Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Deng, Mingli' 'Leong, Weng Kee' _publ_contact_author_name 'Dr Weng Kee Leong' _publ_contact_author_address ; Chemistry National University of Singapore Kent Ridge Crescent Singapore 119260 SINGAPORE ; _publ_contact_author_email 'CHMLWK@NUS.EDU.SG' _publ_section_title ; Novel Higher Nuclearity Osmium-Antimony Clusters by Alkene- or Diene-Assisted Cluster Condensation ; data_3 _database_code_CSD 171668 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H22 Cl2 O14 Os5 Sb2' _chemical_formula_weight 1979.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7386(2) _cell_length_b 13.5125(3) _cell_length_c 16.0955(2) _cell_angle_alpha 79.6280(10) _cell_angle_beta 75.1440(10) _cell_angle_gamma 74.2680(10) _cell_volume 2358.44(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Irregular block' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 14.714 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.034671 _exptl_absorpt_correction_T_max 0.116198 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11192 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 29.35 _reflns_number_total 18978 _reflns_number_gt 9612 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+16.1928P] 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 11192 _refine_ls_number_parameters 572 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0870 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.148 _refine_ls_shift/su_mean 0.003 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 0.81484(3) 0.73422(3) 0.19394(2) 0.03496(8) Uani 1 1 d . . . Os2 Os 0.57935(3) 0.77450(3) 0.14689(2) 0.03166(8) Uani 1 1 d . . . Os3 Os 0.53090(3) 0.59458(3) 0.27277(2) 0.03235(8) Uani 1 1 d . . . Os4 Os 0.33559(3) 0.93535(3) 0.40190(2) 0.03530(8) Uani 1 1 d . . . Os5 Os 0.17426(3) 0.88462(3) 0.30370(2) 0.03669(8) Uani 1 1 d . . . H12 H 0.669(9) 0.802(8) 0.225(6) 0.050 Uiso 1 1 d . . . H45 H 0.197(9) 0.904(8) 0.395(6) 0.050 Uiso 1 1 d . . . Sb6 Sb 0.41148(4) 0.80475(4) 0.28336(3) 0.03175(12) Uani 1 1 d . . . Sb7 Sb 0.73326(5) 0.59746(4) 0.31880(3) 0.03271(12) Uani 1 1 d . . . O11 O 0.8450(8) 0.8537(7) 0.3289(6) 0.073(2) Uani 1 1 d . . . O12 O 0.8842(8) 0.8908(7) 0.0376(6) 0.077(3) Uani 1 1 d . . . O13 O 1.0755(7) 0.6025(8) 0.1708(7) 0.088(3) Uani 1 1 d . . . O21 O 0.5914(8) 0.9906(6) 0.0610(6) 0.066(2) Uani 1 1 d . . . O22 O 0.4058(8) 0.7735(8) 0.0374(6) 0.079(3) Uani 1 1 d . . . O31 O 0.3167(8) 0.5914(8) 0.1983(7) 0.084(3) Uani 1 1 d . . . O32 O 0.6314(8) 0.3622(6) 0.2656(6) 0.071(2) Uani 1 1 d . . . O33 O 0.3931(7) 0.5744(7) 0.4611(5) 0.065(2) Uani 1 1 d . . . O41 O 0.5820(8) 0.9696(9) 0.3988(6) 0.084(3) Uani 1 1 d . . . O42 O 0.3186(8) 0.7854(8) 0.5707(5) 0.076(3) Uani 1 1 d . . . O43 O 0.1829(8) 1.1269(6) 0.4874(5) 0.072(2) Uani 1 1 d . . . O51 O 0.1319(8) 0.8454(8) 0.1355(6) 0.082(3) Uani 1 1 d . . . O52 O 0.1062(10) 0.6823(8) 0.3987(7) 0.086(3) Uani 1 1 d . . . O53 O -0.0715(6) 1.0357(7) 0.3576(6) 0.075(3) Uani 1 1 d . . . C11 C 0.8338(8) 0.8122(9) 0.2787(6) 0.049(2) Uani 1 1 d . . . C12 C 0.8576(9) 0.8334(8) 0.0972(6) 0.047(2) Uani 1 1 d . . . C13 C 0.9787(8) 0.6525(9) 0.1797(7) 0.051(2) Uani 1 1 d . . . C21 C 0.5852(8) 0.9086(8) 0.0936(6) 0.046(2) Uani 1 1 d . . . C22 C 0.4718(9) 0.7738(9) 0.0792(6) 0.050(2) Uani 1 1 d . . . C31 C 0.3963(9) 0.5941(8) 0.2252(7) 0.049(2) Uani 1 1 d . . . C32 C 0.5985(8) 0.4482(7) 0.2683(6) 0.044(2) Uani 1 1 d . . . C33 C 0.4444(8) 0.5833(7) 0.3917(6) 0.042(2) Uani 1 1 d . . . C41 C 0.4915(10) 0.9555(9) 0.4005(7) 0.054(3) Uani 1 1 d . . . C42 C 0.3271(9) 0.8355(9) 0.5081(6) 0.049(2) Uani 1 1 d . . . C43 C 0.2403(9) 1.0551(8) 0.4585(6) 0.048(2) Uani 1 1 d . . . C51 C 0.1499(9) 0.8602(10) 0.1973(8) 0.059(3) Uani 1 1 d . . . C52 C 0.1293(9) 0.7587(9) 0.3671(7) 0.053(2) Uani 1 1 d . . . C53 C 0.0179(9) 0.9795(9) 0.3364(7) 0.052(2) Uani 1 1 d . . . C101 C 0.7613(7) 0.6497(7) 0.1134(5) 0.0360(18) Uani 1 1 d . . . C102 C 0.6557(8) 0.6061(7) 0.1391(5) 0.0380(19) Uani 1 1 d . . . C103 C 0.6376(9) 0.5473(8) 0.0798(6) 0.047(2) Uani 1 1 d . . . H10A H 0.5695 0.5198 0.0949 0.056 Uiso 1 1 calc R . . C104 C 0.7162(11) 0.5301(9) 0.0022(7) 0.058(3) Uani 1 1 d . . . H10B H 0.7011 0.4916 -0.0345 0.070 Uiso 1 1 calc R . . C105 C 0.8200(11) 0.5706(9) -0.0223(7) 0.060(3) Uani 1 1 d . . . H10C H 0.8753 0.5567 -0.0742 0.072 Uiso 1 1 calc R . . C106 C 0.8396(9) 0.6305(8) 0.0302(6) 0.046(2) Uani 1 1 d . . . H10D H 0.9062 0.6600 0.0114 0.056 Uiso 1 1 calc R . . C201 C 0.3264(7) 1.0365(7) 0.2826(5) 0.0364(18) Uani 1 1 d . . . C202 C 0.2500(8) 1.0129(7) 0.2377(5) 0.0371(18) Uani 1 1 d . . . C203 C 0.2358(9) 1.0714(9) 0.1587(6) 0.053(3) Uani 1 1 d . . . H20A H 0.1873 1.0558 0.1277 0.064 Uiso 1 1 calc R . . C204 C 0.2919(10) 1.1515(8) 0.1255(7) 0.055(3) Uani 1 1 d . . . H20B H 0.2799 1.1900 0.0731 0.067 Uiso 1 1 calc R . . C205 C 0.3650(11) 1.1748(9) 0.1689(7) 0.061(3) Uani 1 1 d . . . H20C H 0.4024 1.2293 0.1463 0.073 Uiso 1 1 calc R . . C206 C 0.3840(10) 1.1155(8) 0.2490(7) 0.056(3) Uani 1 1 d . . . H20D H 0.4351 1.1303 0.2782 0.067 Uiso 1 1 calc R . . C711 C 0.7262(7) 0.6242(7) 0.4467(6) 0.0357(17) Uani 1 1 d . . . C712 C 0.6209(9) 0.6772(9) 0.4964(6) 0.050(2) Uani 1 1 d . . . H71A H 0.5515 0.7002 0.4739 0.060 Uiso 1 1 calc R . . C713 C 0.6157(10) 0.6971(10) 0.5786(7) 0.062(3) Uani 1 1 d . . . H71B H 0.5442 0.7344 0.6104 0.074 Uiso 1 1 calc R . . C714 C 0.7167(12) 0.6615(11) 0.6129(7) 0.069(3) Uani 1 1 d . . . H71C H 0.7134 0.6724 0.6690 0.083 Uiso 1 1 calc R . . C715 C 0.8235(13) 0.6093(12) 0.5640(9) 0.083(4) Uani 1 1 d . . . H71D H 0.8922 0.5852 0.5872 0.100 Uiso 1 1 calc R . . C716 C 0.8292(9) 0.5925(9) 0.4804(8) 0.057(3) Uani 1 1 d . . . H71E H 0.9023 0.5598 0.4470 0.068 Uiso 1 1 calc R . . C721 C 0.8561(7) 0.4478(7) 0.3126(6) 0.0373(18) Uani 1 1 d . . . C722 C 0.8745(8) 0.3804(8) 0.3862(6) 0.048(2) Uani 1 1 d . . . H72A H 0.8317 0.3999 0.4402 0.058 Uiso 1 1 calc R . . C723 C 0.9544(9) 0.2857(9) 0.3811(7) 0.057(3) Uani 1 1 d . . . H72B H 0.9646 0.2409 0.4312 0.069 Uiso 1 1 calc R . . C724 C 1.0208(9) 0.2563(8) 0.2999(8) 0.058(3) Uani 1 1 d . . . H72C H 1.0780 0.1934 0.2960 0.070 Uiso 1 1 calc R . . C725 C 1.0008(11) 0.3208(9) 0.2265(8) 0.069(3) Uani 1 1 d . . . H72D H 1.0421 0.3005 0.1724 0.083 Uiso 1 1 calc R . . C726 C 0.9181(10) 0.4178(8) 0.2325(7) 0.059(3) Uani 1 1 d . . . H72E H 0.9051 0.4617 0.1825 0.071 Uiso 1 1 calc R . . C10 C -0.203(3) 1.1462(17) 0.0902(15) 0.213(16) Uani 0.907(13) 1 d PD A 1 H10E H -0.2767 1.1497 0.0722 0.256 Uiso 0.907(13) 1 calc PR A 1 H10F H -0.1375 1.1010 0.0543 0.256 Uiso 0.907(13) 1 calc PR A 1 Cl11 Cl -0.2167(15) 1.0892(8) 0.1904(6) 0.272(8) Uani 0.907(13) 1 d PD A 1 Cl12 Cl -0.1761(8) 1.2647(5) 0.0664(5) 0.153(3) Uani 0.907(13) 1 d PD A 1 C20 C -0.203(3) 1.1462(17) 0.0902(15) 0.213(16) Uani 0.09 1 d PD A 2 H20E H -0.1825 1.0962 0.0492 0.256 Uiso 0.093(13) 1 calc PR A 2 H20F H -0.2334 1.2135 0.0603 0.256 Uiso 0.093(13) 1 calc PR A 2 Cl21 Cl -0.315(5) 1.118(9) 0.170(4) 0.272(8) Uani 0.09 1 d PD A 2 Cl22 Cl -0.075(4) 1.149(5) 0.115(4) 0.153(3) Uani 0.09 1 d PD A 2 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 0.02938(15) 0.03610(18) 0.03621(16) -0.00274(14) -0.00471(12) -0.00582(13) Os2 0.03148(15) 0.02975(16) 0.02948(15) -0.00378(12) -0.00639(11) -0.00028(12) Os3 0.02988(14) 0.02776(16) 0.03637(16) -0.00452(13) -0.00546(12) -0.00300(12) Os4 0.03580(16) 0.03635(18) 0.03023(15) -0.00707(14) -0.00766(12) -0.00029(13) Os5 0.02865(15) 0.03886(19) 0.03888(17) -0.00709(15) -0.00798(12) 0.00027(13) Sb6 0.0282(2) 0.0308(3) 0.0321(3) -0.0062(2) -0.00581(19) 0.0008(2) Sb7 0.0288(2) 0.0304(3) 0.0333(3) -0.0031(2) -0.00544(19) 0.0005(2) O11 0.081(6) 0.086(6) 0.067(5) -0.027(5) -0.021(4) -0.031(5) O12 0.086(6) 0.064(5) 0.072(6) 0.019(5) -0.005(5) -0.029(5) O13 0.034(4) 0.103(8) 0.119(8) -0.034(6) -0.014(4) 0.009(4) O21 0.078(5) 0.038(4) 0.072(5) 0.005(4) -0.011(4) -0.008(4) O22 0.083(6) 0.090(7) 0.079(6) 0.001(5) -0.052(5) -0.020(5) O31 0.061(5) 0.099(7) 0.113(8) -0.041(6) -0.030(5) -0.023(5) O32 0.086(6) 0.033(4) 0.080(6) -0.005(4) -0.005(5) -0.005(4) O33 0.059(4) 0.065(5) 0.049(4) 0.003(4) 0.010(3) -0.008(4) O41 0.056(5) 0.114(8) 0.092(7) -0.019(6) -0.014(4) -0.032(5) O42 0.074(5) 0.084(6) 0.047(4) 0.020(4) -0.011(4) -0.001(5) O43 0.093(6) 0.052(5) 0.051(4) -0.019(4) -0.009(4) 0.016(4) O51 0.084(6) 0.113(8) 0.065(5) -0.031(5) -0.032(5) -0.023(6) O52 0.115(8) 0.062(6) 0.084(6) 0.006(5) -0.020(6) -0.039(6) O53 0.039(4) 0.060(5) 0.115(7) -0.031(5) -0.007(4) 0.011(4) C11 0.043(5) 0.063(7) 0.045(5) -0.003(5) -0.011(4) -0.023(5) C12 0.052(5) 0.043(5) 0.045(5) 0.000(4) -0.005(4) -0.018(4) C13 0.035(4) 0.056(6) 0.059(6) -0.006(5) -0.007(4) -0.008(4) C21 0.045(5) 0.042(5) 0.045(5) -0.003(4) -0.012(4) -0.002(4) C22 0.045(5) 0.055(6) 0.046(5) -0.004(5) -0.011(4) -0.008(4) C31 0.048(5) 0.042(5) 0.064(6) -0.010(5) -0.020(5) -0.012(4) C32 0.041(4) 0.036(5) 0.044(5) 0.000(4) 0.000(4) -0.005(4) C33 0.033(4) 0.036(5) 0.045(5) -0.001(4) 0.004(4) -0.003(4) C41 0.055(6) 0.064(7) 0.043(5) -0.015(5) -0.010(4) -0.010(5) C42 0.048(5) 0.054(6) 0.042(5) -0.015(5) -0.006(4) -0.001(4) C43 0.059(6) 0.045(6) 0.035(4) -0.006(4) -0.003(4) -0.006(5) C51 0.046(5) 0.062(7) 0.066(7) -0.007(6) -0.018(5) -0.004(5) C52 0.046(5) 0.053(6) 0.050(6) -0.004(5) -0.009(4) 0.000(5) C53 0.040(5) 0.056(6) 0.059(6) -0.004(5) -0.009(4) -0.014(5) C101 0.036(4) 0.031(4) 0.030(4) -0.003(3) -0.005(3) 0.007(3) C102 0.042(4) 0.031(4) 0.031(4) -0.003(3) -0.003(3) 0.005(3) C103 0.052(5) 0.041(5) 0.047(5) -0.014(4) -0.009(4) -0.009(4) C104 0.081(8) 0.048(6) 0.045(5) -0.016(5) -0.003(5) -0.018(6) C105 0.076(7) 0.054(7) 0.040(5) -0.017(5) 0.008(5) -0.009(6) C106 0.047(5) 0.046(5) 0.038(5) -0.009(4) 0.010(4) -0.012(4) C201 0.038(4) 0.032(4) 0.034(4) -0.007(4) -0.004(3) -0.001(3) C202 0.040(4) 0.032(4) 0.032(4) -0.007(3) -0.009(3) 0.006(3) C203 0.057(6) 0.053(6) 0.037(5) -0.001(5) -0.013(4) 0.005(5) C204 0.067(6) 0.037(5) 0.043(5) 0.001(4) -0.004(5) 0.008(5) C205 0.074(7) 0.045(6) 0.054(6) 0.002(5) 0.006(5) -0.019(5) C206 0.065(6) 0.047(6) 0.050(6) -0.010(5) 0.004(5) -0.018(5) C711 0.039(4) 0.030(4) 0.040(4) -0.008(4) -0.010(3) -0.008(3) C712 0.040(5) 0.059(6) 0.048(5) -0.014(5) -0.012(4) 0.000(4) C713 0.053(6) 0.076(8) 0.053(6) -0.026(6) -0.004(5) -0.004(5) C714 0.087(9) 0.082(9) 0.046(6) -0.014(6) -0.022(6) -0.021(7) C715 0.079(8) 0.091(10) 0.088(9) -0.036(8) -0.055(8) 0.019(7) C716 0.045(5) 0.057(7) 0.071(7) -0.024(6) -0.027(5) 0.005(5) C721 0.035(4) 0.030(4) 0.043(4) -0.003(4) -0.008(3) -0.002(3) C722 0.045(5) 0.040(5) 0.046(5) -0.001(4) 0.003(4) -0.001(4) C723 0.050(5) 0.047(6) 0.059(6) 0.008(5) -0.011(5) 0.004(5) C724 0.047(5) 0.035(5) 0.078(8) -0.013(5) 0.006(5) 0.002(4) C725 0.072(7) 0.052(7) 0.058(7) -0.004(6) 0.007(6) 0.005(6) C726 0.065(6) 0.043(6) 0.048(6) -0.009(5) 0.006(5) 0.006(5) C10 0.38(5) 0.12(2) 0.18(3) 0.04(2) -0.16(3) -0.08(3) Cl11 0.55(2) 0.142(8) 0.159(8) 0.023(6) -0.191(11) -0.056(11) Cl12 0.210(8) 0.106(5) 0.144(6) -0.033(4) -0.026(5) -0.040(5) C20 0.38(5) 0.12(2) 0.18(3) 0.04(2) -0.16(3) -0.08(3) Cl21 0.55(2) 0.142(8) 0.159(8) 0.023(6) -0.191(11) -0.056(11) Cl22 0.210(8) 0.106(5) 0.144(6) -0.033(4) -0.026(5) -0.040(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 1.919(10) . ? Os1 C13 1.920(9) . ? Os1 C11 1.955(10) . ? Os1 C101 2.172(9) . ? Os1 Sb7 2.6470(6) . ? Os1 Os2 2.9360(4) . ? Os2 C22 1.870(10) . ? Os2 C21 1.871(10) . ? Os2 C102 2.222(8) . ? Os2 C101 2.340(8) . ? Os2 Sb6 2.5577(6) . ? Os2 Os3 2.9537(5) . ? Os3 C33 1.924(9) . ? Os3 C31 1.926(10) . ? Os3 C32 1.928(10) . ? Os3 C102 2.277(8) . ? Os3 Sb7 2.6751(6) . ? Os3 Sb6 2.8199(6) . ? Os4 C41 1.916(11) . ? Os4 C43 1.931(10) . ? Os4 C42 1.976(11) . ? Os4 C201 2.156(9) . ? Os4 Sb6 2.6527(6) . ? Os4 Os5 3.0305(5) . ? Os5 C51 1.905(12) . ? Os5 C53 1.939(10) . ? Os5 C52 1.950(12) . ? Os5 C202 2.148(9) . ? Os5 Sb6 2.6563(6) . ? Sb7 C711 2.131(8) . ? Sb7 C721 2.144(8) . ? O11 C11 1.114(12) . ? O12 C12 1.153(12) . ? O13 C13 1.141(12) . ? O21 C21 1.151(12) . ? O22 C22 1.150(12) . ? O31 C31 1.137(12) . ? O32 C32 1.126(12) . ? O33 C33 1.127(11) . ? O41 C41 1.122(13) . ? O42 C42 1.106(12) . ? O43 C43 1.122(12) . ? O51 C51 1.129(13) . ? O52 C52 1.135(14) . ? O53 C53 1.128(12) . ? C101 C106 1.440(11) . ? C101 C102 1.450(13) . ? C102 C103 1.434(13) . ? C103 C104 1.366(14) . ? C104 C105 1.407(16) . ? C105 C106 1.367(15) . ? C201 C206 1.373(14) . ? C201 C202 1.414(12) . ? C202 C203 1.395(12) . ? C203 C204 1.373(16) . ? C204 C205 1.363(17) . ? C205 C206 1.425(16) . ? C711 C712 1.378(12) . ? C711 C716 1.382(12) . ? C712 C713 1.379(14) . ? C713 C714 1.369(16) . ? C714 C715 1.380(18) . ? C715 C716 1.385(16) . ? C721 C726 1.380(13) . ? C721 C722 1.383(13) . ? C722 C723 1.369(14) . ? C723 C724 1.403(15) . ? C724 C725 1.368(16) . ? C725 C726 1.406(15) . ? C10 Cl11 1.646(17) . ? C10 Cl12 1.673(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 C12 Os1 C13 92.4(4) . . ? C12 Os1 C11 93.9(4) . . ? C13 Os1 C11 93.4(4) . . ? C12 Os1 C101 91.7(4) . . ? C13 Os1 C101 94.9(4) . . ? C11 Os1 C101 169.8(3) . . ? C12 Os1 Sb7 172.9(3) . . ? C13 Os1 Sb7 92.4(3) . . ? C11 Os1 Sb7 91.1(3) . . ? C101 Os1 Sb7 82.7(2) . . ? C12 Os1 Os2 87.3(3) . . ? C13 Os1 Os2 146.8(3) . . ? C11 Os1 Os2 119.8(3) . . ? C101 Os1 Os2 52.0(2) . . ? Sb7 Os1 Os2 85.768(16) . . ? C22 Os2 C21 88.1(4) . . ? C22 Os2 C102 89.5(4) . . ? C21 Os2 C102 146.0(4) . . ? C22 Os2 C101 111.6(4) . . ? C21 Os2 C101 114.6(4) . . ? C102 Os2 C101 36.9(3) . . ? C22 Os2 Sb6 93.5(3) . . ? C21 Os2 Sb6 103.5(3) . . ? C102 Os2 Sb6 110.6(2) . . ? C101 Os2 Sb6 134.2(2) . . ? C22 Os2 Os1 156.7(3) . . ? C21 Os2 Os1 93.8(3) . . ? C102 Os2 Os1 76.1(2) . . ? C101 Os2 Os1 47.0(2) . . ? Sb6 Os2 Os1 108.596(17) . . ? C22 Os2 Os3 96.8(3) . . ? C21 Os2 Os3 163.9(3) . . ? C102 Os2 Os3 49.8(2) . . ? C101 Os2 Os3 77.9(2) . . ? Sb6 Os2 Os3 61.048(15) . . ? Os1 Os2 Os3 87.734(12) . . ? C33 Os3 C31 95.4(4) . . ? C33 Os3 C32 96.2(4) . . ? C31 Os3 C32 93.0(4) . . ? C33 Os3 C102 172.3(4) . . ? C31 Os3 C102 92.3(4) . . ? C32 Os3 C102 82.7(3) . . ? C33 Os3 