Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Ang, Siau-Gek' 'Ang, How-Ghee' 'Zhong, Xinhau' _publ_contact_author_name 'Prof Siau-Gek Ang' _publ_contact_author_address ; Prof Siau-Gek Ang Department of Chemistry National University of Singapore 119260 SINGAPORE ; data_1 _database_code_CSD 158406 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36.75 H23 Cl0.50 O11 Os3 P3' _chemical_formula_weight 1321.79 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' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.787(3) _cell_length_b 33.007(7) _cell_length_c 16.283(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.47(3) _cell_angle_gamma 90.00 _cell_volume 8316(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18313 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not measured _exptl_crystal_density_diffrn 2.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4904 _exptl_absorpt_coefficient_mu 9.347 _exptl_absorpt_correction_type sadas (Sheldrick, 1996) _exptl_absorpt_correction_T_min 0.040764 _exptl_absorpt_correction_T_max 0.109530 _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 54537 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 29.43 _reflns_number_total 20704 _reflns_number_gt 12208 _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^)+(0.0434P)^2^+23.2904P] 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 20704 _refine_ls_number_parameters 1096 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1142 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1056 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.347 _refine_ls_shift/su_mean 0.022 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 0.03124(2) 0.196625(12) 0.18343(2) 0.04688(10) Uani 1 1 d . . . Os2 Os 0.09371(3) 0.128605(13) 0.29248(3) 0.05560(12) Uani 1 1 d . . . Os3 Os 0.21095(3) 0.174687(14) 0.21337(3) 0.05820(12) Uani 1 1 d . . . Os4 Os 0.55410(2) 0.390534(12) 0.27022(2) 0.04821(10) Uani 1 1 d . . . Os5 Os 0.72748(3) 0.413308(14) 0.25956(3) 0.05792(12) Uani 1 1 d . . . Os6 Os 0.58495(3) 0.462722(13) 0.17641(3) 0.05422(11) Uani 1 1 d . . . Cl1 Cl 0.484(4) -0.0365(16) 0.546(4) 0.40(4) Uani 0.25 1 d P . . P1 P -0.11878(16) 0.19716(8) 0.17665(14) 0.0451(6) Uani 1 1 d . . . P2 P -0.19643(17) 