106(9) -0.00054(10) 0.01146(11) Sb2 0.02412(14) 0.02093(13) 0.02073(12) -0.00097(10) -0.00117(10) 0.01198(12) Sb3 0.02694(15) 0.02371(14) 0.01875(12) -0.00272(10) -0.00219(10) 0.01228(12) Sb4 0.02729(15) 0.02601(15) 0.01967(12) -0.00350(10) 0.00084(10) 0.01431(12) Co1 0.0642(7) 0.0642(7) 0.0604(10) 0.000 0.000 0.0321(4) Co2 0.0289(3) 0.0289(3) 0.0137(4) 0.000 0.000 0.01443(16) Co3 0.0224(3) 0.0204(3) 0.0209(3) 0.0005(2) -0.0003(2) 0.0098(2) Cl1 0.0833(13) 0.0372(8) 0.0843(12) 0.0184(8) -0.0422(11) 0.0155(8) Cl2 0.0969(16) 0.0928(16) 0.0890(15) 0.0668(13) 0.0255(12) 0.0567(14) Cl3 0.1010(17) 0.0661(12) 0.0588(11) -0.0130(9) -0.0517(12) 0.0017(11) Cl4 0.132(3) 0.150(3) 0.138(3) -0.008(2) 0.079(2) 0.092(2) O1 0.0250(15) 0.0277(15) 0.0142(12) 0.0006(11) 0.0001(11) 0.0125(13) O2 0.0196(16) 0.0196(16) 0.034(3) 0.000 0.000 0.0098(8) O3 0.0221(15) 0.0215(15) 0.0221(14) -0.0005(11) 0.0008(11) 0.0103(13) O4 0.0232(15) 0.0265(16) 0.0208(13) -0.0019(11) -0.0012(11) 0.0116(13) O5 0.0286(16) 0.0291(16) 0.0190(13) 0.0032(12) 0.0007(12) 0.0143(14) O6 0.0276(16) 0.0282(16) 0.0249(14) -0.0014(12) 0.0020(12) 0.0168(14) O7 0.0309(18) 0.0333(17) 0.0218(14) -0.0061(13) -0.0036(12) 0.0176(15) O8 0.0309(17) 0.0208(15) 0.0235(14) -0.0016(12) -0.0045(12) 0.0127(13) O9 0.0283(16) 0.0259(16) 0.0203(15) 0.0019(11) 0.0013(11) 0.0114(13) O10 0.0245(15) 0.0267(16) 0.0231(15) 0.0007(12) -0.0024(11) 0.0111(13) C11 0.030(2) 0.026(2) 0.026(2) 0.0009(16) -0.0032(17) 0.0147(19) C12 0.035(3) 0.029(2) 0.036(2) -0.0013(19) -0.009(2) 0.014(2) C13 0.041(3) 0.026(2) 0.045(3) 0.007(2) -0.008(2) 0.008(2) C14 0.058(4) 0.027(3) 0.038(3) 0.004(2) -0.014(2) 0.018(3) C15 0.045(3) 0.041(3) 0.044(3) -0.006(2) -0.019(2) 0.024(3) C16 0.030(2) 0.028(2) 0.040(3) 0.0023(19) -0.002(2) 0.011(2) C21 0.038(3) 0.028(2) 0.022(2) 0.0050(16) 0.0024(17) 0.020(2) C22 0.046(3) 0.044(3) 0.035(3) 0.006(2) -0.006(2) 0.021(3) C23 0.061(4) 0.067(4) 0.041(3) 0.019(3) 0.000(3) 0.041(4) C24 0.066(4) 0.049(3) 0.040(3) 0.024(3) 0.012(3) 0.036(3) C25 0.043(3) 0.041(3) 0.066(4) 0.026(3) 0.014(3) 0.019(3) C26 0.035(3) 0.035(3) 0.047(3) 0.012(2) 0.002(2) 0.017(2) C31 0.033(2) 0.030(2) 0.025(2) -0.0060(17) -0.0075(18) 0.015(2) C32 0.046(3) 0.054(4) 0.028(3) 0.003(2) -0.003(2) 0.010(3) C33 0.074(5) 0.057(4) 0.026(3) -0.005(2) -0.019(3) 0.023(4) C34 0.055(4) 0.043(3) 0.033(3) -0.011(2) -0.018(3) 0.012(3) C35 0.057(4) 0.040(3) 0.049(3) 0.000(3) -0.013(3) 0.013(3) C36 0.039(3) 0.048(3) 0.033(3) 0.003(2) -0.007(2) 0.009(3) C41 0.031(3) 0.035(3) 0.037(3) -0.002(2) 0.014(2) 0.014(2) C42 0.063(4) 0.061(4) 0.035(3) -0.003(3) 0.012(3) 0.035(3) C43 0.092(6) 0.067(5) 0.047(4) -0.002(3) 0.034(4) 0.037(5) C44 0.077(6) 0.075(5) 0.077(5) 0.002(4) 0.045(5) 0.047(5) C45 0.077(6) 0.135(10) 0.095(7) -0.017(6) 0.015(5) 0.077(7) C46 0.072(5) 0.126(8) 0.053(4) -0.021(5) 0.000(4) 0.067(6) Cl5 0.0758(18) 0.0758(18) 0.0415(18) 0.0058(11) -0.0058(11) 0.012(2) Cl6 0.066(3) 0.134(6) 0.085(3) 0.012(3) 0.0059(17) 0.067(3) Cl6A 0.066(3) 0.134(6) 0.085(3) 0.012(3) 0.0059(17) 0.067(3) OW1 0.046(2) 0.048(2) 0.0279(17) 0.0004(15) -0.0019(15) 0.0197(19) OW2 0.040(2) 0.0324(19) 0.0359(18) 0.0009(14) 0.0046(15) 0.0166(17) OW3 0.041(2) 0.0345(19) 0.0314(17) 0.0011(14) 0.0006(15) 0.0171(17) OW4 0.043(2) 0.044(2) 0.040(2) -0.0001(16) -0.0014(16) 0.0251(19) OW5 0.113(6) 0.129(7) 0.096(5) -0.022(5) -0.007(4) 0.081(6) OW7 0.223(13) 0.223(13) 0.051(6) 0.000 0.000 0.112(7) OW10 0.44(3) 0.33(2) 0.153(11) -0.052(14) -0.029(15) 0.30(2) OW11 0.147(10) 0.214(14) 0.188(11) -0.037(10) -0.010(8) 0.120(10) OW12 0.33(2) 0.240(17) 0.194(12) 0.117(12) 0.120(14) 0.192(17) _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 Sb1 O10 1.977(3) . ? Sb1 O10 2.001(3) 3_565 ? Sb1 O4 2.009(3) . ? Sb1 O3 2.025(3) . ? Sb1 C21 2.109(4) . ? Sb1 O2 2.123(3) . ? Sb1 Sb2 3.1086(4) . ? Sb1 Sb1 3.1865(5) 2_665 ? Sb1 Sb1 3.1865(5) 3_565 ? Sb2 O8 1.979(3) . ? Sb2 O6 1.995(3) . ? Sb2 O3 2.021(3) . ? Sb2 O4 2.022(3) . ? Sb2 C11 2.098(5) . ? Sb2 O1 2.122(3) . ? Sb2 Sb3 3.1756(4) . ? Sb2 Sb4 3.1922(4) . ? Sb3 O7 1.986(3) . ? Sb3 O8 1.992(3) . ? Sb3 O5 2.018(3) . ? Sb3 O9 2.025(3) 3_565 ? Sb3 C31 2.098(5) . ? Sb3 O1 2.111(3) . ? Sb3 Sb4 3.1211(4) 3_565 ? Sb3 Sb4 3.1871(4) . ? Sb4 O7 1.976(3) . ? Sb4 O6 1.984(3) . ? Sb4 O5 2.017(3) 2_665 ? Sb4 O9 2.027(3) . ? Sb4 C41 2.116(5) . ? Sb4 O1 2.128(3) . ? Sb4 Sb3 3.1211(4) 2_665 ? Co1 O1 2.150(3) . ? Co1 O1 2.150(3) 2_665 ? Co1 O1 2.150(3) 3_565 ? Co1 O2 2.154(6) . ? Co2 OW1 2.118(4) . ? Co2 OW1 2.118(4) 2_665 ? Co2 OW1 2.118(4) 3_565 ? Co2 O9 2.133(3) . ? Co2 O9 2.133(3) 3_565 ? Co2 O9 2.133(3) 2_665 ? Co3 OW3 2.098(4) . ? Co3 OW2 2.098(4) . ? Co3 OW4 2.110(4) . ? Co3 O3 2.134(3) 3_565 ? Co3 O4 2.153(3) . ? Co3 O5 2.162(3) . ? Cl1 C14 1.740(5) . ? Cl2 C24 1.735(5) . ? Cl3 C34 1.740(6) . ? Cl4 C44 1.734(7) . ? O2 Sb1 2.123(3) 2_665 ? O2 Sb1 2.123(3) 3_565 ? O3 Co3 2.134(3) 2_665 ? O5 Sb4 2.017(3) 3_565 ? O9 Sb3 2.025(3) 2_665 ? O10 Sb1 2.001(3) 2_665 ? C11 C12 1.371(7) . ? C11 C16 1.432(7) . ? C12 C13 1.397(7) . ? C13 C14 1.344(8) . ? C14 C15 1.400(9) . ? C15 C16 1.362(8) . ? C21 C26 1.397(8) . ? C21 C22 1.397(7) . ? C22 C23 1.368(8) . ? C23 C24 1.404(10) . ? C24 C25 1.340(10) . ? C25 C26 1.396(8) . ? C31 C36 1.392(8) . ? C31 C32 1.410(7) . ? C32 C33 1.380(9) . ? C33 C34 1.368(10) . ? C34 C35 1.380(9) . ? C35 C36 1.390(9) . ? C41 C46 1.376(10) . ? C41 C42 1.388(8) . ? C42 C43 1.407(10) . ? C43 C44 1.378(14) . ? C44 C45 1.364(14) . ? C45 C46 1.428(11) . ? OW6 OW6A 0.94(7) . ? OW9 OW9A 0.97(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Sb1 O10 96.06(19) . 3_565 ? O10 Sb1 O4 162.73(13) . . ? O10 Sb1 O4 92.06(13) 3_565 . ? O10 Sb1 O3 90.01(13) . . ? O10 Sb1 O3 162.61(13) 3_565 . ? O4 Sb1 O3 78.11(13) . . ? O10 Sb1 C21 95.78(17) . . ? O10 Sb1 C21 92.82(16) 3_565 . ? O4 Sb1 C21 99.02(17) . . ? O3 Sb1 C21 102.79(15) . . ? O10 Sb1 O2 78.38(13) . . ? O10 Sb1 O2 77.88(13) 3_565 . ? O4 Sb1 O2 88.50(14) . . ? O3 Sb1 O2 87.46(13) . . ? C21 Sb1 O2 168.30(18) . . ? O10 Sb1 Sb2 129.76(10) . . ? O10 Sb1 Sb2 131.73(10) 3_565 . ? O4 Sb1 Sb2 39.70(9) . . ? O3 Sb1 Sb2 39.75(9) . . ? C21 Sb1 Sb2 96.17(13) . . ? O2 Sb1 Sb2 95.34(13) . . ? O10 Sb1 Sb1 37.02(9) . 2_665 ? O10 Sb1 Sb1 86.51(9) 3_565 2_665 ? O4 Sb1 Sb1 128.96(9) . 2_665 ? O3 Sb1 Sb1 88.62(9) . 2_665 ? C21 Sb1 Sb1 132.01(14) . 2_665 ? O2 Sb1 Sb1 41.36(9) . 2_665 ? Sb2 Sb1 Sb1 119.413(9) . 2_665 ? O10 Sb1 Sb1 86.89(10) . 3_565 ? O10 Sb1 Sb1 36.52(9) 3_565 3_565 ? O4 Sb1 Sb1 90.66(9) . 3_565 ? O3 Sb1 Sb1 128.21(9) . 3_565 ? C21 Sb1 Sb1 128.96(13) . 3_565 ? O2 Sb1 Sb1 41.36(9) . 3_565 ? Sb2 Sb1 Sb1 120.590(9) . 3_565 ? Sb1 Sb1 Sb1 60.0 2_665 3_565 ? O8 Sb2 O6 96.56(14) . . ? O8 Sb2 O3 162.28(13) . . ? O6 Sb2 O3 91.49(13) . . ? O8 Sb2 O4 90.32(13) . . ? O6 Sb2 O4 162.92(13) . . ? O3 Sb2 O4 77.90(13) . . ? O8 Sb2 C11 97.33(16) . . ? O6 Sb2 C11 95.32(16) . . ? O3 Sb2 C11 97.60(16) . . ? O4 Sb2 C11 99.29(16) . . ? O8 Sb2 O1 78.29(12) . . ? O6 Sb2 O1 77.92(13) . . ? O3 Sb2 O1 88.06(12) . . ? O4 Sb2 O1 88.26(12) . . ? C11 Sb2 O1 171.35(15) . . ? O8 Sb2 Sb1 129.71(10) . . ? O6 Sb2 Sb1 131.32(10) . . ? O3 Sb2 Sb1 39.84(9) . . ? O4 Sb2 Sb1 39.39(9) . . ? C11 Sb2 Sb1 92.99(13) . . ? O1 Sb2 Sb1 95.54(8) . . ? O8 Sb2 Sb3 37.03(9) . . ? O6 Sb2 Sb3 86.53(9) . . ? O3 Sb2 Sb3 128.51(9) . . ? O4 Sb2 Sb3 89.67(9) . . ? C11 Sb2 Sb3 133.84(13) . . ? O1 Sb2 Sb3 41.27(8) . . ? Sb1 Sb2 Sb3 119.788(11) . . ? O8 Sb2 Sb4 87.31(9) . . ? O6 Sb2 Sb4 36.54(9) . . ? O3 Sb2 Sb4 89.87(8) . . ? O4 Sb2 Sb4 128.89(9) . . ? C11 Sb2 Sb4 131.65(14) . . ? O1 Sb2 Sb4 41.38(8) . . ? Sb1 Sb2 Sb4 120.377(11) . . ? Sb3 Sb2 Sb4 60.066(9) . . ? O7 Sb3 O8 97.43(14) . . ? O7 Sb3 O5 162.17(14) . . ? O8 Sb3 O5 90.63(13) . . ? O7 Sb3 O9 90.58(14) . 3_565 ? O8 Sb3 O9 162.37(12) . 3_565 ? O5 Sb3 O9 77.62(13) . 3_565 ? O7 Sb3 C31 95.20(17) . . ? O8 Sb3 C31 94.69(17) . . ? O5 Sb3 C31 99.98(17) . . ? O9 Sb3 C31 100.23(17) 3_565 . ? O7 Sb3 O1 77.78(13) . . ? O8 Sb3 O1 78.28(13) . . ? O5 Sb3 O1 88.40(13) . . ? O9 Sb3 O1 88.17(13) 3_565 . ? C31 Sb3 O1 169.19(17) . . ? O7 Sb3 Sb4 130.22(10) . 3_565 ? O8 Sb3 Sb4 129.94(9) . 3_565 ? O5 Sb3 Sb4 39.31(9) . 3_565 ? O9 Sb3 Sb4 39.65(9) 3_565 3_565 ? C31 Sb3 Sb4 95.11(14) . 3_565 ? O1 Sb3 Sb4 95.71(9) . 3_565 ? O7 Sb3 Sb2 87.10(9) . . ? O8 Sb3 Sb2 36.76(9) . . ? O5 Sb3 Sb2 89.97(9) . . ? O9 Sb3 Sb2 128.86(9) 3_565 . ? C31 Sb3 Sb2 130.87(14) . . ? O1 Sb3 Sb2 41.52(8) . . ? Sb4 Sb3 Sb2 120.160(11) 3_565 . ? O7 Sb3 Sb4 36.35(9) . . ? O8 Sb3 Sb4 87.25(10) . . ? O5 Sb3 Sb4 129.06(10) . . ? O9 Sb3 Sb4 90.02(10) 3_565 . ? C31 Sb3 Sb4 130.92(15) . . ? O1 Sb3 Sb4 41.45(8) . . ? Sb4 Sb3 Sb4 120.488(14) 3_565 . ? Sb2 Sb3 Sb4 60.226(9) . . ? O7 Sb4 O6 96.49(15) . . ? O7 Sb4 O5 161.47(14) . 2_665 ? O6 Sb4 O5 91.59(14) . 2_665 ? O7 Sb4 O9 90.20(14) . . ? O6 Sb4 O9 162.31(13) . . ? O5 Sb4 O9 77.60(14) 2_665 . ? O7 Sb4 C41 97.04(18) . . ? O6 Sb4 C41 96.21(18) . . ? O5 Sb4 C41 98.63(18) 2_665 . ? O9 Sb4 C41 99.20(18) . . ? O7 Sb4 O1 77.60(13) . . ? O6 Sb4 O1 78.01(13) . . ? O5 Sb4 O1 87.86(13) 2_665 . ? O9 Sb4 O1 87.53(13) . . ? C41 Sb4 O1 171.48(17) . . ? O7 Sb4 Sb3 129.78(10) . 2_665 ? O6 Sb4 Sb3 130.92(10) . 2_665 ? O5 Sb4 Sb3 39.35(9) 2_665 2_665 ? O9 Sb4 Sb3 39.60(9) . 2_665 ? C41 Sb4 Sb3 93.57(15) . 2_665 ? O1 Sb4 Sb3 94.95(9) . 2_665 ? O7 Sb4 Sb3 36.56(10) . . ? O6 Sb4 Sb3 86.38(10) . . ? O5 Sb4 Sb3 128.12(10) 2_665 . ? O9 Sb4 Sb3 89.36(9) . . ? C41 Sb4 Sb3 133.15(16) . . ? O1 Sb4 Sb3 41.06(8) . . ? Sb3 Sb4 Sb3 119.511(14) 2_665 . ? O7 Sb4 Sb2 86.80(10) . . ? O6 Sb4 Sb2 36.77(9) . . ? O5 Sb4 Sb2 89.80(9) 2_665 . ? O9 Sb4 Sb2 128.01(9) . . ? C41 Sb4 Sb2 132.69(16) . . ? O1 Sb4 Sb2 41.24(8) . . ? Sb3 Sb4 Sb2 119.646(11) 2_665 . ? Sb3 Sb4 Sb2 59.708(9) . . ? O1 Co1 O1 109.62(9) . 2_665 ? O1 Co1 O1 109.62(9) . 3_565 ? O1 Co1 O1 109.62(9) 2_665 3_565 ? O1 Co1 O2 109.33(9) . . ? O1 Co1 O2 109.33(9) 2_665 . ? O1 Co1 O2 109.33(9) 3_565 . ? OW1 Co2 OW1 88.78(16) . 2_665 ? OW1 Co2 OW1 88.78(16) . 3_565 ? OW1 Co2 OW1 88.78(16) 2_665 3_565 ? OW1 Co2 O9 86.56(14) . . ? OW1 Co2 O9 88.64(14) 2_665 . ? OW1 Co2 O9 174.73(14) 3_565 . ? OW1 Co2 O9 88.64(14) . 3_565 ? OW1 Co2 O9 174.72(14) 2_665 3_565 ? OW1 Co2 O9 86.56(14) 3_565 3_565 ? O9 Co2 O9 95.80(12) . 3_565 ? OW1 Co2 O9 174.72(14) . 2_665 ? OW1 Co2 O9 86.56(14) 2_665 2_665 ? OW1 Co2 O9 88.64(14) 3_565 2_665 ? O9 Co2 O9 95.80(12) . 2_665 ? O9 Co2 O9 95.80(12) 3_565 2_665 ? OW3 Co3 OW2 88.95(15) . . ? OW3 Co3 OW4 88.63(16) . . ? OW2 Co3 OW4 88.45(16) . . ? OW3 Co3 O3 176.18(14) . 3_565 ? OW2 Co3 O3 87.38(13) . 3_565 ? OW4 Co3 O3 90.25(14) . 3_565 ? OW3 Co3 O4 85.92(14) . . ? OW2 Co3 O4 88.66(14) . . ? OW4 Co3 O4 173.87(15) . . ? O3 Co3 O4 95.02(13) 3_565 . ? OW3 Co3 O5 88.08(14) . . ? OW2 Co3 O5 175.66(15) . . ? OW4 Co3 O5 88.32(14) . . ? O3 Co3 O5 95.53(12) 3_565 . ? O4 Co3 O5 94.28(12) . . ? Sb3 O1 Sb2 97.21(13) . . ? Sb3 O1 Sb4 97.50(12) . . ? Sb2 O1 Sb4 97.38(13) . . ? Sb3 O1 Co1 119.79(15) . . ? Sb2 O1 Co1 119.85(14) . . ? Sb4 O1 Co1 119.94(15) . . ? Sb1 O2 Sb1 97.27(17) . 2_665 ? Sb1 O2 Sb1 97.27(17) . 3_565 ? Sb1 O2 Sb1 97.27(17) 2_665 3_565 ? Sb1 O2 Co1 119.93(13) . . ? Sb1 O2 Co1 119.93(13) 2_665 . ? Sb1 O2 Co1 119.93(13) 3_565 . ? Sb2 O3 Sb1 100.41(13) . . ? Sb2 O3 Co3 127.82(15) . 2_665 ? Sb1 O3 Co3 129.38(15) . 2_665 ? Sb1 O4 Sb2 100.90(14) . . ? Sb1 O4 Co3 127.32(16) . . ? Sb2 O4 Co3 129.09(14) . . ? Sb4 O5 Sb3 101.34(13) 3_565 . ? Sb4 O5 Co3 127.37(17) 3_565 . ? Sb3 O5 Co3 128.72(16) . . ? Sb4 O6 Sb2 106.69(15) . . ? Sb4 O7 Sb3 107.09(14) . . ? Sb2 O8 Sb3 106.21(15) . . ? Sb3 O9 Sb4 100.75(14) 2_665 . ? Sb3 O9 Co2 128.01(16) 2_665 . ? Sb4 O9 Co2 128.47(16) . . ? Sb1 O10 Sb1 106.46(15) . 2_665 ? C12 C11 C16 118.8(5) . . ? C12 C11 Sb2 123.5(4) . . ? C16 C11 Sb2 117.5(4) . . ? C11 C12 C13 120.6(5) . . ? C14 C13 C12 119.6(5) . . ? C13 C14 C15 121.9(5) . . ? C13 C14 Cl1 118.8(5) . . ? C15 C14 Cl1 119.2(4) . . ? C16 C15 C14 119.0(5) . . ? C15 C16 C11 120.1(5) . . ? C26 C21 C22 119.7(5) . . ? C26 C21 Sb1 118.8(4) . . ? C22 C21 Sb1 121.4(4) . . ? C23 C22 C21 120.4(6) . . ? C22 C23 C24 119.1(6) . . ? C25 C24 C23 121.1(5) . . ? C25 C24 Cl2 119.8(5) . . ? C23 C24 Cl2 119.0(5) . . ? C24 C25 C26 120.8(6) . . ? C25 C26 C21 118.8(6) . . ? C36 C31 C32 118.1(5) . . ? C36 C31 Sb3 121.6(4) . . ? C32 C31 Sb3 120.3(4) . . ? C33 C32 C31 119.7(6) . . ? C34 C33 C32 120.7(5) . . ? C33 C34 C35 120.8(6) . . ? C33 C34 Cl3 120.8(4) . . ? C35 C34 Cl3 118.2(5) . . ? C34 C35 C36 118.8(6) . . ? C35 C36 C31 121.4(5) . . ? C46 C41 C42 120.8(6) . . ? C46 C41 Sb4 119.5(4) . . ? C42 C41 Sb4 119.5(5) . . ? C41 C42 C43 118.8(7) . . ? C44 C43 C42 119.5(7) . . ? C45 C44 C43 122.1(7) . . ? C45 C44 Cl4 119.7(8) . . ? C43 C44 Cl4 117.8(7) . . ? C44 C45 C46 117.8(9) . . ? C41 C46 C45 120.0(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.301 _refine_diff_density_min -2.669 _refine_diff_density_rms 0.129 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.000 0.000 0.000 1180.7 317.9 2 0.000 0.193 0.500 59.1 2.7 3 0.333 0.667 0.667 1182.0 318.0 4 0.141 0.474 0.167 59.8 2.6 5 0.193 1.000 0.500 59.2 2.6 6 0.333 0.859 0.167 59.8 2.6 7 0.667 0.333 0.333 1182.0 318.3 8 0.474 0.141 0.833 59.8 2.6 9 0.526 0.667 0.167 60.0 2.6 10 0.667 0.526 0.833 60.0 2.7 11 0.807 0.807 0.500 59.2 2.6 12 0.859 0.333 0.833 59.9 2.6 _platon_squeeze_details ; ;