Sb7 91.6(3) . . ? C31 Os3 Sb7 173.0(3) . . ? C32 Os3 Sb7 86.3(3) . . ? C102 Os3 Sb7 80.7(2) . . ? C33 Os3 Sb6 81.2(3) . . ? C31 Os3 Sb6 82.9(3) . . ? C32 Os3 Sb6 174.9(3) . . ? C102 Os3 Sb6 100.5(2) . . ? Sb7 Os3 Sb6 98.090(19) . . ? C33 Os3 Os2 132.2(3) . . ? C31 Os3 Os2 90.3(3) . . ? C32 Os3 Os2 130.9(3) . . ? C102 Os3 Os2 48.2(2) . . ? Sb7 Os3 Os2 84.915(16) . . ? Sb6 Os3 Os2 52.527(14) . . ? C41 Os4 C43 96.7(5) . . ? C41 Os4 C42 95.7(4) . . ? C43 Os4 C42 95.8(4) . . ? C41 Os4 C201 91.6(4) . . ? C43 Os4 C201 85.7(4) . . ? C42 Os4 C201 172.4(4) . . ? C41 Os4 Sb6 96.8(3) . . ? C43 Os4 Sb6 158.2(3) . . ? C42 Os4 Sb6 99.7(3) . . ? C201 Os4 Sb6 76.9(2) . . ? C41 Os4 Os5 147.6(3) . . ? C43 Os4 Os5 106.0(3) . . ? C42 Os4 Os5 104.4(3) . . ? C201 Os4 Os5 68.0(2) . . ? Sb6 Os4 Os5 55.249(14) . . ? C51 Os5 C53 96.1(5) . . ? C51 Os5 C52 93.7(5) . . ? C53 Os5 C52 97.4(4) . . ? C51 Os5 C202 90.1(4) . . ? C53 Os5 C202 89.8(4) . . ? C52 Os5 C202 171.5(4) . . ? C51 Os5 Sb6 100.1(3) . . ? C53 Os5 Sb6 159.0(3) . . ? C52 Os5 Sb6 94.7(3) . . ? C202 Os5 Sb6 77.1(2) . . ? C51 Os5 Os4 149.0(3) . . ? C53 Os5 Os4 104.9(3) . . ? C52 Os5 Os4 105.7(3) . . ? C202 Os5 Os4 67.8(2) . . ? Sb6 Os5 Os4 55.136(14) . . ? Os2 Sb6 Os4 137.45(3) . . ? Os2 Sb6 Os5 131.25(2) . . ? Os4 Sb6 Os5 69.615(16) . . ? Os2 Sb6 Os3 66.425(15) . . ? Os4 Sb6 Os3 137.71(2) . . ? Os5 Sb6 Os3 126.27(2) . . ? C711 Sb7 C721 100.9(3) . . ? C711 Sb7 Os1 115.1(2) . . ? C721 Sb7 Os1 110.9(2) . . ? C711 Sb7 Os3 120.3(2) . . ? C721 Sb7 Os3 109.7(2) . . ? Os1 Sb7 Os3 100.15(2) . . ? O11 C11 Os1 177.6(10) . . ? O12 C12 Os1 178.1(10) . . ? O13 C13 Os1 178.8(11) . . ? O21 C21 Os2 178.5(9) . . ? O22 C22 Os2 179.9(12) . . ? O31 C31 Os3 178.3(11) . . ? O32 C32 Os3 176.0(9) . . ? O33 C33 Os3 178.3(10) . . ? O41 C41 Os4 178.3(12) . . ? O42 C42 Os4 175.0(10) . . ? O43 C43 Os4 176.3(9) . . ? O51 C51 Os5 177.8(10) . . ? O52 C52 Os5 175.1(10) . . ? O53 C53 Os5 177.5(10) . . ? C106 C101 C102 117.2(8) . . ? C106 C101 Os1 117.9(7) . . ? C102 C101 Os1 124.8(6) . . ? C106 C101 Os2 129.1(6) . . ? C102 C101 Os2 67.1(4) . . ? Os1 C101 Os2 81.1(3) . . ? C103 C102 C101 117.5(7) . . ? C103 C102 Os2 126.0(6) . . ? C101 C102 Os2 76.0(5) . . ? C103 C102 Os3 114.1(7) . . ? C101 C102 Os3 127.4(6) . . ? Os2 C102 Os3 82.1(3) . . ? C104 C103 C102 122.7(10) . . ? C103 C104 C105 120.0(10) . . ? C106 C105 C104 119.9(9) . . ? C105 C106 C101 122.6(9) . . ? C206 C201 C202 120.4(9) . . ? C206 C201 Os4 128.1(7) . . ? C202 C201 Os4 111.5(6) . . ? C203 C202 C201 118.2(9) . . ? C203 C202 Os5 129.2(8) . . ? C201 C202 Os5 112.6(6) . . ? C204 C203 C202 121.5(10) . . ? C205 C204 C203 120.4(10) . . ? C204 C205 C206 119.9(10) . . ? C201 C206 C205 119.6(11) . . ? C712 C711 C716 118.4(8) . . ? C712 C711 Sb7 121.1(6) . . ? C716 C711 Sb7 120.4(7) . . ? C711 C712 C713 121.7(9) . . ? C714 C713 C712 119.5(10) . . ? C713 C714 C715 119.7(10) . . ? C714 C715 C716 120.5(10) . . ? C711 C716 C715 120.0(10) . . ? C726 C721 C722 119.1(8) . . ? C726 C721 Sb7 118.7(7) . . ? C722 C721 Sb7 122.1(6) . . ? C723 C722 C721 121.3(9) . . ? C722 C723 C724 119.7(10) . . ? C725 C724 C723 119.6(10) . . ? C724 C725 C726 120.2(11) . . ? C721 C726 C725 120.0(10) . . ? Cl11 C10 Cl12 120.0(17) . . ? _diffrn_measured_fraction_theta_max 0.864 _diffrn_reflns_theta_full 29.35 _diffrn_measured_fraction_theta_full 0.864 _refine_diff_density_max 1.392 _refine_diff_density_min -1.829 _refine_diff_density_rms 0.255 #END #========================== # Compound 4 = #========================== data_4 _database_code_CSD 171669 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H22 Cl2 O14 Os5 Sb2' _chemical_formula_weight 1979.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.3478(7) _cell_length_b 21.7070(9) _cell_length_c 23.1622(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9224.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7601 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 25.32 _exptl_crystal_description 'Plate' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7072 _exptl_absorpt_coefficient_mu 15.047 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.186666 _exptl_absorpt_correction_T_max 0.357583 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 72060 _diffrn_reflns_av_R_equivalents 0.0944 _diffrn_reflns_av_sigmaI/netI 0.0923 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 29.98 _reflns_number_total 12701 _reflns_number_gt 7454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12701 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 0.889 _refine_ls_restrained_S_all 0.889 _refine_ls_shift/su_max 0.243 _refine_ls_shift/su_mean 0.009 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 0.90210(2) 0.218094(19) 0.728047(19) 0.04252(11) Uani 1 1 d . . . Os2 Os 1.02451(2) 0.326151(18) 0.846161(18) 0.03723(10) Uani 1 1 d . . . Os3 Os 0.90077(2) 0.162128(19) 0.92684(2) 0.04398(12) Uani 1 1 d . . . Os4 Os 1.04314(2) 0.117400(19) 0.87906(2) 0.04428(12) Uani 1 1 d . . . H34 H 0.9589 0.0940 0.9164 0.050 Uiso 1 1 d R . . Os5 Os 1.06843(2) 0.291962(19) 0.961665(19) 0.04219(11) Uani 1 1 d . . . Sb6 Sb 0.96718(3) 0.21068(3) 0.83364(3) 0.03770(16) Uani 1 1 d . . . Sb7 Sb 0.96819(3) 0.32871(3) 0.74098(3) 0.03719(16) Uani 1 1 d . . . O11 O 0.7737(4) 0.2717(4) 0.7962(4) 0.071(3) Uani 1 1 d . . . O12 O 0.8407(4) 0.2415(4) 0.6087(4) 0.068(2) Uani 1 1 d . . . O14 O 0.8466(5) 0.0873(4) 0.7346(5) 0.102(3) Uani 1 1 d . . . O21 O 0.8754(4) 0.3660(4) 0.8933(4) 0.074(3) Uani 1 1 d . . . O22 O 1.0806(4) 0.4583(4) 0.8439(4) 0.071(2) Uani 1 1 d . . . O23 O 1.1748(4) 0.2740(3) 0.8135(4) 0.062(2) Uani 1 1 d . . . O31 O 0.7977(4) 0.2685(4) 0.9464(5) 0.092(3) Uani 1 1 d . . . O32 O 0.8591(4) 0.1077(4) 1.0429(4) 0.070(2) Uani 1 1 d . . . O33 O 0.7948(5) 0.0846(5) 0.8542(4) 0.097(3) Uani 1 1 d . . . O41 O 1.1863(4) 0.1419(4) 0.8172(4) 0.074(3) Uani 1 1 d . . . O42 O 1.1095(5) 0.0196(4) 0.9559(4) 0.089(3) Uani 1 1 d . . . O43 O 0.9833(5) 0.0315(4) 0.7849(4) 0.086(3) Uani 1 1 d . . . O51 O 1.0039(6) 0.4172(4) 0.9833(4) 0.101(3) Uani 1 1 d . . . O52 O 1.2085(5) 0.3541(5) 0.9300(4) 0.111(4) Uani 1 1 d . . . C11 C 0.8215(6) 0.2532(5) 0.7696(5) 0.052(3) Uani 1 1 d . . . C12 C 0.8634(6) 0.2336(5) 0.6530(6) 0.051(3) Uani 1 1 d . . . C14 C 0.8675(6) 0.1368(6) 0.7318(5) 0.063(3) Uani 1 1 d . . . C21 C 0.9311(6) 0.3502(5) 0.8757(5) 0.052(3) Uani 1 1 d . . . C22 C 1.0599(6) 0.4085(5) 0.8446(4) 0.046(3) Uani 1 1 d . . . C23 C 1.1186(6) 0.2924(4) 0.8241(4) 0.045(3) Uani 1 1 d . . . C31 C 0.8363(6) 0.2290(5) 0.9389(5) 0.059(3) Uani 1 1 d . . . C32 C 0.8755(6) 0.1246(5) 0.9989(6) 0.054(3) Uani 1 1 d . . . C33 C 0.8328(6) 0.1130(6) 0.8810(6) 0.062(3) Uani 1 1 d . . . C41 C 1.1322(7) 0.1345(5) 0.8405(5) 0.059(3) Uani 1 1 d . . . C42 C 1.0833(6) 0.0556(5) 0.9265(5) 0.060(3) Uani 1 1 d . . . C43 C 1.0067(7) 0.0620(5) 0.8202(5) 0.059(3) Uani 1 1 d . . . C51 C 1.0285(8) 0.3706(6) 0.9737(5) 0.070(4) Uani 1 1 d . . . C52 C 1.1549(7) 0.3314(6) 0.9408(5) 0.071(4) Uani 1 1 d . . . C131 C 0.9961(5) 0.1771(4) 0.6882(4) 0.044(3) Uani 1 1 d . . . C132 C 0.9892(6) 0.1277(5) 0.6498(5) 0.060(3) Uani 1 1 d . . . H132 H 0.9419 0.1136 0.6415 0.072 Uiso 1 1 calc R . . C133 C 1.0474(7) 0.0981(5) 0.6228(5) 0.069(4) Uani 1 1 d . . . H133 H 1.0390 0.0658 0.5966 0.083 Uiso 1 1 calc R . . C134 C 1.1170(6) 0.1166(6) 0.6350(5) 0.065(3) Uani 1 1 d . . . H134 H 1.1569 0.0974 0.6170 0.078 Uiso 1 1 calc R . . C135 C 1.1282(6) 0.1640(5) 0.6742(5) 0.061(3) Uani 1 1 d . . . H135 H 1.1757 0.1765 0.6836 0.073 Uiso 1 1 calc R . . C136 C 1.0682(5) 0.1931(5) 0.6995(4) 0.049(3) Uani 1 1 d . . . H136 H 1.0771 0.2253 0.7257 0.058 Uiso 1 1 calc R . . C711 C 1.0394(5) 0.3639(4) 0.6771(5) 0.042(2) Uani 1 1 d . . . C712 C 1.0124(6) 0.3902(5) 0.6286(5) 0.062(3) Uani 1 1 d . . . H712 H 0.9617 0.3897 0.6228 0.074 Uiso 1 1 calc R . . C713 C 1.0556(7) 0.4175(6) 0.5873(5) 0.075(4) Uani 1 1 d . . . H713 H 1.0346 0.4357 0.5545 0.090 Uiso 1 1 calc R . . C714 C 1.1283(8) 0.4179(6) 0.5946(6) 0.076(4) Uani 1 1 d . . . H714 H 1.1582 0.4369 0.5669 0.092 Uiso 1 1 calc R . . C715 C 1.1580(7) 0.3915(7) 0.6405(7) 0.105(6) Uani 1 1 d . . . H715 H 1.2089 0.3911 0.6449 0.127 Uiso 1 1 calc R . . C716 C 1.1142(6) 0.3644(6) 0.6820(6) 0.077(4) Uani 1 1 d . . . H716 H 1.1360 0.3460 0.7143 0.093 Uiso 1 1 calc R . . C721 C 0.8855(5) 0.3961(5) 0.7335(5) 0.044(3) Uani 1 1 d . . . C722 C 0.8855(6) 0.4500(5) 0.7661(5) 0.061(3) Uani 1 1 d . . . H722 H 0.9229 0.4564 0.7933 0.073 Uiso 1 1 calc R . . C723 C 0.8316(7) 0.4949(6) 0.7596(6) 0.085(4) Uani 1 1 d . . . H723 H 0.8327 0.5312 0.7817 0.102 Uiso 1 1 calc R . . C724 C 0.7788(8) 0.4851(7) 0.7215(8) 0.105(6) Uani 1 1 d . . . H724 H 0.7422 0.5150 0.7170 0.126 Uiso 1 1 calc R . . C725 C 0.7762(7) 0.4344(7) 0.6896(7) 0.094(5) Uani 1 1 d . . . H725 H 0.7385 0.4288 0.6626 0.113 Uiso 1 1 calc R . . C726 C 0.8300(6) 0.3895(5) 0.6967(5) 0.067(3) Uani 1 1 d . . . H726 H 0.8270 0.3532 0.6746 0.080 Uiso 1 1 calc R . . C1 C 0.9901(6) 0.2031(4) 0.9694(5) 0.045(3) Uani 1 1 d . . . C2 C 1.0593(5) 0.1807(4) 0.9470(4) 0.038(2) Uani 1 1 d . . . C3 C 1.1230(5) 0.1978(5) 0.9767(5) 0.054(3) Uani 1 1 d . . . H3 H 1.1685 0.1864 0.9615 0.065 Uiso 1 1 calc R . . C4 C 1.1206(6) 0.2313(5) 1.0284(5) 0.053(3) Uani 1 1 d . . . H4 H 1.1640 0.2394 1.0486 0.064 Uiso 1 1 calc R . . C5 C 1.0540(6) 0.2526(5) 1.0501(5) 0.055(3) Uani 1 1 d . . . H5 H 1.0524 0.2758 1.0843 0.065 Uiso 1 1 calc R . . C6 C 0.9900(6) 0.2389(5) 1.0199(5) 0.050(3) Uani 1 1 d . . . H6 H 0.9454 0.2542 1.0339 0.060 Uiso 1 1 calc R . . C10 C 0.8223(11) 0.0250(10) 0.5394(8) 0.184(11) Uani 1 1 d . . . H10A H 0.8014 -0.0028 0.5683 0.221 Uiso 1 1 calc R . . H10B H 0.8754 0.0226 0.5438 0.221 Uiso 1 1 calc R . . Cl1 Cl 0.7992(3) 0.0932(3) 0.5577(3) 0.177(3) Uani 1 1 d . . . Cl2 Cl 0.8033(3) -0.0042(3) 0.4767(3) 0.175(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0346(2) 0.0406(2) 0.0524(3) -0.00664(19) -0.0075(2) -0.00323(18) Os2 0.0342(2) 0.0351(2) 0.0425(2) -0.00332(18) -0.00184(19) -0.00368(17) Os3 0.0303(2) 0.0413(2) 0.0603(3) 0.0030(2) 0.0027(2) -0.00230(18) Os4 0.0368(2) 0.0366(2) 0.0595(3) -0.0033(2) -0.0002(2) 0.00550(18) Os5 0.0399(2) 0.0432(3) 0.0435(3) -0.00316(19) -0.0040(2) -0.00261(19) Sb6 0.0307(3) 0.0344(4) 0.0480(4) -0.0023(3) -0.0022(3) -0.0019(3) Sb7 0.0319(3) 0.0363(4) 0.0433(4) -0.0035(3) -0.0014(3) 0.0008(3) O11 0.039(4) 0.095(7) 0.080(7) -0.006(5) 0.003(4) 0.005(4) O12 0.060(5) 0.091(7) 0.052(6) -0.016(5) -0.014(5) 0.018(5) O14 0.095(7) 0.063(7) 0.149(10) -0.011(6) -0.023(6) -0.036(5) O21 0.068(5) 0.068(6) 0.088(7) -0.007(5) 0.032(5) 0.013(5) O22 0.075(6) 0.048(5) 0.089(7) 0.000(4) -0.009(5) -0.024(4) O23 0.038(4) 0.064(5) 0.084(6) -0.003(4) 0.008(4) 0.008(4) O31 0.055(5) 0.059(6) 0.161(10) 0.017(6) 0.026(6) 0.017(4) O32 0.064(5) 0.069(6) 0.076(7) 0.013(5) 0.018(5) -0.004(4) O33 0.064(6) 0.118(9) 0.110(9) -0.017(6) -0.005(6) -0.040(6) O41 0.051(5) 0.071(6) 0.100(7) -0.003(5) 0.023(5) 0.007(4) O42 0.118(8) 0.060(6) 0.088(7) -0.001(5) -0.026(6) 0.026(5) O43 0.092(7) 0.064(6) 0.103(8) -0.032(5) -0.025(6) 0.007(5) O51 0.179(10) 0.053(6) 0.071(7) -0.015(5) -0.024(6) 0.038(7) O52 0.071(6) 0.155(10) 0.107(8) 0.025(7) -0.013(6) -0.075(7) C11 0.034(6) 0.062(8) 0.060(8) 0.009(6) -0.019(6) -0.018(5) C12 0.041(6) 0.047(7) 0.066(9) -0.010(6) -0.005(6) 0.003(5) C14 0.059(7) 0.075(9) 0.055(8) -0.016(7) -0.011(6) -0.026(7) C21 0.065(7) 0.029(6) 0.061(8) -0.005(5) -0.005(7) -0.001(5) C22 0.054(7) 0.050(7) 0.034(6) -0.002(5) -0.003(5) -0.004(5) C23 0.050(6) 0.037(6) 0.047(7) 0.003(5) 0.002(6) -0.001(5) C31 0.034(6) 0.054(8) 0.088(10) 0.004(7) 0.013(6) -0.006(5) C32 0.041(6) 0.042(7) 0.077(10) 0.010(6) 0.001(6) -0.004(5) C33 0.037(6) 0.065(9) 0.083(10) 0.011(7) 0.001(7) -0.005(6) C41 0.063(8) 0.044(7) 0.070(9) -0.026(6) -0.011(7) 0.014(6) C42 0.070(8) 0.045(7) 0.065(9) 0.002(6) -0.011(7) 0.008(6) C43 0.077(8) 0.047(7) 0.051(8) -0.005(6) -0.006(7) 0.008(6) C51 0.116(11) 0.050(8) 0.045(8) -0.011(6) -0.017(7) 0.012(8) C52 0.059(8) 0.100(11) 0.053(9) -0.002(7) -0.015(7) -0.019(8) C131 0.047(6) 0.036(6) 0.049(7) 0.001(5) -0.005(5) 0.001(5) C132 0.057(7) 0.048(7) 0.075(9) -0.003(6) -0.023(7) -0.002(6) C133 0.090(10) 0.054(8) 0.062(9) -0.023(6) -0.023(8) 0.021(7) C134 0.062(8) 0.082(10) 0.052(8) -0.004(7) -0.009(7) 0.030(7) C135 0.050(7) 0.072(9) 0.061(9) -0.011(7) -0.004(6) 0.014(6) C136 0.050(6) 0.056(7) 0.040(7) -0.010(5) -0.003(6) -0.002(5) C711 0.047(6) 0.030(5) 0.051(7) -0.006(5) 0.007(5) -0.002(4) C712 0.043(6) 0.078(9) 0.063(9) 0.001(7) 0.008(6) -0.001(6) C713 0.077(10) 0.098(11) 0.052(9) 0.014(7) 0.004(8) 0.007(8) C714 0.081(10) 0.081(10) 0.067(10) 0.030(8) 0.018(8) -0.003(8) C715 0.037(7) 0.151(16) 0.128(15) 0.047(12) 0.018(9) -0.016(8) C716 0.052(8) 0.115(12) 0.065(9) 0.038(8) -0.006(7) -0.016(7) C721 0.041(6) 0.041(6) 0.049(7) -0.003(5) 0.003(5) 0.009(5) C722 0.060(7) 0.046(7) 0.077(9) -0.003(6) -0.005(7) 0.002(6) C723 0.082(10) 0.060(9) 0.114(13) -0.020(8) -0.010(9) 0.034(8) C724 0.073(10) 0.068(11) 0.175(18) -0.027(11) -0.008(11) 0.044(8) C725 0.056(8) 0.084(11) 0.142(15) -0.012(10) -0.031(9) 0.024(8) C726 0.063(8) 0.056(8) 0.082(10) -0.005(7) -0.014(7) 0.011(6) C1 0.049(6) 0.034(6) 0.053(7) 0.008(5) 0.001(6) 0.000(5) C2 0.032(5) 0.041(6) 0.040(6) 0.008(4) -0.001(5) 0.007(4) C3 0.033(6) 0.048(7) 0.080(9) 0.006(6) -0.005(6) 0.009(5) C4 0.055(7) 0.053(7) 0.053(8) 0.004(6) -0.020(6) -0.008(6) C5 0.064(8) 0.061(8) 0.039(7) -0.001(5) 0.002(6) -0.009(6) C6 0.041(6) 0.063(8) 0.047(7) 0.010(6) 0.000(5) -0.011(5) C10 0.22(2) 0.19(2) 0.141(19) -0.057(16) -0.087(17) 0.108(19) Cl1 0.143(4) 0.154(5) 0.233(7) -0.094(5) -0.062(4) 0.056(4) Cl2 0.173(5) 0.163(6) 0.190(6) -0.065(5) -0.021(5) 0.041(4) _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 C14 1.877(13) . ? Os1 C12 1.907(13) . ? Os1 C11 1.923(13) . ? Os1 C131 2.150(10) . ? Os1 Sb7 2.7066(8) . ? Os1 Sb6 2.7265(8) . ? Os2 C22 1.903(11) . ? Os2 C21 1.918(12) . ? Os2 C23 1.944(11) . ? Os2 Sb7 2.6469(8) . ? Os2 Sb6 2.7338(7) . ? Os2 Os5 2.8910(6) . ? Os3 C31 1.894(12) . ? Os3 C32 1.915(13) . ? Os3 C33 1.955(13) . ? Os3 C1 2.110(11) . ? Os3 Sb6 2.6935(8) . ? Os3 Os4 2.9985(6) . ? Os4 C42 1.885(12) . ? Os4 C41 1.899(13) . ? Os4 C43 1.937(12) . ? Os4 C2 2.110(10) . ? Os4 Sb6 2.6738(8) . ? Os5 C52 1.867(13) . ? Os5 C51 1.879(13) . ? Os5 C5 2.234(11) . ? Os5 C4 2.245(10) . ? Os5 C6 2.285(10) . ? Os5 C3 2.303(10) . ? Os5 C1 2.412(10) . ? Os5 C2 2.444(10) . ? Sb7 C721 2.114(9) . ? Sb7 C711 2.117(10) . ? O11 C11 1.143(12) . ? O12 C12 1.121(12) . ? O14 C14 1.144(13) . ? O21 C21 1.153(12) . ? O22 C22 1.146(11) . ? O23 C23 1.133(11) . ? O31 C31 1.126(12) . ? O32 C32 1.122(12) . ? O33 C33 1.118(13) . ? O41 C41 1.141(12) . ? O42 C42 1.141(12) . ? O43 C43 1.136(12) . ? O51 C51 1.131(13) . ? O52 C52 1.128(13) . ? C131 C136 1.392(13) . ? C131 C132 1.399(14) . ? C132 C133 1.396(15) . ? C133 C134 1.367(15) . ? C134 C135 1.387(15) . ? C135 C136 1.397(13) . ? C711 C712 1.352(14) . ? C711 C716 1.377(14) . ? C712 C713 1.377(15) . ? C713 C714 1.344(16) . ? C714 C715 1.325(17) . ? C715 C716 1.383(16) . ? C721 C726 1.335(14) . ? C721 C722 1.395(14) . ? C722 C723 1.395(15) . ? C723 C724 1.328(18) . ? C724 C725 1.327(17) . ? C725 C726 1.397(15) . ? C1 C6 1.405(14) . ? C1 C2 1.454(13) . ? C2 C3 1.406(13) . ? C3 C4 1.400(14) . ? C4 C5 1.400(14) . ? C5 C6 1.399(14) . ? C10 Cl1 1.598(18) . ? C10 Cl2 1.622(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 C14 Os1 C12 94.7(5) . . ? C14 Os1 C11 95.1(5) . . ? C12 Os1 C11 95.7(4) . . ? C14 Os1 C131 84.4(4) . . ? C12 Os1 C131 88.9(4) . . ? C11 Os1 C131 175.4(4) . . ? C14 Os1 Sb7 168.6(4) . . ? C12 Os1 Sb7 96.4(3) . . ? C11 Os1 Sb7 86.4(3) . . ? C131 Os1 Sb7 93.2(3) . . ? C14 Os1 Sb6 92.9(4) . . ? C12 Os1 Sb6 172.3(3) . . ? C11 Os1 Sb6 84.9(3) . . ? C131 Os1 Sb6 90.5(3) . . ? Sb7 Os1 Sb6 75.93(2) . . ? C22 Os2 C21 93.2(4) . . ? C22 Os2 C23 92.7(4) . . ? C21 Os2 C23 171.9(4) . . ? C22 Os2 Sb7 95.5(3) . . ? C21 Os2 Sb7 88.5(3) . . ? C23 Os2 Sb7 96.5(3) . . ? C22 Os2 Sb6 172.3(3) . . ? C21 Os2 Sb6 86.8(3) . . ? C23 Os2 Sb6 88.2(3) . . ? Sb7 Os2 Sb6 76.79(2) . . ? C22 Os2 Os5 99.4(3) . . ? C21 Os2 Os5 89.4(3) . . ? C23 Os2 Os5 84.2(3) . . ? Sb7 Os2 Os5 165.01(2) . . ? Sb6 Os2 Os5 88.28(2) . . ? C31 Os3 C32 92.6(5) . . ? C31 Os3 C33 95.7(5) . . ? C32 Os3 C33 95.0(5) . . ? C31 Os3 C1 95.3(4) . . ? C32 Os3 C1 87.7(4) . . ? C33 Os3 C1 168.5(4) . . ? C31 Os3 Sb6 95.8(3) . . ? C32 Os3 Sb6 167.1(3) . . ? C33 Os3 Sb6 93.8(3) . . ? C1 Os3 Sb6 81.9(3) . . ? C31 Os3 Os4 147.9(3) . . ? C32 Os3 Os4 113.3(3) . . ? C33 Os3 Os4 100.3(3) . . ? C1 Os3 Os4 68.4(3) . . ? Sb6 Os3 Os4 55.725(17) . . ? C42 Os4 C41 94.4(5) . . ? C42 Os4 C43 96.0(5) . . ? C41 Os4 C43 95.1(5) . . ? C42 Os4 C2 88.5(4) . . ? C41 Os4 C2 95.9(4) . . ? C43 Os4 C2 167.9(4) . . ? C42 Os4 Sb6 166.5(4) . . ? C41 Os4 Sb6 96.6(3) . . ? C43 Os4 Sb6 90.8(3) . . ? C2 Os4 Sb6 82.7(2) . . ? C42 Os4 Os3 110.9(4) . . ? C41 Os4 Os3 149.3(3) . . ? C43 Os4 Os3 99.2(3) . . ? C2 Os4 Os3 68.7(2) . . ? Sb6 Os4 Os3 56.350(18) . . ? C52 Os5 C51 87.3(6) . . ? C52 Os5 C5 120.9(5) . . ? C51 Os5 C5 99.5(5) . . ? C52 Os5 C4 94.9(5) . . ? C51 Os5 C4 126.7(5) . . ? C5 Os5 C4 36.4(4) . . ? C52 Os5 C6 156.9(4) . . ? C51 Os5 C6 97.2(5) . . ? C5 Os5 C6 36.1(3) . . ? C4 Os5 C6 64.3(4) . . ? C52 Os5 C3 94.4(5) . . ? C51 Os5 C3 162.5(5) . . ? C5 Os5 C3 64.7(4) . . ? C4 Os5 C3 35.8(4) . . ? C6 Os5 C3 74.7(4) . . ? C52 Os5 C1 153.2(5) . . ? C51 Os5 C1 118.9(5) . . ? C5 Os5 C1 63.6(4) . . ? C4 Os5 C1 74.5(4) . . ? C6 Os5 C1 34.7(3) . . ? C3 Os5 C1 62.4(3) . . ? C52 Os5 C2 118.4(5) . . ? C51 Os5 C2 153.1(5) . . ? C5 Os5 C2 75.0(4) . . ? C4 Os5 C2 62.9(3) . . ? C6 Os5 C2 62.7(4) . . ? C3 Os5 C2 34.3(3) . . ? C1 Os5 C2 34.8(3) . . ? C52 Os5 Os2 83.1(4) . . ? C51 Os5 Os2 78.2(3) . . ? C5 Os5 Os2 156.0(3) . . ? C4 Os5 Os2 155.0(3) . . ? C6 Os5 Os2 120.0(3) . . ? C3 Os5 Os2 119.3(3) . . ? C1 Os5 Os2 96.2(3) . . ? C2 Os5 Os2 96.1(2) . . ? Os4 Sb6 Os3 67.93(2) . . ? Os4 Sb6 Os1 128.75(3) . . ? Os3 Sb6 Os1 122.95(3) . . ? Os4 Sb6 Os2 116.88(3) . . ? Os3 Sb6 Os2 116.60(3) . . ? Os1 Sb6 Os2 102.09(2) . . ? C721 Sb7 C711 97.8(4) . . ? C721 Sb7 Os2 111.7(3) . . ? C711 Sb7 Os2 114.2(3) . . ? C721 Sb7 Os1 106.4(3) . . ? C711 Sb7 Os1 121.3(3) . . ? Os2 Sb7 Os1 104.96(3) . . ? O11 C11 Os1 176.6(10) . . ? O12 C12 Os1 178.7(10) . . ? O14 C14 Os1 179.4(12) . . ? O21 C21 Os2 178.6(10) . . ? O22 C22 Os2 179.4(11) . . ? O23 C23 Os2 176.8(10) . . ? O31 C31 Os3 179.4(12) . . ? O32 C32 Os3 173.9(11) . . ? O33 C33 Os3 178.9(12) . . ? O41 C41 Os4 176.7(10) . . ? O42 C42 Os4 177.6(12) . . ? O43 C43 Os4 177.0(11) . . ? O51 C51 Os5 177.0(12) . . ? O52 C52 Os5 177.2(12) . . ? C136 C131 C132 113.4(9) . . ? C136 C131 Os1 125.3(8) . . ? C132 C131 Os1 121.1(8) . . ? C133 C132 C131 124.6(10) . . ? C134 C133 C132 119.1(11) . . ? C133 C134 C135 119.4(11) . . ? C134 C135 C136 119.6(11) . . ? C131 C136 C135 123.8(10) . . ? C712 C711 C716 115.5(10) . . ? C712 C711 Sb7 120.4(8) . . ? C716 C711 Sb7 124.1(9) . . ? C711 C712 C713 123.1(11) . . ? C714 C713 C712 119.2(12) . . ? C715 C714 C713 120.4(12) . . ? C714 C715 C716 120.2(12) . . ? C711 C716 C715 121.6(12) . . ? C726 C721 C722 115.9(10) . . ? C726 C721 Sb7 121.7(8) . . ? C722 C721 Sb7 122.4(8) . . ? C721 C722 C723 121.8(11) . . ? C724 C723 C722 118.6(12) . . ? C725 C724 C723 121.9(13) . . ? C724 C725 C726 119.2(13) . . ? C721 C726 C725 122.6(12) . . ? C6 C1 C2 119.0(9) . . ? C6 C1 Os3 128.4(8) . . ? C2 C1 Os3 111.7(7) . . ? C6 C1 Os5 67.7(6) . . ? C2 C1 Os5 73.8(6) . . ? Os3 C1 Os5 139.9(5) . . ? C3 C2 C1 117.5(9) . . ? C3 C2 Os4 130.8(7) . . ? C1 C2 Os4 111.2(7) . . ? C3 C2 Os5 67.3(6) . . ? C1 C2 Os5 71.4(5) . . ? Os4 C2 Os5 139.2(4) . . ? C4 C3 C2 122.0(10) . . ? C4 C3 Os5 69.8(6) . . ? C2 C3 Os5 78.4(6) . . ? C5 C4 C3 120.4(10) . . ? C5 C4 Os5 71.4(6) . . ? C3 C4 Os5 74.3(6) . . ? C4 C5 C6 118.9(10) . . ? C4 C5 Os5 72.2(6) . . ? C6 C5 Os5 73.9(6) . . ? C5 C6 C1 122.1(10) . . ? C5 C6 Os5 70.0(6) . . ? C1 C6 Os5 77.6(6) . . ? Cl1 C10 Cl2 122.9(12) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 2.432 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.227 #END #========================== # Compound 6a = #========================== _database_code_CSD 171670 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H42 O13 Os5 P Sb2' _chemical_formula_weight 2172.39 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' '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 P21/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 15.3508(2) _cell_length_b 16.8332(3) _cell_length_c 24.73940(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.18 _cell_angle_gamma 90.00 _cell_volume 6355.59(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3964 _exptl_absorpt_coefficient_mu 10.873 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.576443 _exptl_absorpt_correction_T_max 0.694619 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 41516 _diffrn_reflns_av_R_equivalents 0.1256 _diffrn_reflns_av_sigmaI/netI 0.1719 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 29.41 _reflns_number_total 15878 _reflns_number_gt 8395 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0241P)^2^+41.0388P] 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 15878 _refine_ls_number_parameters 703 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1753 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_ref 0.1305 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.324 _refine_ls_shift/su_mean 0.006 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 -0.13753(4) 0.48525(4) 0.17487(2) 0.02234(15) Uani 1 1 d . . . Os2 Os -0.24842(4) 0.63115(4) 0.17126(2) 0.02358(15) Uani 1 1 d . . . H12 H -0.2446 0.5252 0.1816 0.050 Uiso 1 1 d R . . Os3 Os -0.15252(4) 0.67824(4) 0.27690(3) 0.02473(16) Uani 1 1 d . . . Os4 Os -0.42270(4) 0.52808(4) 0.31101(3) 0.02655(16) Uani 1 1 d . . . Os5 Os -0.45972(4) 0.70197(4) 0.29153(3) 0.02896(17) Uani 1 1 d . . . H45 H -0.4713 0.6172 0.3347 0.050 Uiso 1 1 d R . . Sb6 Sb -0.32476(7) 0.62507(6) 0.25852(4) 0.0241(2) Uani 1 1 d . . . Sb7 Sb -0.08497(7) 0.53269(6) 0.27491(4) 0.0253(3) Uani 1 1 d . . . P8 P -0.1892(3) 0.4421(3) 0.08375(17) 0.0272(10) Uani 1 1 d . . . O11 O -0.2001(8) 0.3228(7) 0.2107(5) 0.042(3) Uani 1 1 d . . . O12 O 0.0457(8) 0.4190(7) 0.1717(4) 0.042(3) Uani 1 1 d . . . O21 O -0.3960(9) 0.5941(7) 0.0846(6) 0.064(4) Uani 1 1 d . . . O22 O -0.3004(9) 0.8007(8) 0.1438(5) 0.058(4) Uani 1 1 d . . . O31 O -0.2366(9) 0.8444(7) 0.2694(5) 0.055(4) Uani 1 1 d . . . O32 O 0.0289(8) 0.7516(7) 0.3013(5) 0.049(3) Uani 1 1 d . . . O33 O -0.1806(8) 0.6624(9) 0.3962(5) 0.058(4) Uani 1 1 d . . . O41 O -0.2941(9) 0.5184(8) 0.4167(5) 0.059(4) Uani 1 1 d . . . O42 O -0.5800(9) 0.4658(8) 0.3637(5) 0.057(4) Uani 1 1 d . . . O43 O -0.3648(9) 0.3760(8) 0.2599(5) 0.057(4) Uani 1 1 d . . . O51 O -0.6402(8) 0.7316(8) 0.3289(6) 0.061(4) Uani 1 1 d . . . O52 O -0.4573(10) 0.8241(8) 0.2021(6) 0.069(5) Uani 1 1 d . . . O53 O -0.3465(10) 0.7947(9) 0.3798(6) 0.073(5) Uani 1 1 d . . . C11 C -0.1754(9) 0.3837(11) 0.1974(6) 0.027(4) Uani 1 1 d . . . C12 C -0.0241(11) 0.4439(9) 0.1707(6) 0.029(4) Uani 1 1 d . . . C21 C -0.3383(12) 0.6036(9) 0.1179(7) 0.034(4) Uani 1 1 d . . . C22 C -0.2806(11) 0.7364(11) 0.1556(6) 0.032(4) Uani 1 1 d . . . C31 C -0.2048(12) 0.7834(10) 0.2711(6) 0.035(4) Uani 1 1 d . . . C32 C -0.0364(11) 0.7231(10) 0.2908(6) 0.031(4) Uani 1 1 d . . . C33 C -0.1687(11) 0.6698(10) 0.3511(8) 0.037(4) Uani 1 1 d . . . C41 C -0.3377(11) 0.5235(10) 0.3767(7) 0.034(4) Uani 1 1 d . . . C42 C -0.5211(11) 0.4859(10) 0.3445(7) 0.032(4) Uani 1 1 d . . . C43 C -0.3866(10) 0.4304(9) 0.2800(7) 0.033(4) Uani 1 1 d . . . C51 C -0.5729(12) 0.7225(10) 0.3158(8) 0.040(5) Uani 1 1 d . . . C52 C -0.4581(12) 0.7806(12) 0.2372(7) 0.042(5) Uani 1 1 d . . . C53 C -0.3890(11) 0.7577(11) 0.3484(8) 0.041(5) Uani 1 1 d . . . C101 C -0.1124(11) 0.6750(9) 0.1893(6) 0.029(4) Uani 1 1 d . . . C102 C -0.0994(10) 0.6051(9) 0.1562(6) 0.028(4) Uani 1 1 d . . . C103 C -0.0496(10) 0.6182(9) 0.1112(6) 0.028(4) Uani 1 1 d . . . H10A H -0.0392 0.5757 0.0888 0.033 Uiso 1 1 calc R . . C104 C -0.0175(11) 0.6902(10) 0.1003(6) 0.036(4) Uani 1 1 d . . . H10B H 0.0161 0.6956 0.0714 0.043 Uiso 1 1 calc R . . C105 C -0.0334(12) 0.7572(10) 0.1314(7) 0.040(5) Uani 1 1 d . . . H10C H -0.0121 0.8067 0.1227 0.048 Uiso 1 1 calc R . . C106 C -0.0804(10) 0.7484(10) 0.1741(7) 0.033(4) Uani 1 1 d . . . H10D H -0.0919 0.7931 0.1942 0.039 Uiso 1 1 calc R . . C201 C -0.5155(9) 0.5484(9) 0.2392(5) 0.021(3) Uani 1 1 d . . . C202 C -0.5302(10) 0.6293(10) 0.2310(6) 0.028(4) Uani 1 1 d . . . C203 C -0.5911(12) 0.6534(11) 0.1879(7) 0.045(5) Uani 1 1 d . . . H20A H -0.6034 0.7070 0.1823 0.053 Uiso 1 1 calc R . . C204 C -0.6326(13) 0.5968(12) 0.1538(7) 0.055(6) Uani 1 1 d . . . H20B H -0.6720 0.6127 0.1246 0.066 Uiso 1 1 calc R . . C205 C -0.6163(11) 0.5170(12) 0.1624(7) 0.046(5) Uani 1 1 d . . . H20C H -0.6449 0.4794 0.1393 0.056 Uiso 1 1 calc R . . C206 C -0.5585(11) 0.4937(10) 0.2046(7) 0.040(5) Uani 1 1 d . . . H20D H -0.5476 0.4399 0.2103 0.048 Uiso 1 1 calc R . . C711 C 0.0559(10) 0.5386(10) 0.2847(7) 0.034(4) Uani 1 1 d . . . C712 C 0.0950(13) 0.5869(12) 0.2504(8) 0.057(6) Uani 1 1 d . . . H71A H 0.0610 0.6186 0.2256 0.068 Uiso 1 1 calc R . . C713 C 0.1864(12) 0.5890(14) 0.2525(10) 0.070(7) Uani 1 1 d . . . H71B H 0.2124 0.6230 0.2293 0.084 Uiso 1 1 calc R . . C714 C 0.2367(15) 0.5436(15) 0.2867(10) 0.076(7) Uani 1 1 d . . . H71C H 0.2973 0.5453 0.2869 0.091 Uiso 1 1 calc R . . C715 C 0.1983(13) 0.4928(14) 0.3226(10) 0.074(7) Uani 1 1 d . . . H71D H 0.2331 0.4612 0.3470 0.089 Uiso 1 1 calc R . . C716 C 0.1071(12) 0.4906(11) 0.3210(8) 0.050(5) Uani 1 1 d . . . H71E H 0.0808 0.4570 0.3442 0.060 Uiso 1 1 calc R . . C721 C -0.1094(11) 0.4623(9) 0.3439(6) 0.030(4) Uani 1 1 d . . . C722 C -0.1636(12) 0.3982(12) 0.3362(7) 0.050(5) Uani 1 1 d . . . H72A H -0.1885 0.3856 0.3014 0.060 Uiso 1 1 calc R . . C723 C -0.1824(13) 0.3503(12) 0.3810(8) 0.057(6) Uani 1 1 d . . . H72B H -0.2185 0.3060 0.3753 0.068 Uiso 1 1 calc R . . C724 C -0.1470(14) 0.3699(13) 0.4325(8) 0.060(6) Uani 1 1 d . . . H72C H -0.1614 0.3412 0.4624 0.072 Uiso 1 1 calc R . . C725 C -0.0869(17) 0.4360(14) 0.4393(7) 0.073(8) Uani 1 1 d . . . H72D H -0.0587 0.4481 0.4735 0.088 Uiso 1 1 calc R . . C726 C -0.0720(13) 0.4802(11) 0.3954(7) 0.049(5) Uani 1 1 d . . . H72E H -0.0351 0.5241 0.4003 0.059 Uiso 1 1 calc R . . C811 C -0.3068(10) 0.4233(9) 0.0692(6) 0.027(4) Uani 1 1 d . . . C812 C -0.3443(12) 0.4167(12) 0.0175(7) 0.053(6) Uani 1 1 d . . . H81A H -0.3104 0.4221 -0.0112 0.064 Uiso 1 1 calc R . . C813 C -0.4339(16) 0.4017(14) 0.0071(9) 0.078(8) Uani 1 1 d . . . H81B H -0.4588 0.3972 -0.0288 0.094 Uiso 1 1 calc R . . C814 C -0.4865(12) 0.3934(12) 0.0487(9) 0.056(6) Uani 1 1 d . . . H81C H -0.5466 0.3855 0.0416 0.067 Uiso 1 1 calc R . . C815 C -0.4462(12) 0.3974(9) 0.1006(8) 0.038(5) Uani 1 1 d . . . H81D H -0.4795 0.3903 0.1295 0.046 Uiso 1 1 calc R . . C816 C -0.3587(13) 0.4115(10) 0.1115(7) 0.043(5) Uani 1 1 d . . . H81E H -0.3333 0.4132 0.1473 0.052 Uiso 1 1 calc R . . C821 C -0.1382(12) 0.3463(9) 0.0742(7) 0.033(4) Uani 1 1 d . . . C822 C -0.0499(11) 0.3411(11) 0.0628(6) 0.037(4) Uani 1 1 d . . . H82A H -0.0192 0.3877 0.0580 0.045 Uiso 1 1 calc R . . C823 C -0.0084(13) 0.2700(11) 0.0586(6) 0.044(5) Uani 1 1 d . . . H82B H 0.0493 0.2675 0.0507 0.052 Uiso 1 1 calc R . . C824 C -0.0567(16) 0.1998(12) 0.0669(7) 0.056(6) Uani 1 1 d . . . H82C H -0.0302 0.1506 0.0637 0.067 Uiso 1 1 calc R . . C825 C -0.1415(15) 0.2029(12) 0.0794(7) 0.055(6) Uani 1 1 d . . . H82D H -0.1709 0.1563 0.0864 0.066 Uiso 1 1 calc R . . C826 C -0.1840(11) 0.2767(10) 0.0818(7) 0.035(4) Uani 1 1 d . . . H82E H -0.2425 0.2788 0.0884 0.043 Uiso 1 1 calc R . . C831 C -0.1707(10) 0.4985(11) 0.0222(6) 0.033(4) Uani 1 1 d . . . C832 C -0.1970(11) 0.5774(10) 0.0197(7) 0.035(4) Uani 1 1 d . . . H83A H -0.2117 0.6032 0.0507 0.042 Uiso 1 1 calc R . . C833 C -0.2011(12) 0.6178(11) -0.0302(7) 0.046(5) Uani 1 1 d . . . H83B H -0.2200 0.6703 -0.0320 0.055 Uiso 1 1 calc R . . C834 C -0.1784(13) 0.5825(14) -0.0754(8) 0.059(6) Uani 1 1 d . . . H83C H -0.1810 0.6111 -0.1077 0.071 Uiso 1 1 calc R . . C835 C -0.1507(12) 0.5025(12) -0.0743(7) 0.048(5) Uani 1 1 d . . . H83D H -0.1348 0.4775 -0.1053 0.058 Uiso 1 1 calc R . . C836 C -0.1481(12) 0.4629(11) -0.0253(6) 0.042(5) Uani 1 1 d . . . H83E H -0.1304 0.4101 -0.0238 0.050 Uiso 1 1 calc R . . C61 C -0.230(2) 0.858(2) 0.0262(18) 0.080 Uiso 0.50 1 d PD . . H61A H -0.1870 0.8947 0.0418 0.120 Uiso 0.50 1 calc PR . . H61B H -0.2207 0.8473 -0.0109 0.120 Uiso 0.50 1 calc PR . . H61C H -0.2250 0.8089 0.0465 0.120 Uiso 0.50 1 calc PR . . C62 C -0.322(2) 0.8927(19) 0.0282(17) 0.080 Uiso 0.50 1 d PD . . H62A H -0.3360 0.9044 0.0648 0.096 Uiso 0.50 1 calc PR . . H62B H -0.3344 0.9382 0.0046 0.096 Uiso 0.50 1 calc PR . . C63 C -0.3636(15) 0.8155(16) 0.0051(17) 0.080 Uiso 0.50 1 d PD . . H63A H -0.3729 0.7764 0.0327 0.096 Uiso 0.50 1 calc PR . . H63B H -0.3327 0.7922 -0.0232 0.096 Uiso 0.50 1 calc PR . . C64 C -0.4470(15) 0.860(2) -0.0167(13) 0.080 Uiso 0.50 1 d PD . . H64A H -0.4460 0.9159 -0.0071 0.096 Uiso 0.50 1 calc PR . . H64B H -0.4625 0.8533 -0.0555 0.096 Uiso 0.50 1 calc PR . . C65 C -0.502(2) 0.810(2) 0.0177(16) 0.080 Uiso 0.50 1 d PD . . H65A H -0.4863 0.8160 0.0565 0.096 Uiso 0.50 1 calc PR . . H65B H -0.5040 0.7540 0.0077 0.096 Uiso 0.50 1 calc PR . . C66 C -0.585(2) 0.856(2) -0.0042(17) 0.080 Uiso 0.50 1 d PD . . H66A H -0.6325 0.8200 -0.0130 0.120 Uiso 0.50 1 calc PR . . H66B H -0.5737 0.8852 -0.0363 0.120 Uiso 0.50 1 calc PR . . H66C H -0.6000 0.8931 0.0230 0.120 Uiso 0.50 1 calc PR . . 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 0.0197(3) 0.0235(3) 0.0236(3) 0.0002(3) 0.0016(3) 0.0009(3) Os2 0.0200(3) 0.0247(4) 0.0256(3) 0.0005(3) 0.0002(3) 0.0014(3) Os3 0.0220(3) 0.0247(4) 0.0272(3) -0.0023(3) 0.0012(3) -0.0029(3) Os4 0.0230(3) 0.0246(4) 0.0324(4) 0.0005(3) 0.0051(3) -0.0003(3) Os5 0.0253(4) 0.0251(4) 0.0367(4) -0.0040(3) 0.0046(3) 0.0033(3) Sb6 0.0200(6) 0.0230(6) 0.0295(6) -0.0016(5) 0.0035(5) -0.0002(5) Sb7 0.0224(6) 0.0287(6) 0.0243(6) -0.0002(5) -0.0002(5) 0.0016(5) P8 0.022(2) 0.031(3) 0.028(2) 0.0011(19) 0.0001(19) 0.0000(19) O11 0.040(8) 0.048(9) 0.039(7) 0.005(6) 0.011(6) 0.004(7) O12 0.026(7) 0.064(9) 0.035(7) 0.003(6) 0.002(6) 0.008(7) O21 0.056(9) 0.047(9) 0.077(10) -0.005(7) -0.044(8) 0.008(7) O22 0.070(10) 0.036(8) 0.068(9) 0.006(7) 0.002(8) 0.010(8) O31 0.058(9) 0.023(7) 0.083(10) 0.000(7) 0.000(8) 0.008(7) O32 0.036(8) 0.059(9) 0.052(8) -0.008(7) 0.002(7) -0.015(7) O33 0.043(8) 0.103(12) 0.031(7) 0.006(8) 0.017(7) -0.003(8) O41 0.066(10) 0.057(9) 0.048(8) -0.006(7) -0.021(8) 0.011(8) O42 0.048(9) 0.059(9) 0.069(10) 0.010(7) 0.033(8) -0.010(7) O43 0.050(9) 0.047(9) 0.076(10) -0.028(8) 0.014(8) 0.006(7) O51 0.025(7) 0.058(10) 0.102(12) 0.005(8) 0.015(8) 0.005(7) O52 0.084(12) 0.044(9) 0.083(11) 0.026(8) 0.033(9) 0.019(8) O53 0.061(10) 0.065(10) 0.086(11) -0.018(9) -0.016(9) -0.012(9) C11 0.007(8) 0.051(12) 0.024(9) 0.010(8) 0.007(7) 0.017(8) C12 0.034(10) 0.030(10) 0.023(9) -0.006(7) 0.006(8) 0.011(8) C21 0.039(11) 0.016(9) 0.049(11) 0.001(8) 0.013(9) 0.023(8) C22 0.027(10) 0.039(11) 0.032(10) -0.001(8) 0.008(8) 0.007(8) C31 0.046(12) 0.028(10) 0.031(10) -0.008(8) 0.003(9) 0.006(9) C32 0.021(9) 0.049(12) 0.022(9) -0.010(8) -0.004(7) -0.001(8) C33 0.036(11) 0.028(10) 0.049(12) -0.012(9) 0.011(9) 0.011(8) C41 0.036(10) 0.031(10) 0.036(10) -0.007(8) 0.004(9) 0.002(9) C42 0.037(11) 0.027(10) 0.036(10) -0.001(8) 0.019(9) 0.003(8) C43 0.021(9) 0.019(9) 0.059(12) -0.004(9) 0.005(9) 0.012(7) C51 0.033(11) 0.021(10) 0.065(13) -0.010(9) 0.002(10) 0.014(8) C52 0.035(11) 0.053(13) 0.039(11) -0.012(10) 0.010(9) 0.011(10) C53 0.023(10) 0.044(12) 0.059(13) -0.006(10) 0.018(10) 0.014(9) C101 0.033(10) 0.022(9) 0.033(9) -0.004(7) 0.002(8) -0.002(8) C102 0.027(9) 0.031(10) 0.025(9) 0.010(7) 0.005(7) -0.003(8) C103 0.033(10) 0.019(9) 0.031(9) -0.004(7) 0.001(8) -0.002(7) C104 0.041(11) 0.041(11) 0.029(9) 0.012(8) 0.020(8) -0.005(9) C105 0.046(12) 0.026(10) 0.050(12) 0.008(9) 0.018(10) -0.010(9) C106 0.014(8) 0.046(11) 0.038(10) 0.002(8) 0.006(8) -0.004(8) C201 0.017(8) 0.036(10) 0.010(7) 0.004(7) 0.007(6) 0.008(7) C202 0.021(9) 0.040(10) 0.025(9) -0.003(8) 0.002(7) 0.006(8) C203 0.036(11) 0.051(12) 0.048(12) -0.012(10) 0.009(9) 0.004(10) C204 0.062(14) 0.058(14) 0.039(11) 0.000(10) -0.029(10) 0.009(12) C205 0.034(11) 0.066(14) 0.036(11) -0.015(10) -0.010(9) -0.018(10) C206 0.029(10) 0.035(11) 0.054(12) -0.007(9) -0.002(9) 0.003(8) C711 0.010(8) 0.029(10) 0.061(12) -0.012(9) -0.007(8) 0.004(7) C712 0.044(13) 0.065(15) 0.060(14) 0.003(11) -0.004(11) -0.016(12) C713 0.013(10) 0.099(19) 0.095(18) -0.013(15) -0.003(11) -0.014(12) C714 0.035(13) 0.10(2) 0.088(19) 0.004(15) -0.018(13) 0.013(14) C715 0.030(12) 0.080(18) 0.101(19) 0.019(15) -0.042(13) 0.007(12) C716 0.039(12) 0.037(12) 0.070(14) 0.004(10) -0.012(11) 0.011(9) C721 0.039(10) 0.025(9) 0.028(9) 0.002(7) 0.009(8) -0.003(8) C722 0.042(12) 0.066(14) 0.036(11) 0.014(10) -0.023(9) 0.015(11) C723 0.055(14) 0.070(15) 0.043(12) 0.024(11) -0.002(11) -0.011(12) C724 0.064(16) 0.064(16) 0.051(14) 0.027(12) 0.012(12) 0.012(13) C725 0.11(2) 0.092(19) 0.014(10) -0.007(11) -0.004(12) 0.015(17) C726 0.073(15) 0.044(12) 0.028(10) -0.020(9) -0.002(10) 0.000(11) C811 0.027(9) 0.030(10) 0.025(9) -0.003(7) 0.007(7) -0.001(8) C812 0.023(10) 0.099(17) 0.037(11) 0.005(11) 0.002(9) -0.007(11) C813 0.068(17) 0.11(2) 0.051(14) 0.001(14) -0.027(13) -0.009(15) C814 0.016(10) 0.080(16) 0.069(15) -0.013(12) -0.004(10) -0.019(10) C815 0.036(11) 0.032(11) 0.052(12) 0.010(9) 0.024(10) -0.001(9) C816 0.061(14) 0.038(11) 0.029(10) 0.001(8) -0.008(10) 0.003(10) C821 0.039(11) 0.024(9) 0.038(10) -0.009(8) 0.012(9) -0.005(8) C822 0.036(11) 0.040(11) 0.037(10) -0.010(8) 0.010(9) 0.002(9) C823 0.046(12) 0.050(13) 0.029(10) -0.010(9) -0.022(9) 0.012(10) C824 0.082(17) 0.036(12) 0.043(12) -0.015(10) -0.022(12) 0.017(12) C825 0.061(15) 0.056(14) 0.049(13) -0.004(11) 0.006(12) -0.001(12) C826 0.025(10) 0.034(11) 0.047(11) 0.003(9) -0.001(8) 0.012(8) C831 0.011(8) 0.059(12) 0.028(9) 0.002(8) -0.005(7) -0.001(8) C832 0.033(10) 0.045(12) 0.031(10) 0.008(9) 0.021(8) -0.003(9) C833 0.045(12) 0.044(12) 0.046(12) 0.014(10) -0.007(10) 0.004(10) C834 0.044(13) 0.087(18) 0.045(13) 0.016(12) 0.004(11) 0.012(13) C835 0.043(12) 0.072(15) 0.033(10) 0.011(10) 0.014(9) -0.002(11) C836 0.053(13) 0.050(12) 0.023(9) 0.009(9) 0.013(9) 0.006(10) _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 1.889(17) . ? Os1 C11 1.908(18) . ? Os1 C102 2.164(15) . ? Os1 P8 2.419(4) . ? Os1 Sb7 2.6429(12) . ? Os1 Os2 2.9841(9) . ? Os2 C21 1.863(19) . ? Os2 C22 1.869(18) . ? Os2 C101 2.214(16) . ? Os2 C102 2.397(16) . ? Os2 Sb6 2.5668(12) . ? Os2 Os3 2.9660(9) . ? Os3 C33 1.885(19) . ? Os3 C32 1.932(17) . ? Os3 C31 1.942(17) . ? Os3 C101 2.317(16) . ? Os3 Sb7 2.6631(12) . ? Os3 Sb6 2.7820(12) . ? Os4 C43 1.921(16) . ? Os4 C42 1.936(17) . ? Os4 C41 1.973(17) . ? Os4 C201 2.180(13) . ? Os4 Sb6 2.6518(12) . ? Os4 Os5 3.0107(9) . ? Os5 C52 1.89(2) . ? Os5 C53 1.93(2) . ? Os5 C51 1.930(19) . ? Os5 C202 2.135(15) . ? Os5 Sb6 2.6456(12) . ? Sb7 C721 2.144(15) . ? Sb7 C711 2.152(15) . ? P8 C821 1.819(16) . ? P8 C811 1.829(16) . ? P8 C831 1.843(17) . ? O11 C11 1.153(18) . ? O12 C12 1.149(17) . ? O21 C21 1.155(19) . ? O22 C22 1.152(18) . ? O31 C31 1.137(18) . ? O32 C32 1.117(17) . ? O33 C33 1.157(19) . ? O41 C41 1.136(18) . ? O42 C42 1.118(18) . ? O43 C43 1.111(17) . ? O51 C51 1.125(19) . ? O52 C52 1.14(2) . ? O53 C53 1.14(2) . ? C101 C106 1.40(2) . ? C101 C102 1.46(2) . ? C102 C103 1.44(2) . ? C103 C104 1.35(2) . ? C104 C105 1.40(2) . ? C105 C106 1.35(2) . ? C201 C206 1.38(2) . ? C201 C202 1.39(2) . ? C202 C203 1.40(2) . ? C203 C204 1.38(2) . ? C204 C205 1.38(2) . ? C205 C206 1.35(2) . ? C711 C712 1.36(2) . ? C711 C716 1.39(2) . ? C712 C713 1.40(2) . ? C713 C714 1.32(3) . ? C714 C715 1.41(3) . ? C715 C716 1.40(3) . ? C721 C722 1.36(2) . ? C721 C726 1.37(2) . ? C722 C723 1.42(2) . ? C723 C724 1.37(3) . ? C724 C725 1.44(3) . ? C725 C726 1.36(3) . ? C811 C812 1.35(2) . ? C811 C816 1.39(2) . ? C812 C813 1.39(3) . ? C813 C814 1.38(3) . ? C814 C815 1.37(2) . ? C815 C816 1.36(2) . ? C821 C826 1.39(2) . ? C821 C822 1.42(2) . ? C822 C823 1.37(2) . ? C823 C824 1.42(3) . ? C824 C825 1.37(3) . ? C825 C826 1.41(2) . ? C831 C832 1.39(2) . ? C831 C836 1.39(2) . ? C832 C833 1.40(2) . ? C833 C834 1.35(2) . ? C834 C835 1.41(3) . ? C835 C836 1.38(2) . ? C61 C62 1.541(10) . ? C62 C63 1.529(10) . ? C63 C64 1.532(10) . ? C64 C65 1.520(10) . ? C65 C66 1.543(10) . ? 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 89.8(6) . . ? C12 Os1 C102 93.5(6) . . ? C11 Os1 C102 174.5(6) . . ? C12 Os1 P8 92.9(5) . . ? C11 Os1 P8 85.6(5) . . ? C102 Os1 P8 98.7(4) . . ? C12 Os1 Sb7 88.4(5) . . ? C11 Os1 Sb7 94.0(5) . . ? C102 Os1 Sb7 81.7(4) . . ? P8 Os1 Sb7 178.65(11) . . ? C12 Os1 Os2 145.9(5) . . ? C11 Os1 Os2 123.8(4) . . ? C102 Os1 Os2 52.6(4) . . ? P8 Os1 Os2 95.21(10) . . ? Sb7 Os1 Os2 83.97(3) . . ? C21 Os2 C22 86.0(7) . . ? C21 Os2 C101 146.8(7) . . ? C22 Os2 C101 87.0(6) . . ? C21 Os2 C102 119.4(6) . . ? C22 Os2 C102 112.1(6) . . ? C101 Os2 C102 36.6(5) . . ? C21 Os2 Sb6 102.4(5) . . ? C22 Os2 Sb6 94.5(5) . . ? C101 Os2 Sb6 110.5(4) . . ? C102 Os2 Sb6 130.8(3) . . ? C21 Os2 Os3 161.9(5) . . ? C22 Os2 Os3 91.4(5) . . ? C101 Os2 Os3 50.6(4) . . ? C102 Os2 Os3 78.1(4) . . ? Sb6 Os2 Os3 59.86(3) . . ? C21 Os2 Os1 101.1(4) . . ? C22 Os2 Os1 157.5(5) . . ? C101 Os2 Os1 75.3(4) . . ? C102 Os2 Os1 45.8(4) . . ? Sb6 Os2 Os1 104.63(3) . . ? Os3 Os2 Os1 88.06(2) . . ? C33 Os3 C32 94.1(7) . . ? C33 Os3 C31 92.6(7) . . ? C32 Os3 C31 91.3(7) . . ? C33 Os3 C101 170.4(6) . . ? C32 Os3 C101 81.0(6) . . ? C31 Os3 C101 95.8(6) . . ? C33 Os3 Sb7 92.3(5) . . ? C32 Os3 Sb7 90.5(5) . . ? C31 Os3 Sb7 174.6(5) . . ? C101 Os3 Sb7 79.5(4) . . ? C33 Os3 Sb6 85.0(5) . . ? C32 Os3 Sb6 175.6(5) . . ? C31 Os3 Sb6 84.4(5) . . ? C101 Os3 Sb6 100.6(4) . . ? Sb7 Os3 Sb6 93.79(4) . . ? C33 Os3 Os2 137.2(5) . . ? C32 Os3 Os2 128.5(4) . . ? C31 Os3 Os2 90.9(5) . . ? C101 Os3 Os2 47.6(4) . . ? Sb7 Os3 Os2 83.98(3) . . ? Sb6 Os3 Os2 52.93(3) . . ? C43 Os4 C42 97.4(7) . . ? C43 Os4 C41 95.8(7) . . ? C42 Os4 C41 96.3(7) . . ? C43 Os4 C201 90.1(6) . . ? C42 Os4 C201 86.3(6) . . ? C41 Os4 C201 173.2(6) . . ? C43 Os4 Sb6 97.4(5) . . ? C42 Os4 Sb6 161.1(5) . . ? C41 Os4 Sb6 93.9(5) . . ? C201 Os4 Sb6 81.9(4) . . ? C43 Os4 Os5 145.7(5) . . ? C42 Os4 Os5 106.4(5) . . ? C41 Os4 Os5 105.4(5) . . ? C201 Os4 Os5 67.8(4) . . ? Sb6 Os4 Os5 55.27(3) . . ? C52 Os5 C53 97.4(8) . . ? C52 Os5 C51 100.2(7) . . ? C53 Os5 C51 98.1(7) . . ? C52 Os5 C202 87.0(7) . . ? C53 Os5 C202 174.0(7) . . ? C51 Os5 C202 85.1(7) . . ? C52 Os5 Sb6 93.0(5) . . ? C53 Os5 Sb6 93.8(5) . . ? C51 Os5 Sb6 160.9(5) . . ? C202 Os5 Sb6 81.8(4) . . ? C52 Os5 Os4 141.1(5) . . ? C53 Os5 Os4 105.9(5) . . ? C51 Os5 Os4 106.6(5) . . ? C202 Os5 Os4 68.2(4) . . ? Sb6 Os5 Os4 55.46(3) . . ? Os2 Sb6 Os5 133.13(5) . . ? Os2 Sb6 Os4 140.41(5) . . ? Os5 Sb6 Os4 69.27(3) . . ? Os2 Sb6 Os3 67.21(3) . . ? Os5 Sb6 Os3 123.65(4) . . ? Os4 Sb6 Os3 134.19(4) . . ? C721 Sb7 C711 101.3(7) . . ? C721 Sb7 Os1 121.1(4) . . ? C711 Sb7 Os1 108.7(5) . . ? C721 Sb7 Os3 113.0(4) . . ? C711 Sb7 Os3 110.1(4) . . ? Os1 Sb7 Os3 102.42(4) . . ? C821 P8 C811 104.5(8) . . ? C821 P8 C831 104.0(8) . . ? C811 P8 C831 99.4(7) . . ? C821 P8 Os1 106.6(6) . . ? C811 P8 Os1 116.9(5) . . ? C831 P8 Os1 123.5(6) . . ? O11 C11 Os1 178.5(14) . . ? O12 C12 Os1 175.7(14) . . ? O21 C21 Os2 173.5(14) . . ? O22 C22 Os2 177.3(15) . . ? O31 C31 Os3 177.6(16) . . ? O32 C32 Os3 175.8(15) . . ? O33 C33 Os3 177.6(17) . . ? O41 C41 Os4 174.3(16) . . ? O42 C42 Os4 175.9(16) . . ? O43 C43 Os4 176.4(17) . . ? O51 C51 Os5 177.1(17) . . ? O52 C52 Os5 175.5(17) . . ? O53 C53 Os5 175.5(18) . . ? C106 C101 C102 119.3(15) . . ? C106 C101 Os2 126.3(11) . . ? C102 C101 Os2 78.5(9) . . ? C106 C101 Os3 111.6(11) . . ? C102 C101 Os3 127.6(11) . . ? Os2 C101 Os3 81.7(5) . . ? C103 C102 C101 115.3(13) . . ? C103 C102 Os1 119.2(11) . . ? C101 C102 Os1 125.2(11) . . ? C103 C102 Os2 133.6(11) . . ? C101 C102 Os2 64.9(9) . . ? Os1 C102 Os2 81.6(5) . . ? C104 C103 C102 122.0(15) . . ? C103 C104 C105 121.7(15) . . ? C106 C105 C104 118.7(16) . . ? C105 C106 C101 122.7(17) . . ? C206 C201 C202 120.2(14) . . ? C206 C201 Os4 129.0(12) . . ? C202 C201 Os4 110.7(11) . . ? C201 C202 C203 118.6(15) . . ? C201 C202 Os5 113.3(11) . . ? C203 C202 Os5 127.9(13) . . ? C204 C203 C202 119.5(17) . . ? C205 C204 C203 120.9(17) . . ? C206 C205 C204 119.6(17) . . ? C205 C206 C201 121.2(17) . . ? C712 C711 C716 119.6(17) . . ? C712 C711 Sb7 117.6(13) . . ? C716 C711 Sb7 122.6(14) . . ? C711 C712 C713 120(2) . . ? C714 C713 C712 122(2) . . ? C713 C714 C715 120(2) . . ? C716 C715 C714 119.0(19) . . ? C711 C716 C715 120(2) . . ? C722 C721 C726 119.4(16) . . ? C722 C721 Sb7 118.8(12) . . ? C726 C721 Sb7 121.7(13) . . ? C721 C722 C723 120.8(17) . . ? C724 C723 C722 119(2) . . ? C723 C724 C725 118.7(18) . . ? C726 C725 C724 119.3(18) . . ? C725 C726 C721 122.2(19) . . ? C812 C811 C816 118.6(16) . . ? C812 C811 P8 120.8(13) . . ? C816 C811 P8 120.6(13) . . ? C811 C812 C813 120.1(18) . . ? C814 C813 C812 121.6(19) . . ? C815 C814 C813 117.0(17) . . ? C816 C815 C814 122.1(17) . . ? C815 C816 C811 120.5(16) . . ? C826 C821 C822 119.0(16) . . ? C826 C821 P8 119.9(13) . . ? C822 C821 P8 121.0(13) . . ? C823 C822 C821 122.2(18) . . ? C822 C823 C824 117.6(19) . . ? C825 C824 C823 121.6(19) . . ? C824 C825 C826 120(2) . . ? C821 C826 C825 119.6(17) . . ? C832 C831 C836 118.1(16) . . ? C832 C831 P8 117.4(13) . . ? C836 C831 P8 123.3(14) . . ? C831 C832 C833 119.2(16) . . ? C834 C833 C832 121.7(19) . . ? C833 C834 C835 120.6(19) . . ? C836 C835 C834 117.2(18) . . ? C835 C836 C831 123.1(18) . . ? C63 C62 C61 90.4(14) . . ? C62 C63 C64 90.7(15) . . ? C65 C64 C63 91.3(15) . . ? C64 C65 C66 90.3(14) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 29.41 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 1.809 _refine_diff_density_min -1.656 _refine_diff_density_rms 0.366 #END