0.23781(8) 0.08275(16) 0.0503(6) Uani 1 1 d . . . P3 P -0.29520(17) 0.25119(9) 0.15651(19) 0.0579(7) Uani 1 1 d . . . P4 P 0.40363(16) 0.38850(8) 0.26057(16) 0.0482(6) Uani 1 1 d . . . P5 P 0.35152(18) 0.34234(8) 0.33575(16) 0.0521(6) Uani 1 1 d . . . P6 P 0.22977(17) 0.33209(8) 0.24568(17) 0.0549(7) Uani 1 1 d . . . O11 O 0.0023(6) 0.1433(3) 0.0254(5) 0.085(3) Uani 1 1 d . . . O12 O 0.0469(5) 0.2552(2) 0.3313(5) 0.072(2) Uani 1 1 d . . . O13 O 0.0655(5) 0.2678(3) 0.0790(5) 0.080(2) Uani 1 1 d . . . O21 O 0.1242(6) 0.1862(3) 0.4435(6) 0.089(3) Uani 1 1 d . . . O22 O 0.2374(7) 0.0743(3) 0.3839(7) 0.115(4) Uani 1 1 d . . . O23 O -0.0558(6) 0.0897(3) 0.3563(6) 0.090(3) Uani 1 1 d . . . O24 O 0.0457(8) 0.0734(3) 0.1365(7) 0.112(3) Uani 1 1 d . . . O31 O 0.2700(6) 0.2357(3) 0.0957(6) 0.110(4) Uani 1 1 d . . . O32 O 0.2360(5) 0.2384(3) 0.3539(5) 0.083(3) Uani 1 1 d . . . O33 O 0.3808(6) 0.1344(3) 0.2942(7) 0.118(4) Uani 1 1 d . . . O34 O 0.1901(7) 0.1132(4) 0.0680(7) 0.114(4) Uani 1 1 d . . . O41 O 0.6181(6) 0.3198(3) 0.3840(6) 0.087(3) Uani 1 1 d . . . O42 O 0.5701(6) 0.4395(3) 0.4338(5) 0.093(3) Uani 1 1 d . . . O43 O 0.5286(5) 0.3369(3) 0.1128(5) 0.083(3) Uani 1 1 d . . . O51 O 0.8732(7) 0.4597(4) 0.2066(8) 0.130(4) Uani 1 1 d . . . O52 O 0.7135(5) 0.3606(3) 0.1011(6) 0.091(3) Uani 1 1 d . . . O53 O 0.8226(7) 0.3455(4) 0.3649(7) 0.126(4) Uani 1 1 d . . . O54 O 0.7441(7) 0.4673(4) 0.4152(7) 0.124(4) Uani 1 1 d . . . O61 O 0.7073(7) 0.5216(3) 0.1169(7) 0.116(4) Uani 1 1 d . . . O62 O 0.5700(7) 0.4107(3) 0.0184(5) 0.106(3) Uani 1 1 d . . . O63 O 0.4155(6) 0.5039(3) 0.0938(7) 0.116(4) Uani 1 1 d . . . O64 O 0.5833(9) 0.5128(3) 0.3365(7) 0.130(4) Uani 1 1 d . . . H10A H -0.190(11) 0.130(5) 0.263(10) 0.157 Uiso 1 1 d . . . H10B H -0.252(11) 0.070(5) 0.219(11) 0.157 Uiso 1 1 d . . . H10C H -0.277(10) 0.047(5) 0.103(10) 0.157 Uiso 1 1 d . . . H10D H -0.227(15) 0.093(7) 0.020(14) 0.157 Uiso 1 1 d . . . H10E H -0.175(11) 0.150(5) 0.027(11) 0.157 Uiso 1 1 d . . . H20A H -0.137(10) 0.299(5) -0.046(10) 0.157 Uiso 1 1 d . . . H20B H -0.061(10) 0.354(5) -0.027(10) 0.157 Uiso 1 1 d . . . H20C H -0.019(10) 0.385(5) 0.106(10) 0.157 Uiso 1 1 d . . . H20D H -0.049(13) 0.334(7) 0.204(13) 0.157 Uiso 1 1 d . . . H20E H -0.092(10) 0.282(5) 0.219(10) 0.157 Uiso 1 1 d . . . H30A H -0.355(11) 0.176(6) 0.185(11) 0.157 Uiso 1 1 d . . . H30B H -0.483(11) 0.132(5) 0.156(10) 0.157 Uiso 1 1 d . . . H30C H -0.571(11) 0.144(5) 0.037(10) 0.157 Uiso 1 1 d . . . H30D H -0.537(13) 0.205(7) -0.002(13) 0.157 Uiso 1 1 d . . . H30E H -0.438(11) 0.251(5) 0.053(11) 0.157 Uiso 1 1 d . . . H40A H 0.409(10) 0.418(5) 0.441(10) 0.157 Uiso 1 1 d . . . H40B H 0.361(10) 0.483(5) 0.504(10) 0.157 Uiso 1 1 d . . . H40C H 0.288(11) 0.525(5) 0.386(11) 0.157 Uiso 1 1 d . . . H40D H 0.278(11) 0.522(5) 0.251(11) 0.157 Uiso 1 1 d . . . H40E H 0.313(17) 0.457(7) 0.227(16) 0.157 Uiso 1 1 d . . . H50A H 0.420(13) 0.289(7) 0.210(11) 0.157 Uiso 1 1 d . . . H50B H 0.465(10) 0.227(5) 0.177(10) 0.157 Uiso 1 1 d . . . H50C H 0.513(10) 0.194(5) 0.296(10) 0.157 Uiso 1 1 d . . . H50D H 0.492(11) 0.219(5) 0.410(11) 0.157 Uiso 1 1 d . . . H50E H 0.438(11) 0.278(5) 0.432(10) 0.157 Uiso 1 1 d . . . H60A H 0.145(12) 0.333(5) 0.371(12) 0.157 Uiso 1 1 d . . . H60B H 0.062(13) 0.365(6) 0.415(12) 0.157 Uiso 1 1 d . . . H60C H 0.008(10) 0.438(5) 0.387(10) 0.157 Uiso 1 1 d . . . H60D H 0.072(11) 0.453(5) 0.262(11) 0.157 Uiso 1 1 d . . . H60E H 0.162(11) 0.411(5) 0.215(11) 0.157 Uiso 1 1 d . . . H70A H -0.354(10) 0.251(5) 0.299(10) 0.157 Uiso 1 1 d . . . H70B H -0.269(11) 0.234(5) 0.445(11) 0.157 Uiso 1 1 d . . . H70C H -0.131(13) 0.194(6) 0.444(12) 0.157 Uiso 1 1 d . . . H70D H -0.068(11) 0.188(5) 0.364(11) 0.157 Uiso 1 1 d . . . H80A H 0.121(10) 0.342(5) 0.062(10) 0.157 Uiso 1 1 d . . . H80B H 0.166(10) 0.369(5) -0.044(10) 0.157 Uiso 1 1 d . . . H80C H 0.308(10) 0.403(5) -0.048(10) 0.157 Uiso 1 1 d . . . H80D H 0.410(10) 0.419(5) 0.090(10) 0.157 Uiso 1 1 d . . . C1 C 0.931(4) 0.4527(17) 0.611(4) 0.11(2) Uani 0.25 1 d PD . . C2 C 0.989(3) 0.4694(14) 0.578(4) 0.12(3) Uani 0.25 1 d PD . . C3 C 0.966(2) 0.4913(13) 0.513(3) 0.075(18) Uani 0.25 1 d PD . . C4 C 0.440(9) -0.002(3) 0.472(6) 0.25(7) Uani 0.25 1 d P . . C11 C 0.0165(7) 0.1615(3) 0.0860(7) 0.058(3) Uani 1 1 d . . . C12 C 0.0442(6) 0.2326(3) 0.2785(6) 0.052(2) Uani 1 1 d . . . C13 C 0.0496(6) 0.2408(4) 0.1176(6) 0.057(3) Uani 1 1 d . . . C21 C 0.1131(8) 0.1664(4) 0.3853(7) 0.065(3) Uani 1 1 d . . . C22 C 0.1829(8) 0.0943(4) 0.3490(8) 0.075(3) Uani 1 1 d . . . C23 C -0.0004(8) 0.1054(3) 0.3315(7) 0.064(3) Uani 1 1 d . . . C24 C 0.0651(9) 0.0949(4) 0.1920(8) 0.082(4) Uani 1 1 d . . . C31 C 0.2477(7) 0.2139(4) 0.1412(7) 0.071(3) Uani 1 1 d . . . C32 C 0.2228(7) 0.2149(4) 0.3031(7) 0.064(3) Uani 1 1 d . . . C33 C 0.3173(8) 0.1491(4) 0.2634(9) 0.081(4) Uani 1 1 d . . . C34 C 0.1934(8) 0.1346(4) 0.1238(9) 0.080(4) Uani 1 1 d . . . C41 C 0.5898(7) 0.3452(4) 0.3393(8) 0.066(3) Uani 1 1 d . . . C42 C 0.5634(7) 0.4229(3) 0.3706(8) 0.060(3) Uani 1 1 d . . . C43 C 0.5415(7) 0.3579(3) 0.1698(7) 0.057(3) Uani 1 1 d . . . C51 C 0.8179(8) 0.4420(4) 0.2277(9) 0.086(4) Uani 1 1 d . . . C52 C 0.7169(7) 0.3803(4) 0.1590(8) 0.067(3) Uani 1 1 d . . . C53 C 0.7857(8) 0.3698(4) 0.3233(8) 0.078(4) Uani 1 1 d . . . C54 C 0.7334(8) 0.4472(4) 0.3583(9) 0.085(4) Uani 1 1 d . . . C61 C 0.6600(8) 0.4996(4) 0.1390(8) 0.074(3) Uani 1 1 d . . . C62 C 0.5769(8) 0.4285(3) 0.0786(7) 0.065(3) Uani 1 1 d . . . C63 C 0.4770(9) 0.4880(4) 0.1258(8) 0.081(4) Uani 1 1 d . . . C64 C 0.5841(8) 0.4931(4) 0.2806(9) 0.075(3) Uani 1 1 d . . . C101 C -0.1756(6) 0.1497(3) 0.1464(6) 0.047(2) Uani 1 1 d . . . C102 C -0.2002(8) 0.1243(4) 0.2058(7) 0.064(3) Uani 1 1 d . . . C103 C -0.2428(9) 0.0878(4) 0.1828(11) 0.086(4) Uani 1 1 d . . . C104 C -0.2618(9) 0.0774(5) 0.1000(11) 0.092(4) Uani 1 1 d . . . C105 C -0.2391(12) 0.1024(6) 0.0410(10) 0.084(5) Uani 1 1 d . . . C106 C -0.1960(8) 0.1378(3) 0.0628(7) 0.065(3) Uani 1 1 d . . . C201 C -0.1381(6) 0.2863(3) 0.0994(6) 0.050(2) Uani 1 1 d . . . C202 C -0.1319(7) 0.3077(4) 0.0266(7) 0.063(3) Uani 1 1 d . . . C203 C -0.0917(8) 0.3456(4) 0.0316(9) 0.073(3) Uani 1 1 d . . . C204 C -0.0576(8) 0.3612(4) 0.1084(10) 0.081(4) Uani 1 1 d . . . C205 C -0.0636(9) 0.3411(5) 0.1810(9) 0.065(3) Uani 1 1 d . . . C206 C -0.1036(7) 0.3036(4) 0.1776(7) 0.060(3) Uani 1 1 d . . . C301 C -0.3797(7) 0.2138(3) 0.1172(7) 0.059(3) Uani 1 1 d . . . C302 C -0.3935(7) 0.1787(4) 0.1566(8) 0.064(3) Uani 1 1 d . . . C303 C -0.4631(9) 0.1547(4) 0.1289(9) 0.077(4) Uani 1 1 d . . . C304 C -0.5222(9) 0.1653(4) 0.0593(9) 0.080(4) Uani 1 1 d . . . C305 C -0.5085(10) 0.2000(6) 0.0167(10) 0.090(5) Uani 1 1 d . . . C306 C -0.4380(9) 0.2251(4) 0.0436(8) 0.076(4) Uani 1 1 d . . . C401 C 0.3584(7) 0.4343(3) 0.3006(7) 0.057(3) Uani 1 1 d . . . C402 C 0.3696(8) 0.4394(3) 0.3869(8) 0.070(3) Uani 1 1 d . . . C403 C 0.3428(12) 0.4751(5) 0.4196(10) 0.100(5) Uani 1 1 d . . . C404 C 0.2967(13) 0.5027(5) 0.3634(16) 0.120(7) Uani 1 1 d . . . C405 C 0.2845(11) 0.4977(5) 0.2783(13) 0.106(5) Uani 1 1 d . . . C406 C 0.3156(13) 0.4636(5) 0.2447(13) 0.080(5) Uani 1 1 d . . . C501 C 0.4088(6) 0.2961(3) 0.3161(6) 0.049(2) Uani 1 1 d . . . C502 C 0.4172(9) 0.2818(4) 0.2380(7) 0.062(3) Uani 1 1 d . . . C503 C 0.4572(8) 0.2459(4) 0.2279(8) 0.068(3) Uani 1 1 d . . . C504 C 0.4901(7) 0.2221(4) 0.2980(7) 0.065(3) Uani 1 1 d . . . C505 C 0.4798(9) 0.2361(4) 0.3771(8) 0.071(3) Uani 1 1 d . . . C506 C 0.4403(8) 0.2718(4) 0.3845(7) 0.059(3) Uani 1 1 d . . . C601 C 0.1590(7) 0.3685(4) 0.2859(7) 0.060(3) Uani 1 1 d . . . C602 C 0.1284(8) 0.3560(4) 0.3554(9) 0.077(4) Uani 1 1 d . . . C603 C 0.0737(11) 0.3803(7) 0.3880(10) 0.096(5) Uani 1 1 d . . . C604 C 0.0509(10) 0.4168(7) 0.3539(13) 0.117(6) Uani 1 1 d . . . C605 C 0.0807(10) 0.4290(5) 0.2841(11) 0.090(4) Uani 1 1 d . . . C606 C 0.1353(8) 0.4051(4) 0.2506(9) 0.073(4) Uani 1 1 d . . . C701 C -0.1630(6) 0.2115(3) 0.2691(6) 0.049(2) Uani 1 1 d . . . C702 C -0.2409(7) 0.2309(3) 0.2575(6) 0.056(3) Uani 1 1 d . . . C703 C -0.2789(8) 0.2389(4) 0.3284(8) 0.071(3) Uani 1 1 d . . . C704 C -0.2363(11) 0.2264(5) 0.4068(8) 0.093(5) Uani 1 1 d . . . C705 C -0.1591(11) 0.2078(5) 0.4182(8) 0.083(5) Uani 1 1 d . . . C706 C -0.1204(8) 0.2000(4) 0.3492(7) 0.065(3) Uani 1 1 d . . . C801 C 0.3319(6) 0.3802(3) 0.1578(6) 0.053(2) Uani 1 1 d . . . C802 C 0.2557(6) 0.3586(3) 0.1544(6) 0.053(2) Uani 1 1 d . . . C803 C 0.1985(8) 0.3535(4) 0.0775(7) 0.068(3) Uani 1 1 d . . . C804 C 0.2177(9) 0.3704(4) 0.0050(7) 0.082(4) Uani 1 1 d . . . C805 C 0.2960(8) 0.3924(4) 0.0099(7) 0.070(3) Uani 1 1 d . . . C806 C 0.3527(8) 0.3966(3) 0.0850(7) 0.061(3) 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 0.0473(2) 0.0512(2) 0.03946(19) 0.00156(17) 0.00216(16) 0.00151(18) Os2 0.0603(3) 0.0516(3) 0.0522(2) 0.00809(19) 0.00494(19) -0.0002(2) Os3 0.0467(2) 0.0656(3) 0.0592(3) 0.0080(2) 0.00295(19) -0.0012(2) Os4 0.0482(2) 0.0463(2) 0.0491(2) 0.00205(18) 0.00709(17) -0.00323(18) Os5 0.0453(2) 0.0595(3) 0.0666(3) 0.0024(2) 0.00535(19) 0.0003(2) Os6 0.0558(2) 0.0480(2) 0.0588(2) 0.00774(19) 0.01126(19) 0.00158(19) Cl1 0.36(7) 0.32(6) 0.50(10) -0.22(7) 0.02(6) 0.07(6) P1 0.0484(14) 0.0488(15) 0.0368(12) -0.0012(11) 0.0055(10) 0.0018(11) P2 0.0506(15) 0.0535(16) 0.0451(14) 0.0010(12) 0.0050(11) 0.0002(12) P3 0.0481(15) 0.0563(17) 0.0701(18) -0.0023(14) 0.0136(13) 0.0047(13) P4 0.0505(15) 0.0473(15) 0.0469(14) -0.0008(11) 0.0104(11) -0.0039(12) P5 0.0594(16) 0.0513(16) 0.0465(14) 0.0013(12) 0.0131(12) -0.0038(13) P6 0.0532(16) 0.0549(17) 0.0555(16) 0.0012(13) 0.0080(12) -0.0116(13) O11 0.097(6) 0.092(6) 0.056(5) -0.023(4) -0.003(4) 0.026(5) O12 0.080(5) 0.075(6) 0.053(4) -0.014(4) -0.002(4) 0.005(4) O13 0.076(5) 0.084(6) 0.076(6) 0.026(5) 0.006(4) -0.016(5) O21 0.121(8) 0.081(6) 0.062(5) 0.000(5) 0.011(5) 0.004(5) O22 0.108(8) 0.097(8) 0.124(9) 0.021(6) -0.015(6) 0.033(6) O23 0.078(6) 0.102(7) 0.087(6) 0.035(5) 0.012(5) -0.016(5) O24 0.160(10) 0.080(7) 0.091(7) -0.011(6) 0.011(7) -0.029(7) O31 0.109(8) 0.139(9) 0.077(6) 0.040(6) 0.004(5) -0.042(7) O32 0.078(6) 0.089(6) 0.071(6) -0.012(5) -0.017(4) -0.016(5) O33 0.071(6) 0.119(8) 0.153(10) 0.031(7) -0.002(6) 0.035(6) O34 0.108(8) 0.125(9) 0.114(8) -0.044(7) 0.034(7) 0.006(7) O41 0.085(6) 0.072(6) 0.101(7) 0.034(5) 0.013(5) 0.008(5) O42 0.109(7) 0.109(7) 0.060(5) -0.027(5) 0.019(5) -0.034(6) O43 0.080(6) 0.090(6) 0.084(6) -0.037(5) 0.024(5) -0.009(5) O51 0.077(7) 0.136(10) 0.175(12) 0.036(8) 0.018(7) -0.018(7) O52 0.067(5) 0.110(8) 0.097(7) -0.031(6) 0.015(5) 0.004(5) O53 0.107(8) 0.137(9) 0.120(9) 0.048(8) -0.007(7) 0.037(7) O54 0.093(7) 0.148(10) 0.124(9) -0.067(8) 0.004(6) -0.016(7) O61 0.102(8) 0.106(8) 0.150(10) 0.037(7) 0.050(7) -0.021(6) O62 0.161(10) 0.100(7) 0.050(5) -0.008(5) 0.004(6) 0.025(6) O63 0.077(6) 0.105(8) 0.158(10) 0.041(7) 0.004(6) 0.032(6) O64 0.215(13) 0.079(7) 0.102(8) -0.020(6) 0.042(8) 0.036(8) C1 0.09(4) 0.07(4) 0.17(6) 0.01(4) 0.00(4) 0.07(3) C2 0.02(2) 0.05(3) 0.28(9) -0.05(4) 0.01(4) 0.02(2) C3 0.03(2) 0.04(3) 0.13(4) -0.05(3) -0.03(3) 0.05(2) C4 0.33(13) 0.09(6) 0.23(10) -0.08(6) -0.15(9) 0.15(8) C11 0.055(6) 0.060(7) 0.055(6) 0.000(5) 0.005(5) 0.012(5) C12 0.056(6) 0.044(6) 0.052(6) -0.004(5) 0.005(5) 0.007(5) C13 0.045(6) 0.072(8) 0.050(6) 0.007(5) 0.004(5) -0.005(5) C21 0.075(8) 0.063(8) 0.055(7) 0.018(6) 0.008(6) 0.015(6) C22 0.078(8) 0.064(8) 0.081(9) 0.010(6) 0.009(7) 0.014(7) C23 0.077(8) 0.058(7) 0.049(6) 0.015(5) -0.006(5) -0.010(6) C24 0.114(11) 0.065(9) 0.070(8) 0.001(7) 0.026(8) -0.024(8) C31 0.065(7) 0.086(9) 0.061(7) 0.007(7) 0.010(6) 0.003(7) C32 0.057(7) 0.063(8) 0.065(7) 0.014(6) -0.005(6) 0.005(6) C33 0.060(8) 0.084(9) 0.099(10) 0.019(8) 0.016(7) 0.004(7) C34 0.064(8) 0.084(10) 0.092(10) -0.001(8) 0.012(7) 0.015(7) C41 0.072(8) 0.052(7) 0.074(8) 0.003(6) 0.012(6) -0.001(6) C42 0.055(6) 0.051(7) 0.073(8) -0.002(6) 0.007(6) -0.014(5) C43 0.069(7) 0.039(6) 0.067(7) -0.001(5) 0.021(6) 0.002(5) C51 0.065(8) 0.079(9) 0.106(11) 0.018(8) -0.003(7) -0.019(7) C52 0.054(7) 0.059(8) 0.087(9) 0.005(6) 0.016(6) 0.005(6) C53 0.064(8) 0.095(10) 0.072(8) 0.014(7) 0.007(6) 0.013(7) C54 0.072(8) 0.081(10) 0.098(10) -0.023(8) 0.006(8) 0.005(7) C61 0.077(8) 0.066(8) 0.080(8) 0.007(6) 0.023(7) 0.004(7) C62 0.086(8) 0.045(7) 0.060(7) 0.010(5) 0.006(6) 0.008(6) C63 0.092(10) 0.063(8) 0.091(9) 0.027(7) 0.024(8) 0.004(7) C64 0.089(9) 0.048(7) 0.091(10) 0.011(7) 0.024(8) 0.008(6) C101 0.040(5) 0.047(6) 0.054(6) 0.000(5) 0.011(4) 0.001(4) C102 0.065(7) 0.067(8) 0.054(6) 0.008(6) -0.004(6) 0.004(6) C103 0.086(9) 0.056(9) 0.109(12) 0.023(8) 0.003(8) -0.007(7) C104 0.084(10) 0.069(9) 0.109(12) -0.002(9) -0.012(9) -0.007(8) C105 0.081(9) 0.079(11) 0.083(11) -0.013(8) -0.008(8) -0.003(8) C106 0.086(9) 0.046(7) 0.062(7) -0.014(5) 0.014(6) 0.000(6) C201 0.049(6) 0.045(6) 0.057(6) 0.002(5) 0.013(5) 0.008(4) C202 0.052(6) 0.074(8) 0.061(7) 0.014(6) 0.011(5) 0.000(6) C203 0.075(8) 0.063(8) 0.079(9) 0.010(7) 0.010(7) -0.015(6) C204 0.072(8) 0.062(8) 0.106(11) 0.013(8) 0.012(8) -0.010(6) C205 0.053(7) 0.061(8) 0.076(9) -0.008(7) 0.002(6) -0.006(6) C206 0.060(7) 0.061(8) 0.056(6) -0.002(5) 0.007(5) 0.005(6) C301 0.057(6) 0.067(8) 0.055(6) -0.005(5) 0.014(5) -0.006(6) C302 0.064(8) 0.057(7) 0.073(8) -0.005(6) 0.014(6) -0.002(6) C303 0.084(9) 0.069(9) 0.076(9) -0.004(7) 0.015(7) -0.020(7) C304 0.084(9) 0.080(10) 0.074(9) -0.009(7) 0.010(7) -0.022(7) C305 0.077(10) 0.115(13) 0.074(10) -0.001(9) 0.005(8) -0.016(10) C306 0.073(8) 0.078(9) 0.075(8) -0.009(7) 0.013(7) -0.009(7) C401 0.070(7) 0.040(6) 0.067(7) 0.005(5) 0.026(6) 0.003(5) C402 0.096(9) 0.050(7) 0.072(8) -0.016(6) 0.037(7) -0.014(6) C403 0.144(14) 0.070(10) 0.096(11) -0.024(8) 0.047(10) -0.013(10) C404 0.138(15) 0.060(11) 0.19(2) -0.028(12) 0.087(16) 0.001(10) C405 0.126(13) 0.058(10) 0.148(16) 0.006(10) 0.062(12) 0.022(9) C406 0.078(8) 0.057(9) 0.113(13) 0.019(8) 0.036(9) 0.006(7) C501 0.043(5) 0.056(6) 0.043(5) -0.006(5) 0.000(4) -0.009(5) C502 0.059(7) 0.071(9) 0.055(7) -0.001(6) 0.010(6) -0.002(6) C503 0.064(7) 0.072(9) 0.068(8) 0.001(6) 0.013(6) 0.004(6) C504 0.065(7) 0.067(8) 0.065(7) 0.002(6) 0.014(6) 0.005(6) C505 0.083(8) 0.066(9) 0.064(8) 0.005(6) 0.013(6) 0.004(7) C506 0.069(7) 0.056(7) 0.051(6) 0.004(5) 0.013(6) 0.004(6) C601 0.051(6) 0.067(8) 0.061(7) -0.002(6) 0.008(5) -0.007(5) C602 0.052(7) 0.107(11) 0.072(8) -0.006(8) 0.017(6) -0.007(7) C603 0.085(11) 0.130(17) 0.076(10) 0.002(10) 0.020(8) -0.001(11) C604 0.073(10) 0.150(18) 0.130(16) -0.061(14) 0.029(10) 0.001(11) C605 0.085(10) 0.076(10) 0.111(12) 0.002(9) 0.020(9) 0.010(8) C606 0.067(8) 0.066(8) 0.089(10) -0.007(7) 0.019(7) 0.005(7) C701 0.054(6) 0.051(6) 0.039(5) -0.004(4) 0.005(4) -0.003(5) C702 0.065(7) 0.065(7) 0.046(6) -0.012(5) 0.027(5) -0.004(6) C703 0.081(8) 0.065(8) 0.071(8) -0.025(6) 0.027(7) -0.020(6) C704 0.107(12) 0.127(13) 0.053(8) -0.033(8) 0.036(8) -0.032(10) C705 0.095(12) 0.103(12) 0.054(8) -0.016(7) 0.018(7) -0.024(9) C706 0.083(8) 0.071(8) 0.041(6) -0.005(5) 0.014(6) -0.018(6) C801 0.058(6) 0.056(6) 0.044(5) 0.002(5) 0.009(5) -0.003(5) C802 0.055(6) 0.050(6) 0.051(6) 0.001(5) 0.006(5) -0.001(5) C803 0.063(7) 0.077(8) 0.060(7) -0.002(6) 0.006(6) 0.001(6) C804 0.086(9) 0.106(11) 0.043(6) 0.002(7) -0.009(6) 0.005(8) C805 0.066(7) 0.088(9) 0.053(7) 0.006(6) 0.007(6) -0.004(7) C806 0.073(7) 0.058(7) 0.053(6) 0.003(5) 0.010(6) -0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C13 1.866(11) . ? Os1 C12 1.929(10) . ? Os1 C11 1.941(11) . ? Os1 P1 2.349(3) . ? Os1 Os3 2.8742(8) . ? Os1 Os2 2.9103(7) . ? Os2 C23 1.890(13) . ? Os2 C22 1.897(12) . ? Os2 C21 1.936(13) . ? Os2 C24 1.955(14) . ? Os2 Os3 2.8891(8) . ? Os3 C33 1.911(13) . ? Os3 C31 1.914(13) . ? Os3 C34 1.948(15) . ? Os3 C32 1.956(13) . ? