# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2208 data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C53 H43 O20 Os6 Sb2' _chemical_formula_weight 2384.57 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 14.8356(4) _cell_length_b 11.8116(3) _cell_length_c 19.4734(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.5870(10) _cell_angle_gamma 90.00 _cell_volume 3342.82(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5792 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'BLOCK' _exptl_crystal_colour 'ORANGE' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured ' _exptl_crystal_density_diffrn 2.369 _exptl_crystal_density_method ? _exptl_crystal_F_000 2158 _exptl_absorpt_coefficient_mu 12.213 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.155817 _exptl_absorpt_correction_T_max 0.262266 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19021 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.84 _reflns_number_total 7128 _reflns_number_observed 5717 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+7.0127P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7128 _refine_ls_number_parameters 358 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_obs 0.0323 _refine_ls_wR_factor_all 0.0808 _refine_ls_wR_factor_obs 0.0704 _refine_ls_goodness_of_fit_all 1.189 _refine_ls_goodness_of_fit_obs 1.164 _refine_ls_restrained_S_all 1.188 _refine_ls_restrained_S_obs 1.164 _refine_ls_shift/esd_max 0.367 _refine_ls_shift/esd_mean 0.012 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Os1 Os 0.53883(2) 0.79495(2) 0.392545(15) 0.03691(8) Uani 1 d D . Os2 Os 0.69303(2) 0.76918(2) 0.309589(15) 0.03838(8) Uani 1 d D . Os3 Os 0.72710(2) 0.85920(3) 0.45033(2) 0.04834(10) Uani 1 d . . Sb4 Sb 0.37772(3) 0.71059(4) 0.32339(2) 0.03575(12) Uani 1 d . . O11 O 0.5757(5) 0.5665(6) 0.4701(4) 0.085(2) Uani 1 d . . O12 O 0.4637(5) 0.8765(6) 0.5178(4) 0.081(2) Uani 1 d . . O13 O 0.4991(4) 1.0314(5) 0.3267(3) 0.063(2) Uani 1 d . . O21 O 0.7099(5) 0.5158(6) 0.3506(4) 0.075(2) Uani 1 d . . O22 O 0.8970(5) 0.7763(7) 0.3080(4) 0.091(2) Uani 1 d . . O23 O 0.6856(5) 1.0132(5) 0.2519(3) 0.067(2) Uani 1 d . . O31 O 0.7736(6) 0.6145(7) 0.5016(4) 0.092(2) Uani 1 d . . O32 O 0.6926(6) 0.9380(7) 0.5919(4) 0.098(3) Uani 1 d . . O33 O 0.6865(5) 1.1032(6) 0.3939(4) 0.076(2) Uani 1 d . . O34 O 0.9334(5) 0.9053(9) 0.4703(5) 0.115(3) Uani 1 d . . C11 C 0.5627(6) 0.6503(8) 0.4398(5) 0.053(2) Uani 1 d . . C12 C 0.4916(6) 0.8439(7) 0.4702(4) 0.050(2) Uani 1 d . . C13 C 0.5134(5) 0.9439(7) 0.3500(4) 0.046(2) Uani 1 d . . C21 C 0.7038(6) 0.6107(7) 0.3373(4) 0.051(2) Uani 1 d . . C22 C 0.8202(7) 0.7723(8) 0.3071(5) 0.059(2) Uani 1 d . . C23 C 0.6854(5) 0.9252(7) 0.2758(4) 0.046(2) Uani 1 d . . C31 C 0.7549(7) 0.7040(10) 0.4810(5) 0.069(3) Uani 1 d . . C32 C 0.7048(7) 0.9066(8) 0.5394(5) 0.067(3) Uani 1 d . . C33 C 0.6993(6) 1.0125(8) 0.4142(5) 0.057(2) Uani 1 d . . C34 C 0.8565(7) 0.8887(9) 0.4631(5) 0.071(3) Uani 1 d . . C41 C 0.3808(6) 0.5284(6) 0.3281(4) 0.045(2) Uani 1 d . . C42 C 0.3013(7) 0.4695(7) 0.3317(5) 0.067(3) Uani 1 d . . H42A H 0.2479(7) 0.5096(7) 0.3337(5) 0.080 Uiso 1 calc R . C43 C 0.2993(10) 0.3511(9) 0.3324(7) 0.094(4) Uani 1 d . . H43A H 0.2454(10) 0.3122(9) 0.3345(7) 0.113 Uiso 1 calc R . C44 C 0.3797(11) 0.2934(9) 0.3298(7) 0.095(4) Uani 1 d . . H44A H 0.3796(11) 0.2146(9) 0.3290(7) 0.114 Uiso 1 calc R . C45 C 0.4589(9) 0.3507(9) 0.3284(7) 0.091(4) Uani 1 d . . H45A H 0.5131(9) 0.3111(9) 0.3288(7) 0.110 Uiso 1 calc R . C46 C 0.4589(7) 0.4677(7) 0.3265(5) 0.066(3) Uani 1 d . . H46A H 0.5130(7) 0.5058(7) 0.3241(5) 0.080 Uiso 1 calc R . C51 C 0.2788(5) 0.7371(6) 0.3886(4) 0.044(2) Uani 1 d . . C52 C 0.2058(6) 0.8113(8) 0.3710(5) 0.059(2) Uani 1 d . . H52A H 0.1975(6) 0.8513(8) 0.3291(5) 0.071 Uiso 1 calc R . C53 C 0.1443(7) 0.8264(9) 0.4159(6) 0.076(3) Uani 1 d . . H53A H 0.0956(7) 0.8771(9) 0.4043(6) 0.091 Uiso 1 calc R . C54 C 0.1562(8) 0.7662(10) 0.4775(6) 0.078(3) Uani 1 d . . H54A H 0.1141(8) 0.7750(10) 0.5067(6) 0.093 Uiso 1 calc R . C55 C 0.2279(8) 0.6941(9) 0.4966(5) 0.072(3) Uani 1 d . . H55A H 0.2357(8) 0.6549(9) 0.5388(5) 0.086 Uiso 1 calc R . C56 C 0.2901(7) 0.6792(8) 0.4522(5) 0.060(2) Uani 1 d . . H56A H 0.3396(7) 0.6301(8) 0.4651(5) 0.072 Uiso 1 calc R . C1 C 0.9874(25) 0.4945(31) 0.4080(19) 0.159(13) Uiso 0.50 d P . H1A H 0.9689(202) 0.5685(66) 0.4200(68) 0.239 Uiso 0.50 calc PR . H1B H 1.0404(67) 0.4709(250) 0.4417(31) 0.239 Uiso 0.50 calc PR . H1C H 0.9380(145) 0.4419(197) 0.4079(48) 0.239 Uiso 0.50 calc PR . C2 C 1.0066(25) 0.4972(32) 0.3492(19) 0.153(13) Uiso 0.50 d P . H2A H 1.0455(25) 0.4315(32) 0.3552(19) 0.230 Uiso 0.50 calc PR . H2B H 1.0493(25) 0.5589(32) 0.3585(19) 0.230 Uiso 0.50 calc PR . C3 C 0.9946(25) 0.5016(28) 0.2807(15) 0.139(12) Uiso 0.50 d P . H3A H 0.9462(25) 0.4462(28) 0.2727(15) 0.209 Uiso 0.50 calc PR . H3B H 0.9618(25) 0.5721(28) 0.2766(15) 0.209 Uiso 0.50 calc PR . C4 C -0.0553(26) 1.2171(26) 0.3523(18) 0.150 Uiso 0.50 d PD 1 H4A H -0.0206(159) 1.2260(74) 0.3992(59) 0.225 Uiso 0.50 calc PR 1 H4B H -0.1191(34) 1.2320(84) 0.3516(143) 0.225 Uiso 0.50 calc PR 1 H4C H -0.0330(185) 1.2693(28) 0.3218(90) 0.225 Uiso 0.50 calc PR 1 C5 C -0.0462(27) 1.1169(28) 0.3317(18) 0.150 Uiso 0.50 d PD 1 H5A H -0.0101(27) 1.0808(28) 0.3723(18) 0.225 Uiso 0.50 calc PR 1 H5B H -0.1068(27) 1.0856(28) 0.3272(18) 0.225 Uiso 0.50 calc PR 1 C6 C -0.0178(27) 1.0741(26) 0.2831(18) 0.150 Uiso 0.50 d PD 1 H6A H -0.0674(27) 1.0217(26) 0.2686(18) 0.225 Uiso 0.50 calc PR 1 H6B H 0.0298(27) 1.0285(26) 0.3104(18) 0.225 Uiso 0.50 calc PR 1 C7 C -0.1144(25) 1.1597(31) 0.2812(16) 0.150 Uiso 0.50 d PD 2 H7A H -0.0893(161) 1.1164(155) 0.3224(33) 0.225 Uiso 0.50 calc PR 2 H7B H -0.1804(27) 1.1563(227) 0.2727(65) 0.225 Uiso 0.50 calc PR 2 H7C H -0.0948(173) 1.2370(82) 0.2882(95) 0.225 Uiso 0.50 calc PR 2 C8 C -0.0869(26) 1.1200(28) 0.2300(16) 0.150 Uiso 0.50 d PD 2 H8A H -0.0433(26) 1.0641(28) 0.2516(16) 0.225 Uiso 0.50 calc PR 2 H8B H -0.1394(26) 1.0773(28) 0.2069(16) 0.225 Uiso 0.50 calc PR 2 C9 C -0.0542(13) 1.1509(28) 0.1817(11) 0.150 Uiso 0.50 d PD 2 H9A H -0.0997(13) 1.1957(28) 0.1516(11) 0.225 Uiso 0.50 d PR 2 H9B H 0.0026(13) 1.1923(28) 0.1926(11) 0.225 Uiso 0.50 d PR 2 H12 H 0.5745(13) 0.7662(28) 0.3121(11) 0.080 Uiso 1 d RD . 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 Os1 0.0377(2) 0.0364(2) 0.0371(2) -0.00055(11) 0.00843(12) -0.00117(12) Os2 0.0365(2) 0.0389(2) 0.0396(2) -0.00157(12) 0.00736(12) 0.00121(12) Os3 0.0441(2) 0.0564(2) 0.0426(2) -0.00724(14) 0.00392(14) -0.00861(15) Sb4 0.0364(3) 0.0318(2) 0.0399(3) 0.0020(2) 0.0096(2) -0.0016(2) O11 0.087(5) 0.070(5) 0.094(5) 0.040(4) 0.011(4) 0.009(4) O12 0.100(6) 0.089(5) 0.064(4) -0.020(4) 0.038(4) -0.008(4) O13 0.077(4) 0.039(3) 0.074(4) 0.006(3) 0.016(3) 0.005(3) O21 0.087(5) 0.053(4) 0.085(5) 0.015(3) 0.015(4) 0.018(4) O22 0.045(4) 0.115(6) 0.116(6) 0.010(5) 0.024(4) 0.003(4) O23 0.087(5) 0.048(4) 0.068(4) 0.009(3) 0.016(4) -0.004(3) O31 0.101(6) 0.080(5) 0.087(5) 0.015(4) -0.007(4) 0.017(5) O32 0.143(8) 0.096(6) 0.061(4) -0.019(4) 0.036(5) -0.035(5) O33 0.095(5) 0.058(4) 0.073(4) -0.006(4) 0.012(4) -0.006(4) O34 0.052(5) 0.147(8) 0.137(7) -0.017(6) -0.002(5) -0.027(5) C11 0.044(5) 0.057(5) 0.058(5) 0.008(4) 0.013(4) 0.000(4) C12 0.054(5) 0.051(5) 0.049(5) -0.009(4) 0.017(4) -0.007(4) C13 0.046(5) 0.047(5) 0.045(4) -0.011(4) 0.011(4) -0.006(4) C21 0.053(5) 0.050(5) 0.049(5) -0.003(4) 0.007(4) 0.008(4) C22 0.055(6) 0.056(5) 0.067(6) 0.002(4) 0.013(5) 0.002(5) C23 0.043(4) 0.046(5) 0.049(4) -0.007(4) 0.009(4) -0.006(4) C31 0.071(7) 0.075(7) 0.054(6) -0.010(5) -0.003(5) -0.008(6) C32 0.088(7) 0.065(6) 0.049(5) -0.011(5) 0.017(5) -0.019(5) C33 0.057(5) 0.060(6) 0.053(5) -0.014(4) 0.010(4) -0.014(5) C34 0.049(6) 0.090(7) 0.071(6) -0.015(5) 0.002(5) -0.008(5) C41 0.063(5) 0.032(4) 0.042(4) 0.000(3) 0.015(4) -0.007(4) C42 0.073(7) 0.044(5) 0.087(7) 0.004(5) 0.022(6) -0.006(5) C43 0.113(10) 0.046(6) 0.132(11) 0.000(6) 0.044(9) -0.024(7) C44 0.150(13) 0.035(5) 0.112(10) -0.003(5) 0.053(9) -0.002(7) C45 0.110(10) 0.050(6) 0.123(10) 0.002(6) 0.043(8) 0.029(7) C46 0.069(6) 0.047(5) 0.090(7) -0.005(5) 0.032(6) 0.006(5) C51 0.043(4) 0.041(4) 0.049(4) -0.003(3) 0.016(4) -0.004(4) C52 0.053(5) 0.066(6) 0.061(5) 0.006(5) 0.019(4) 0.013(5) C53 0.052(6) 0.085(7) 0.095(8) -0.001(6) 0.028(6) 0.016(5) C54 0.074(7) 0.093(8) 0.080(7) -0.009(6) 0.050(6) -0.015(6) C55 0.084(8) 0.076(7) 0.063(6) 0.004(5) 0.033(6) -0.010(6) C56 0.068(6) 0.061(5) 0.055(5) 0.011(4) 0.020(5) 0.004(5) _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 Os1 C12 1.881(8) . ? Os1 C11 1.939(9) . ? Os1 C13 1.949(9) . ? Os1 Sb4 2.6881(6) . ? Os1 Os3 2.8950(4) . ? Os1 Os2 3.0693(4) . ? Os2 C22 1.897(10) . ? Os2 C21 1.946(9) . ? Os2 C23 1.953(8) . ? Os2 Sb4 2.6823(6) 2_655 ? Os2 Os3 2.8881(4) . ? Os3 C32 1.914(9) . ? Os3 C34 1.917(10) . ? Os3 C31 1.946(12) . ? Os3 C33 1.956(10) . ? Sb4 C51 2.148(7) . ? Sb4 C41 2.154(7) . ? Sb4 Os2 2.6823(5) 2_655 ? O11 C11 1.149(10) . ? O12 C12 1.155(9) . ? O13 C13 1.131(9) . ? O21 C21 1.149(10) . ? O22 C22 1.137(11) . ? O23 C23 1.138(9) . ? O31 C31 1.145(12) . ? O32 C32 1.135(10) . ? O33 C33 1.145(10) . ? O34 C34 1.138(11) . ? C41 C46 1.369(12) . ? C41 C42 1.383(11) . ? C42 C43 1.400(13) . ? C43 C44 1.38(2) . ? C44 C45 1.36(2) . ? C45 C46 1.381(13) . ? C51 C52 1.383(11) . ? C51 C56 1.394(11) . ? C52 C53 1.396(12) . ? C53 C54 1.375(14) . ? C54 C55 1.355(15) . ? C55 C56 1.396(12) . ? C1 C2 1.23(4) . ? C2 C3 1.31(4) . ? C3 C3 1.24(5) 2_755 ? C4 C5 1.27(2) . ? C5 C6 1.22(2) . ? C6 C6 1.49(6) 2 ? C7 C8 1.24(2) . ? C8 C9 1.20(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 C12 Os1 C11 87.2(4) . . ? C12 Os1 C13 89.6(3) . . ? C11 Os1 C13 176.7(3) . . ? C12 Os1 Sb4 94.6(3) . . ? C11 Os1 Sb4 88.3(3) . . ? C13 Os1 Sb4 92.6(2) . . ? C12 Os1 Os3 95.3(3) . . ? C11 Os1 Os3 88.7(3) . . ? C13 Os1 Os3 91.0(2) . . ? Sb4 Os1 Os3 169.49(2) . . ? C12 Os1 Os2 153.0(3) . . ? C11 Os1 Os2 94.5(2) . . ? C13 Os1 Os2 88.1(2) . . ? Sb4 Os1 Os2 112.414(15) . . ? Os3 Os1 Os2 57.835(10) . . ? C22 Os2 C21 89.9(4) . . ? C22 Os2 C23 87.9(4) . . ? C21 Os2 C23 175.9(3) . . ? C22 Os2 Sb4 100.3(3) . 2_655 ? C21 Os2 Sb4 90.8(2) . 2_655 ? C23 Os2 Sb4 86.2(2) . 2_655 ? C22 Os2 Os3 91.8(3) . . ? C21 Os2 Os3 95.9(2) . . ? C23 Os2 Os3 87.7(2) . . ? Sb4 Os2 Os3 166.19(2) 2_655 . ? C22 Os2 Os1 149.5(3) . . ? C21 Os2 Os1 88.7(2) . . ? C23 Os2 Os1 94.9(2) . . ? Sb4 Os2 Os1 110.194(15) 2_655 . ? Os3 Os2 Os1 58.055(10) . . ? C32 Os3 C34 100.3(4) . . ? C32 Os3 C31 93.6(4) . . ? C34 Os3 C31 89.2(5) . . ? C32 Os3 C33 89.6(4) . . ? C34 Os3 C33 90.7(4) . . ? C31 Os3 C33 176.8(4) . . ? C32 Os3 Os2 159.9(3) . . ? C34 Os3 Os2 99.8(3) . . ? C31 Os3 Os2 86.0(3) . . ? C33 Os3 Os2 90.9(2) . . ? C32 Os3 Os1 95.8(3) . . ? C34 Os3 Os1 163.9(3) . . ? C31 Os3 Os1 90.0(3) . . ? C33 Os3 Os1 89.2(3) . . ? Os2 Os3 Os1 64.110(10) . . ? C51 Sb4 C41 97.6(3) . . ? C51 Sb4 Os2 110.6(2) . 2_655 ? C41 Sb4 Os2 107.4(2) . 2_655 ? C51 Sb4 Os1 107.1(2) . . ? C41 Sb4 Os1 109.9(2) . . ? Os2 Sb4 Os1 121.61(2) 2_655 . ? O11 C11 Os1 177.2(8) . . ? O12 C12 Os1 178.3(7) . . ? O13 C13 Os1 178.6(7) . . ? O21 C21 Os2 177.0(7) . . ? O22 C22 Os2 177.4(9) . . ? O23 C23 Os2 173.8(7) . . ? O31 C31 Os3 177.0(8) . . ? O32 C32 Os3 177.9(9) . . ? O33 C33 Os3 177.3(8) . . ? O34 C34 Os3 179.3(10) . . ? C46 C41 C42 118.2(8) . . ? C46 C41 Sb4 122.2(6) . . ? C42 C41 Sb4 119.5(6) . . ? C41 C42 C43 121.5(10) . . ? C44 C43 C42 118.2(11) . . ? C45 C44 C43 120.6(9) . . ? C44 C45 C46 120.2(11) . . ? C41 C46 C45 121.2(10) . . ? C52 C51 C56 118.6(8) . . ? C52 C51 Sb4 122.7(6) . . ? C56 C51 Sb4 118.6(6) . . ? C51 C52 C53 120.2(9) . . ? C54 C53 C52 119.7(9) . . ? C55 C54 C53 121.3(9) . . ? C54 C55 C56 119.3(9) . . ? C51 C56 C55 120.8(9) . . ? C1 C2 C3 159.3(44) . . ? C3 C3 C2 164.9(54) 2_755 . ? C6 C5 C4 135.1(35) . . ? C5 C6 C6 155.5(22) . 2 ? C9 C8 C7 139.9(36) . . ? _refine_diff_density_max 1.654 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.463 #===END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34.50 H21 Cl O10 Os3 P Sb' _chemical_formula_weight 1354.28 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' 'P' 'P' 0.1023 0.0942 '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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.631 _cell_length_b 18.0529(2) _cell_length_c 17.18850(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.4690(10) _cell_angle_gamma 90.00 _cell_volume 3907.45(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5663 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.225 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.040 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2476 _exptl_absorpt_coefficient_mu 10.569 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.308205 _exptl_absorpt_correction_T_max 0.534071 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 25323 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 29.35 _reflns_number_total 9701 _reflns_number_gt 6860 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SIEMENS SMART' _computing_cell_refinement 'SIEMENS SAINT' _computing_data_reduction 'SIEMENS SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. ; _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^)+(0.0280P)^2^+21.0682P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9701 _refine_ls_number_parameters 453 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.175 _refine_ls_shift/su_mean 0.013 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 Os1 Os -0.02445(3) 0.077138(19) -0.16533(2) 0.03898(10) Uani 1 1 d . . . Os2 Os -0.16154(3) 0.249907(17) -0.317549(19) 0.03190(8) Uani 1 1 d . . . Os3 Os -0.22922(3) 0.161248(19) -0.18652(2) 0.04080(10) Uani 1 1 d . . . Sb4 Sb 0.01261(5) 0.17346(3) -0.28021(3) 0.03471(13) Uani 1 1 d . . . P5 P -0.32472(17) 0.24891(12) -0.26055(13) 0.0344(5) Uani 1 1 d . . . O11 O -0.1128(6) -0.0202(4) -0.3032(4) 0.066(2) Uani 1 1 d . . . O12 O 0.1892(7) -0.0015(5) -0.1499(5) 0.083(3) Uani 1 1 d . . . O13 O 0.0559(7) 0.1901(5) -0.0396(5) 0.081(3) Uani 1 1 d . . . O14 O -0.1409(8) -0.0139(5) -0.0458(5) 0.096(3) Uani 1 1 d . . . O21 O -0.2382(7) 0.1274(4) -0.4332(5) 0.075(2) Uani 1 1 d . . . O22 O -0.1387(8) 0.3573(5) -0.4521(5) 0.087(3) Uani 1 1 d . . . O23 O -0.0771(7) 0.3760(4) -0.2099(5) 0.073(2) Uani 1 1 d . . . O31 O -0.3302(7) 0.0390(4) -0.2920(6) 0.096(3) Uani 1 1 d . . . O32 O -0.3639(10) 0.1130(8) -0.0595(8) 0.156(5) Uani 1 1 d . . . O33 O -0.1381(7) 0.2825(5) -0.0748(4) 0.080(3) Uani 1 1 d . . . C11 C -0.0826(8) 0.0150(5) -0.2526(6) 0.046(2) Uani 1 1 d . . . C12 C 0.1105(9) 0.0289(5) -0.1570(5) 0.051(3) Uani 1 1 d . . . C13 C 0.0236(9) 0.1508(6) -0.0865(6) 0.054(3) Uani 1 1 d . . . C14 C -0.0975(9) 0.0211(6) -0.0897(6) 0.059(3) Uani 1 1 d . . . C21 C -0.2108(8) 0.1714(5) -0.3905(6) 0.049(2) Uani 1 1 d . . . C22 C -0.1472(9) 0.3153(5) -0.4012(6) 0.053(3) Uani 1 1 d . . . C23 C -0.1078(8) 0.3282(5) -0.2481(5) 0.047(2) Uani 1 1 d . . . C31 C -0.2889(8) 0.0845(6) -0.2550(7) 0.062(3) Uani 1 1 d . . . C32 C -0.3086(9) 0.1268(6) -0.1188(11) 0.102(6) Uani 1 1 d . . . C33 C -0.1694(8) 0.2370(6) -0.1177(6) 0.049(2) Uani 1 1 d . . . C411 C 0.1456(7) 0.2470(5) -0.2546(6) 0.046(2) Uani 1 1 d . . . C412 C 0.2130(10) 0.2392(8) -0.1892(7) 0.079(4) Uani 1 1 d . . . H412 H 0.2035 0.2013 -0.1538 0.095 Uiso 1 1 calc R . . C413 C 0.2977(11) 0.2900(10) -0.1762(9) 0.098(5) Uani 1 1 d . . . H413 H 0.3420 0.2870 -0.1305 0.117 Uiso 1 1 calc R . . C414 C 0.3146(11) 0.3416(8) -0.2280(11) 0.094(5) Uani 1 1 d . . . H414 H 0.3714 0.3740 -0.2188 0.113 Uiso 1 1 calc R . . C415 C 0.2492(11) 0.3481(7) -0.2957(10) 0.091(5) Uani 1 1 d . . . H415 H 0.2625 0.3836 -0.3328 0.109 Uiso 1 1 calc R . . C416 C 0.1626(9) 0.3005(6) -0.3074(8) 0.069(3) Uani 1 1 d . . . H416 H 0.1162 0.3054 -0.3518 0.083 Uiso 1 1 calc R . . C421 C 0.0698(7) 0.1146(4) -0.3765(5) 0.0351(19) Uani 1 1 d . . . C422 C 0.0514(8) 0.1430(5) -0.4513(5) 0.050(2) Uani 1 1 d . . . H422 H 0.0121 0.1863 -0.4592 0.060 Uiso 1 1 calc R . . C423 C 0.0907(10) 0.1077(6) -0.5136(6) 0.066(3) Uani 1 1 d . . . H423 H 0.0786 0.1276 -0.5634 0.079 Uiso 1 1 calc R . . C424 C 0.1480(10) 0.0428(7) -0.5029(6) 0.071(3) Uani 1 1 d . . . H424 H 0.1751 0.0195 -0.5454 0.085 Uiso 1 1 calc R . . C425 C 0.1650(8) 0.0124(6) -0.4292(6) 0.058(3) Uani 1 1 d . . . H425 H 0.2017 -0.0321 -0.4220 0.069 Uiso 1 1 calc R . . C426 C 0.1268(8) 0.0489(5) -0.3659(5) 0.046(2) Uani 1 1 d . . . H426 H 0.1395 0.0293 -0.3160 0.055 Uiso 1 1 calc R . . C511 C -0.4412(7) 0.2230(5) -0.3203(6) 0.046(2) Uani 1 1 d . . . C512 C -0.4582(10) 0.2440(8) -0.3960(7) 0.082(4) Uani 1 1 d . . . H512 H -0.4062 0.2709 -0.4191 0.098 Uiso 1 1 calc R . . C513 C -0.5529(12) 0.2257(11) -0.4405(10) 0.119(6) Uani 1 1 d . . . H513 H -0.5631 0.2411 -0.4921 0.143 Uiso 1 1 calc R . . C514 C -0.6308(12) 0.1852(10) -0.4078(12) 0.109(7) Uani 1 1 d . . . H514 H -0.6931 0.1725 -0.4371 0.131 Uiso 1 1 calc R . . C515 C -0.6150(10) 0.1651(7) -0.3347(12) 0.101(6) Uani 1 1 d . . . H515 H -0.6674 0.1380 -0.3123 0.121 Uiso 1 1 calc R . . C516 C -0.5222(9) 0.1830(6) -0.2891(8) 0.073(3) Uani 1 1 d . . . H516 H -0.5144 0.1681 -0.2372 0.087 Uiso 1 1 calc R . . C521 C -0.3675(6) 0.3332(5) -0.2109(5) 0.040(2) Uani 1 1 d . . . C522 C -0.3742(9) 0.4000(5) -0.2517(7) 0.059(3) Uani 1 1 d . . . H522 H -0.3540 0.4026 -0.3025 0.070 Uiso 1 1 calc R . . C523 C -0.4112(10) 0.4620(6) -0.2159(9) 0.076(4) Uani 1 1 d . . . H523 H -0.4177 0.5061 -0.2437 0.092 Uiso 1 1 calc R . . C524 C -0.4382(9) 0.4606(7) -0.1414(8) 0.073(4) Uani 1 1 d . . . H524 H -0.4604 0.5036 -0.1177 0.087 Uiso 1 1 calc R . . C525 C -0.4326(9) 0.3963(7) -0.1018(7) 0.069(3) Uani 1 1 d . . . H525 H -0.4529 0.3950 -0.0510 0.083 Uiso 1 1 calc R . . C526 C -0.3968(8) 0.3311(6) -0.1357(6) 0.057(3) Uani 1 1 d . . . H526 H -0.3929 0.2871 -0.1075 0.069 Uiso 1 1 calc R . . C10 C -0.580(3) 0.034(2) -0.0231(15) 0.146(15) Uiso 0.50 1 d PD . . H10A H -0.5146 0.0170 -0.0431 0.175 Uiso 0.50 1 calc PR . . H10B H -0.6319 -0.0052 -0.0290 0.175 Uiso 0.50 1 calc PR . . Cl11 Cl -0.6273(16) 0.1133(12) -0.0760(11) 0.256(6) Uiso 0.50 1 d PD . . Cl12 Cl -0.5564(15) 0.0580(11) 0.0770(12) 0.256(6) Uiso 0.50 1 d PD . . 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 Os1 0.0473(2) 0.03494(18) 0.03447(18) 0.00217(14) 0.00159(15) 0.00552(16) Os2 0.03291(18) 0.02772(15) 0.03498(17) -0.00054(13) 0.00204(13) 0.00021(14) Os3 0.0405(2) 0.03685(19) 0.0457(2) 0.00654(15) 0.00779(15) 0.00144(16) Sb4 0.0349(3) 0.0314(3) 0.0377(3) 0.0000(2) 0.0020(2) 0.0023(2) P5 0.0281(11) 0.0360(11) 0.0395(12) -0.0009(9) 0.0046(9) 0.0014(9) O11 0.069(5) 0.067(5) 0.060(5) -0.026(4) -0.001(4) -0.002(4) O12 0.082(6) 0.091(6) 0.074(6) 0.005(5) -0.001(5) 0.042(5) O13 0.083(6) 0.086(6) 0.071(5) -0.042(5) -0.004(4) -0.008(5) O14 0.137(9) 0.089(6) 0.062(5) 0.029(5) 0.021(5) -0.023(6) O21 0.089(6) 0.063(5) 0.071(5) -0.039(4) -0.010(4) -0.013(4) O22 0.138(8) 0.066(5) 0.058(5) 0.016(4) 0.026(5) 0.001(5) O23 0.087(6) 0.049(4) 0.083(6) -0.029(4) -0.001(5) -0.016(4) O31 0.063(6) 0.047(5) 0.175(10) -0.023(5) -0.020(6) -0.005(4) O32 0.122(10) 0.205(14) 0.149(11) 0.073(10) 0.068(8) 0.003(10) O33 0.113(7) 0.068(5) 0.054(5) -0.015(4) -0.013(5) 0.004(5) C11 0.049(6) 0.040(5) 0.049(6) 0.010(4) 0.004(4) -0.003(4) C12 0.063(7) 0.047(5) 0.043(5) 0.006(4) -0.006(5) 0.024(5) C13 0.060(7) 0.054(6) 0.048(6) -0.003(5) 0.003(5) 0.008(5) C14 0.075(8) 0.055(6) 0.046(6) 0.000(5) 0.003(5) 0.006(6) C21 0.047(6) 0.051(6) 0.048(6) 0.004(5) -0.003(4) 0.001(5) C22 0.066(7) 0.043(5) 0.053(6) 0.002(5) 0.017(5) -0.009(5) C23 0.049(6) 0.048(6) 0.042(5) 0.002(4) -0.002(4) 0.004(5) C31 0.040(6) 0.045(6) 0.099(9) 0.014(6) -0.009(6) -0.001(5) C32 0.044(7) 0.049(7) 0.218(18) 0.054(9) 0.034(9) 0.011(6) C33 0.053(6) 0.052(6) 0.042(5) 0.005(4) -0.006(5) 0.014(5) C411 0.038(5) 0.043(5) 0.057(6) -0.011(4) 0.004(4) -0.005(4) C412 0.067(8) 0.097(10) 0.070(8) 0.002(7) -0.013(6) -0.022(7) C413 0.067(9) 0.128(13) 0.092(11) -0.003(10) -0.026(8) -0.043(9) C414 0.055(8) 0.072(9) 0.155(15) -0.029(9) -0.006(9) -0.014(7) C415 0.067(9) 0.051(7) 0.152(14) 0.016(8) -0.007(9) -0.017(6) C416 0.057(7) 0.053(6) 0.096(9) 0.013(6) -0.007(6) -0.012(6) C421 0.031(5) 0.034(4) 0.040(5) 0.004(4) 0.004(4) 0.000(4) C422 0.061(7) 0.045(5) 0.044(6) 0.001(4) 0.012(5) 0.018(5) C423 0.088(9) 0.072(7) 0.037(6) -0.005(5) 0.002(5) 0.018(7) C424 0.087(9) 0.086(9) 0.040(6) -0.014(6) 0.004(6) 0.014(7) C425 0.057(7) 0.044(5) 0.073(8) -0.011(5) 0.010(5) 0.015(5) C426 0.054(6) 0.043(5) 0.040(5) 0.003(4) 0.007(4) 0.009(4) C511 0.033(5) 0.043(5) 0.061(6) -0.010(4) 0.004(4) -0.002(4) C512 0.052(7) 0.129(12) 0.061(8) -0.007(8) -0.013(6) -0.012(8) C513 0.069(10) 0.187(18) 0.097(12) -0.042(12) -0.027(9) 0.006(12) C514 0.052(9) 0.121(14) 0.149(16) -0.076(13) -0.029(10) -0.005(9) C515 0.040(7) 0.066(8) 0.194(18) -0.045(11) -0.012(10) -0.005(6) C516 0.050(7) 0.051(6) 0.117(11) -0.001(6) 0.005(7) 0.002(5) C521 0.025(4) 0.038(5) 0.054(6) -0.003(4) -0.003(4) -0.002(4) C522 0.061(7) 0.042(6) 0.073(7) -0.004(5) 0.013(6) -0.001(5) C523 0.079(9) 0.037(6) 0.111(11) -0.009(6) -0.010(8) 0.010(6) C524 0.060(8) 0.058(7) 0.098(10) -0.031(7) -0.007(7) 0.017(6) C525 0.057(7) 0.084(9) 0.067(8) -0.021(7) 0.004(6) 0.019(6) C526 0.063(7) 0.050(6) 0.059(7) -0.008(5) 0.011(5) 0.009(5) _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 Os1 C12 1.910(10) . ? Os1 C14 1.936(12) . ? Os1 C13 1.962(10) . ? Os1 C11 1.970(10) . ? Os1 Sb4 2.6993(6) . ? Os1 Os3 2.9968(5) . ? Os2 C22 1.880(10) . ? Os2 C23 1.939(10) . ? Os2 C21 1.961(10) . ? Os2 P5 2.350(2) . ? Os2 Sb4 2.6334(6) . ? Os2 Os3 2.9436(5) . ? Os3 C32 1.711(14) . ? Os3 C33 1.924(10) . ? Os3 C31 1.932(12) . ? Os3 P5 2.311(2) . ? Sb4 C421 2.139(8) . ? Sb4 C411 2.160(9) . ? P5 C511 1.790(9) . ? P5 C521 1.845(9) . ? O11 C11 1.119(11) . ? O12 C12 1.134(11) . ? O13 C13 1.125(11) . ? O14 C14 1.155(13) . ? O21 C21 1.119(11) . ? O22 C22 1.168(11) . ? O23 C23 1.134(11) . ? O31 C31 1.141(12) . ? O32 C32 1.304(17) . ? O33 C33 1.154(11) . ? C411 C416 1.353(14) . ? C411 C412 1.364(14) . ? C412 C413 1.412(17) . ? C413 C414 1.317(19) . ? C414 C415 1.379(19) . ? C415 C416 1.393(15) . ? C421 C422 1.387(12) . ? C421 C426 1.391(12) . ? C422 C423 1.372(13) . ? C423 C424 1.383(15) . ? C424 C425 1.382(14) . ? C425 C426 1.391(13) . ? C511 C512 1.356(15) . ? C511 C516 1.394(15) . ? C512 C513 1.407(17) . ? C513 C514 1.38(2) . ? C514 C515 1.31(2) . ? C515 C516 1.396(17) . ? C521 C526 1.373(13) . ? C521 C522 1.394(13) . ? C522 C523 1.377(15) . ? C523 C524 1.350(17) . ? C524 C525 1.344(17) . ? C525 C526 1.404(14) . ? C10 Cl11 1.77(3) . ? C10 Cl12 1.78(3) . ? 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 C12 Os1 C14 100.4(4) . . ? C12 Os1 C13 91.8(4) . . ? C14 Os1 C13 91.6(4) . . ? C12 Os1 C11 94.3(4) . . ? C14 Os1 C11 92.6(4) . . ? C13 Os1 C11 171.9(4) . . ? C12 Os1 Sb4 98.2(3) . . ? C14 Os1 Sb4 161.1(3) . . ? C13 Os1 Sb4 90.4(3) . . ? C11 Os1 Sb4 83.4(3) . . ? C12 Os1 Os3 175.6(3) . . ? C14 Os1 Os3 83.9(3) . . ? C13 Os1 Os3 87.6(3) . . ? C11 Os1 Os3 85.9(3) . . ? Sb4 Os1 Os3 77.402(16) . . ? C22 Os2 C23 87.9(4) . . ? C22 Os2 C21 90.5(4) . . ? C23 Os2 C21 177.6(4) . . ? C22 Os2 P5 117.6(3) . . ? C23 Os2 P5 91.4(3) . . ? C21 Os2 P5 90.9(3) . . ? C22 Os2 Sb4 112.8(3) . . ? C23 Os2 Sb4 89.2(3) . . ? C21 Os2 Sb4 89.7(3) . . ? P5 Os2 Sb4 129.60(6) . . ? C22 Os2 Os3 167.8(3) . . ? C23 Os2 Os3 91.9(3) . . ? C21 Os2 Os3 90.0(3) . . ? P5 Os2 Os3 50.24(5) . . ? Sb4 Os2 Os3 79.365(17) . . ? C32 Os3 C33 93.6(7) . . ? C32 Os3 C31 86.1(7) . . ? C33 Os3 C31 179.5(4) . . ? C32 Os3 P5 108.4(4) . . ? C33 Os3 P5 90.9(3) . . ? C31 Os3 P5 89.6(3) . . ? C32 Os3 Os2 159.8(4) . . ? C33 Os3 Os2 87.7(3) . . ? C31 Os3 Os2 92.7(3) . . ? P5 Os3 Os2 51.43(5) . . ? C32 Os3 Os1 106.2(4) . . ? C33 Os3 Os1 89.5(3) . . ? C31 Os3 Os1 90.2(3) . . ? P5 Os3 Os1 145.34(6) . . ? Os2 Os3 Os1 93.965(14) . . ? C421 Sb4 C411 99.1(3) . . ? C421 Sb4 Os2 113.5(2) . . ? C411 Sb4 Os2 110.4(3) . . ? C421 Sb4 Os1 109.5(2) . . ? C411 Sb4 Os1 115.1(3) . . ? Os2 Sb4 Os1 109.07(2) . . ? C511 P5 C521 102.9(4) . . ? C511 P5 Os3 120.5(3) . . ? C521 P5 Os3 118.0(3) . . ? C511 P5 Os2 118.1(3) . . ? C521 P5 Os2 119.0(3) . . ? Os3 P5 Os2 78.33(7) . . ? O11 C11 Os1 177.9(9) . . ? O12 C12 Os1 177.2(10) . . ? O13 C13 Os1 175.8(10) . . ? O14 C14 Os1 178.3(10) . . ? O21 C21 Os2 178.7(10) . . ? O22 C22 Os2 178.4(9) . . ? O23 C23 Os2 177.3(9) . . ? O31 C31 Os3 175.0(11) . . ? O32 C32 Os3 168.2(15) . . ? O33 C33 Os3 176.7(10) . . ? C416 C411 C412 120.3(10) . . ? C416 C411 Sb4 117.6(7) . . ? C412 C411 Sb4 122.0(8) . . ? C411 C412 C413 118.6(12) . . ? C414 C413 C412 120.9(13) . . ? C413 C414 C415 120.8(13) . . ? C414 C415 C416 118.8(13) . . ? C411 C416 C415 120.5(12) . . ? C422 C421 C426 118.9(8) . . ? C422 C421 Sb4 119.4(6) . . ? C426 C421 Sb4 121.7(6) . . ? C423 C422 C421 120.5(9) . . ? C422 C423 C424 120.5(10) . . ? C425 C424 C423 120.1(10) . . ? C424 C425 C426 119.4(10) . . ? C421 C426 C425 120.6(9) . . ? C512 C511 C516 116.6(10) . . ? C512 C511 P5 122.7(8) . . ? C516 C511 P5 120.6(9) . . ? C511 C512 C513 121.4(14) . . ? C514 C513 C512 120.4(16) . . ? C515 C514 C513 118.6(14) . . ? C514 C515 C516 122.2(16) . . ? C511 C516 C515 120.9(14) . . ? C526 C521 C522 119.1(9) . . ? C526 C521 P5 121.6(7) . . ? C522 C521 P5 119.3(8) . . ? C523 C522 C521 119.2(11) . . ? C524 C523 C522 121.9(12) . . ? C525 C524 C523 119.3(11) . . ? C524 C525 C526 121.3(12) . . ? C521 C526 C525 119.2(10) . . ? Cl11 C10 Cl12 109(2) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 29.35 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 3.291 _refine_diff_density_min -1.824 _refine_diff_density_rms 0.203 #====END data_2a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H27 O10 Os3 Sb2' _chemical_formula_weight 1445.69 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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3803(2) _cell_length_b 17.9495(2) _cell_length_c 17.69960(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.0970(10) _cell_angle_gamma 90.00 _cell_volume 4208.53(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'blocks' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.225 _exptl_crystal_size_mid 0.155 _exptl_crystal_size_min 0.120 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2636 _exptl_absorpt_coefficient_mu 10.342 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.219775 _exptl_absorpt_correction_T_max 0.372986 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 26494 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 29.14 _reflns_number_total 10238 _reflns_number_gt 6246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+3.8353P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10238 _refine_ls_number_parameters 341 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1125 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1490 _refine_ls_wR_factor_gt 0.1212 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.010 _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 Os1 Os -0.01539(3) 1.07810(2) 0.82775(3) 0.04484(14) Uani 1 1 d . . . Os2 Os -0.14960(3) 1.25293(2) 0.67103(3) 0.04172(13) Uani 1 1 d . . . Os3 Os -0.21211(4) 1.16030(3) 0.80040(3) 0.05204(15) Uani 1 1 d . . . Sb4 Sb 0.01539(5) 1.17505(4) 0.71569(4) 0.04108(18) Uani 1 1 d . . . Sb5 Sb -0.32456(6) 1.25867(4) 0.72075(5) 0.0519(2) Uani 1 1 d . . . O11 O -0.1067(8) 0.9790(6) 0.6916(6) 0.080(3) Uani 1 1 d . . . O12 O 0.1907(8) 0.9980(6) 0.8484(6) 0.092(3) Uani 1 1 d . . . O13 O 0.0622(8) 1.1957(7) 0.9500(6) 0.093(3) Uani 1 1 d . . . O14 O -0.1150(10) 0.9859(7) 0.9446(6) 0.105(4) Uani 1 1 d . . . O21 O -0.2237(8) 1.1290(6) 0.5552(6) 0.091(3) Uani 1 1 d . . . O22 O -0.1140(10) 1.3585(6) 0.5425(6) 0.102(4) Uani 1 1 d . . . O23 O -0.0742(9) 1.3765(5) 0.7878(6) 0.090(3) Uani 1 1 d . . . O31 O -0.3102(9) 1.0428(6) 0.6851(8) 0.114(5) Uani 1 1 d . . . O32 O -0.3295(13) 1.1000(11) 0.9219(11) 0.195(9) Uani 1 1 d . . . O33 O -0.1296(9) 1.2826(7) 0.9153(6) 0.094(4) Uani 1 1 d . . . C11 C -0.0733(9) 1.0165(7) 0.7428(7) 0.056(3) Uani 1 1 d . . . C12 C 0.1123(11) 1.0298(8) 0.8411(8) 0.065(4) Uani 1 1 d . . . C13 C 0.0315(10) 1.1521(8) 0.9034(8) 0.062(3) Uani 1 1 d . . . C14 C -0.0793(11) 1.0219(8) 0.9018(7) 0.063(3) Uani 1 1 d . . . C21 C -0.1959(10) 1.1737(7) 0.5992(8) 0.059(3) Uani 1 1 d . . . C22 C -0.1290(11) 1.3171(8) 0.5901(8) 0.064(4) Uani 1 1 d . . . C23 C -0.0998(9) 1.3314(7) 0.7456(7) 0.054(3) Uani 1 1 d . . . C31 C -0.2715(10) 1.0851(8) 0.7289(10) 0.076(4) Uani 1 1 d . . . C32 C -0.2839(13) 1.1225(11) 0.8749(11) 0.105(6) Uani 1 1 d . . . C33 C -0.1551(11) 1.2365(9) 0.8714(8) 0.066(4) Uani 1 1 d . . . C411 C 0.1422(10) 1.2483(7) 0.7457(7) 0.058(3) Uiso 1 1 d . . . C412 C 0.1522(12) 1.3078(9) 0.6958(9) 0.082(4) Uiso 1 1 d . . . H412 H 0.1037 1.3165 0.6537 0.098 Uiso 1 1 calc R . . C413 C 0.2426(15) 1.3565(11) 0.7123(11) 0.107(6) Uiso 1 1 d . . . H413 H 0.2558 1.3937 0.6785 0.128 Uiso 1 1 calc R . . C414 C 0.3047(16) 1.3445(11) 0.7781(11) 0.110(6) Uiso 1 1 d . . . H414 H 0.3537 1.3804 0.7932 0.132 Uiso 1 1 calc R . . C415 C 0.3016(16) 1.2864(12) 0.8225(12) 0.116(7) Uiso 1 1 d . . . H415 H 0.3526 1.2780 0.8629 0.140 Uiso 1 1 calc R . . C416 C 0.2167(14) 1.2352(10) 0.8073(10) 0.098(5) Uiso 1 1 d . . . H416 H 0.2125 1.1941 0.8386 0.118 Uiso 1 1 calc R . . C421 C 0.0677(8) 1.1154(5) 0.6226(6) 0.038(2) Uiso 1 1 d . . . C422 C 0.0475(10) 1.1421(7) 0.5510(7) 0.057(3) Uiso 1 1 d . . . H422 H 0.0098 1.1855 0.5422 0.069 Uiso 1 1 calc R . . C423 C 0.0824(11) 1.1053(8) 0.4888(8) 0.072(4) Uiso 1 1 d . . . H423 H 0.0698 1.1255 0.4399 0.087 Uiso 1 1 calc R . . C424 C 0.1351(10) 1.0394(7) 0.5014(8) 0.066(4) Uiso 1 1 d . . . H424 H 0.1557 1.0132 0.4610 0.079 Uiso 1 1 calc R . . C425 C 0.1569(10) 1.0126(8) 0.5758(8) 0.070(4) Uiso 1 1 d . . . H425 H 0.1954 0.9696 0.5852 0.084 Uiso 1 1 calc R . . C426 C 0.1224(9) 1.0487(6) 0.6354(7) 0.053(3) Uiso 1 1 d . . . H426 H 0.1353 1.0290 0.6844 0.064 Uiso 1 1 calc R . . C511 C -0.4582(11) 1.2231(8) 0.6516(8) 0.065(3) Uiso 1 1 d . . . C512 C -0.4636(15) 1.2134(10) 0.5769(11) 0.106(6) Uiso 1 1 d . . . H512 H -0.4080 1.2255 0.5531 0.127 Uiso 1 1 calc R . . C513 C -0.5568(18) 1.1834(12) 0.5293(14) 0.138(8) Uiso 1 1 d . . . H513 H -0.5604 1.1730 0.4776 0.166 Uiso 1 1 calc R . . C514 C -0.6340(18) 1.1731(12) 0.5683(13) 0.124(7) Uiso 1 1 d . . . H514 H -0.6943 1.1581 0.5397 0.148 Uiso 1 1 calc R . . C515 C -0.6362(18) 1.1813(12) 0.6429(13) 0.130(7) Uiso 1 1 d . . . H515 H -0.6939 1.1721 0.6652 0.156 Uiso 1 1 calc R . . C516 C -0.5448(14) 1.2049(10) 0.6855(11) 0.094(5) Uiso 1 1 d . . . H516 H -0.5413 1.2087 0.7382 0.113 Uiso 1 1 calc R . . C521 C -0.3734(10) 1.3533(7) 0.7780(7) 0.061(3) Uiso 1 1 d . . . C522 C -0.4007(12) 1.4176(9) 0.7362(10) 0.089(5) Uiso 1 1 d . . . H522 H -0.3957 1.4199 0.6844 0.107 Uiso 1 1 calc R . . C523 C -0.4368(15) 1.4800(11) 0.7747(11) 0.112(6) Uiso 1 1 d . . . H523 H -0.4581 1.5226 0.7471 0.134 Uiso 1 1 calc R . . C524 C -0.4400(13) 1.4779(10) 0.8484(10) 0.094(5) Uiso 1 1 d . . . H524 H -0.4612 1.5198 0.8727 0.113 Uiso 1 1 calc R . . C525 C -0.4141(14) 1.4181(10) 0.8880(11) 0.102(6) Uiso 1 1 d . . . H525 H -0.4171 1.4181 0.9402 0.122 Uiso 1 1 calc R . . C526 C -0.3814(12) 1.3533(9) 0.8533(9) 0.086(5) Uiso 1 1 d . . . H526 H -0.3655 1.3106 0.8823 0.103 Uiso 1 1 calc R . . C100 C -0.311(4) 1.629(3) 0.498(3) 0.186(12) Uiso 0.50 1 d PD A -1 H10A H -0.2971 1.6609 0.4574 0.279 Uiso 0.50 1 calc PR A -1 H10B H -0.2540 1.5964 0.5123 0.279 Uiso 0.50 1 calc PR A -1 H10C H -0.3212 1.6587 0.5415 0.279 Uiso 0.50 1 calc PR A -1 C200 C -0.401(5) 1.585(3) 0.474(3) 0.186(12) Uiso 0.50 1 d PD A -1 H20A H -0.3878 1.5582 0.4280 0.223 Uiso 0.50 1 calc PR A -1 H20B H -0.4544 1.6198 0.4573 0.223 Uiso 0.50 1 calc PR A -1 C300 C -0.443(6) 1.529(4) 0.522(5) 0.186(12) Uiso 0.50 1 d PD A -1 H30A H -0.3932 1.4922 0.5412 0.223 Uiso 0.50 1 calc PR A -1 H30B H -0.4687 1.5530 0.5646 0.223 Uiso 0.50 1 calc PR A -1 C400 C -0.525(6) 1.496(4) 0.469(4) 0.186(12) Uiso 0.50 1 d PD A -1 H40A H -0.5027 1.4805 0.4212 0.223 Uiso 0.50 1 calc PR A -1 H40B H -0.5825 1.5295 0.4575 0.223 Uiso 0.50 1 calc PR A -1 C500 C -0.548(5) 1.432(3) 0.516(4) 0.186(12) Uiso 0.50 1 d PD A -1 H50A H -0.4873 1.4037 0.5336 0.223 Uiso 0.50 1 calc PR A -1 H50B H -0.5793 1.4480 0.5592 0.223 Uiso 0.50 1 calc PR A -1 C600 C -0.618(4) 1.390(3) 0.461(3) 0.186(12) Uiso 0.50 1 d PD A -1 H60A H -0.6387 1.3457 0.4848 0.279 Uiso 0.50 1 calc PR A -1 H60B H -0.5846 1.3761 0.4180 0.279 Uiso 0.50 1 calc PR A -1 H60C H -0.6757 1.4199 0.4433 0.279 Uiso 0.50 1 calc PR A -1 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 Os1 0.0446(3) 0.0437(2) 0.0456(3) 0.0034(2) 0.0040(2) 0.00154(19) Os2 0.0388(2) 0.0385(2) 0.0478(3) -0.00030(19) 0.00635(19) 0.00118(18) Os3 0.0380(3) 0.0535(3) 0.0659(3) 0.0121(2) 0.0120(2) -0.0005(2) Sb4 0.0364(4) 0.0398(4) 0.0470(4) 0.0001(3) 0.0054(3) -0.0001(3) Sb5 0.0360(4) 0.0523(5) 0.0673(5) 0.0012(4) 0.0072(4) 0.0044(3) O11 0.083(7) 0.078(7) 0.072(6) -0.017(6) -0.010(5) -0.015(6) O12 0.075(7) 0.099(8) 0.094(8) 0.000(6) -0.013(6) 0.032(6) O13 0.086(8) 0.108(8) 0.084(7) -0.040(7) 0.006(6) -0.009(7) O14 0.138(11) 0.103(9) 0.079(7) 0.017(7) 0.034(7) -0.031(8) O21 0.086(8) 0.079(7) 0.100(8) -0.037(6) -0.009(6) -0.006(6) O22 0.161(12) 0.083(7) 0.065(7) 0.016(6) 0.027(7) 0.016(8) O23 0.119(10) 0.058(6) 0.095(8) -0.032(6) 0.018(7) -0.024(6) O31 0.075(8) 0.072(7) 0.179(13) -0.030(8) -0.037(8) -0.017(6) O32 0.146(14) 0.25(2) 0.210(17) 0.113(16) 0.104(13) -0.012(14) O33 0.110(9) 0.100(8) 0.069(7) -0.018(7) -0.003(6) 0.017(7) C11 0.053(8) 0.057(7) 0.060(8) 0.013(6) 0.011(6) 0.004(6) C12 0.055(8) 0.065(8) 0.071(9) 0.003(7) -0.003(7) -0.003(7) C13 0.051(8) 0.083(10) 0.053(8) 0.005(7) 0.008(6) 0.000(7) C14 0.073(10) 0.067(8) 0.049(8) -0.002(7) 0.008(7) 0.000(7) C21 0.050(8) 0.052(7) 0.075(9) -0.002(7) 0.003(7) 0.002(6) C22 0.074(10) 0.062(8) 0.058(8) 0.001(7) 0.014(7) -0.002(7) C23 0.054(8) 0.060(8) 0.050(7) 0.010(6) 0.012(6) 0.002(6) C31 0.037(7) 0.053(8) 0.131(13) 0.017(9) -0.006(8) -0.012(6) C32 0.075(12) 0.123(15) 0.124(15) 0.051(12) 0.039(11) 0.014(10) C33 0.061(9) 0.086(10) 0.052(8) 0.012(8) 0.010(7) 0.011(8) _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 Os1 C12 1.900(15) . ? Os1 C13 1.927(15) . ? Os1 C11 1.938(14) . ? Os1 C14 1.946(15) . ? Os1 Sb4 2.7132(8) . ? Os1 Os3 2.9967(6) . ? Os2 C22 1.888(14) . ? Os2 C21 1.950(14) . ? Os2 C23 1.980(14) . ? Os2 Sb5 2.6164(9) . ? Os2 Sb4 2.6384(8) . ? Os2 Os3 3.0408(6) . ? Os3 C32 1.865(17) . ? Os3 C33 1.940(17) . ? Os3 C31 1.943(16) . ? Os3 Sb5 2.6023(9) . ? Sb4 C411 2.153(13) . ? Sb4 C421 2.163(10) . ? Sb5 C511 2.118(14) . ? Sb5 C521 2.127(13) . ? O11 C11 1.166(14) . ? O12 C12 1.186(16) . ? O13 C13 1.169(15) . ? O14 C14 1.148(15) . ? O21 C21 1.144(14) . ? O22 C22 1.161(15) . ? O23 C23 1.123(14) . ? O31 C31 1.154(16) . ? O32 C32 1.170(19) . ? O33 C33 1.153(16) . ? C411 C416 1.39(2) . ? C411 C412 1.405(18) . ? C412 C413 1.49(2) . ? C413 C414 1.35(2) . ? C414 C415 1.31(2) . ? C415 C416 1.46(3) . ? C421 C422 1.346(15) . ? C421 C426 1.404(15) . ? C422 C423 1.418(18) . ? C423 C424 1.380(18) . ? C424 C425 1.393(17) . ? C425 C426 1.372(17) . ? C511 C512 1.33(2) . ? C511 C516 1.42(2) . ? C512 C513 1.50(3) . ? C513 C514 1.33(3) . ? C514 C515 1.33(3) . ? C515 C516 1.41(3) . ? C521 C526 1.352(19) . ? C521 C522 1.392(19) . ? C522 C523 1.43(2) . ? C523 C524 1.31(2) . ? C524 C525 1.30(2) . ? C525 C526 1.41(2) . ? C100 C200 1.46(3) . ? C200 C300 1.48(3) . ? C300 C400 1.47(2) . ? C400 C500 1.48(3) . ? C500 C600 1.47(3) . ? 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 C12 Os1 C13 91.7(6) . . ? C12 Os1 C11 95.2(5) . . ? C13 Os1 C11 171.0(5) . . ? C12 Os1 C14 98.8(6) . . ? C13 Os1 C14 91.2(5) . . ? C11 Os1 C14 93.5(5) . . ? C12 Os1 Sb4 99.0(4) . . ? C13 Os1 Sb4 89.8(4) . . ? C11 Os1 Sb4 83.3(4) . . ? C14 Os1 Sb4 162.1(4) . . ? C12 Os1 Os3 176.7(4) . . ? C13 Os1 Os3 88.0(4) . . ? C11 Os1 Os3 84.8(4) . . ? C14 Os1 Os3 84.5(4) . . ? Sb4 Os1 Os3 77.67(2) . . ? C22 Os2 C21 91.0(6) . . ? C22 Os2 C23 90.0(5) . . ? C21 Os2 C23 178.4(5) . . ? C22 Os2 Sb5 117.7(4) . . ? C21 Os2 Sb5 91.8(4) . . ? C23 Os2 Sb5 88.9(4) . . ? C22 Os2 Sb4 110.2(4) . . ? C21 Os2 Sb4 89.1(4) . . ? C23 Os2 Sb4 89.3(4) . . ? Sb5 Os2 Sb4 132.12(3) . . ? C22 Os2 Os3 171.8(4) . . ? C21 Os2 Os3 89.8(4) . . ? C23 Os2 Os3 89.4(3) . . ? Sb5 Os2 Os3 54.14(2) . . ? Sb4 Os2 Os3 77.99(2) . . ? C32 Os3 C33 89.6(8) . . ? C32 Os3 C31 90.2(8) . . ? C33 Os3 C31 178.9(6) . . ? C32 Os3 Sb5 108.3(5) . . ? C33 Os3 Sb5 91.0(4) . . ? C31 Os3 Sb5 88.1(4) . . ? C32 Os3 Os1 103.6(5) . . ? C33 Os3 Os1 89.2(4) . . ? C31 Os3 Os1 91.9(4) . . ? Sb5 Os3 Os1 148.13(3) . . ? C32 Os3 Os2 162.7(5) . . ? C33 Os3 Os2 88.7(4) . . ? C31 Os3 Os2 91.1(5) . . ? Sb5 Os3 Os2 54.58(2) . . ? Os1 Os3 Os2 93.574(17) . . ? C411 Sb4 C421 99.3(4) . . ? C411 Sb4 Os2 110.3(3) . . ? C421 Sb4 Os2 112.4(3) . . ? C411 Sb4 Os1 114.0(3) . . ? C421 Sb4 Os1 109.8(3) . . ? Os2 Sb4 Os1 110.61(3) . . ? C511 Sb5 C521 103.0(5) . . ? C511 Sb5 Os3 119.0(4) . . ? C521 Sb5 Os3 118.5(4) . . ? C511 Sb5 Os2 121.1(4) . . ? C521 Sb5 Os2 122.8(4) . . ? Os3 Sb5 Os2 71.28(2) . . ? O11 C11 Os1 179.0(12) . . ? O12 C12 Os1 178.1(12) . . ? O13 C13 Os1 178.1(13) . . ? O14 C14 Os1 177.0(13) . . ? O21 C21 Os2 177.6(12) . . ? O22 C22 Os2 177.2(13) . . ? O23 C23 Os2 178.0(12) . . ? O31 C31 Os3 176.8(12) . . ? O32 C32 Os3 179(2) . . ? O33 C33 Os3 174.0(13) . . ? C416 C411 C412 120.0(14) . . ? C416 C411 Sb4 123.0(11) . . ? C412 C411 Sb4 116.8(10) . . ? C411 C412 C413 118.1(15) . . ? C414 C413 C412 117.4(19) . . ? C415 C414 C413 125(2) . . ? C414 C415 C416 119(2) . . ? C411 C416 C415 119.6(17) . . ? C422 C421 C426 119.1(11) . . ? C422 C421 Sb4 119.8(8) . . ? C426 C421 Sb4 121.1(8) . . ? C421 C422 C423 121.4(12) . . ? C424 C423 C422 119.3(13) . . ? C423 C424 C425 118.9(14) . . ? C426 C425 C424 121.0(14) . . ? C425 C426 C421 120.1(12) . . ? C512 C511 C516 117.3(16) . . ? C512 C511 Sb5 122.6(13) . . ? C516 C511 Sb5 120.0(12) . . ? C511 C512 C513 122.0(19) . . ? C514 C513 C512 114(2) . . ? C515 C514 C513 129(3) . . ? C514 C515 C516 115(2) . . ? C515 C516 C511 122.9(18) . . ? C526 C521 C522 118.2(14) . . ? C526 C521 Sb5 122.8(11) . . ? C522 C521 Sb5 119.0(11) . . ? C521 C522 C523 118.6(16) . . ? C524 C523 C522 120.7(19) . . ? C525 C524 C523 121(2) . . ? C524 C525 C526 121.3(18) . . ? C521 C526 C525 120.0(16) . . ? C100 C200 C300 124(6) . . ? C400 C300 C200 102(6) . . ? C300 C400 C500 98(4) . . ? C600 C500 C400 101(6) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 3.246 _refine_diff_density_min -1.355 _refine_diff_density_rms 0.260 #====END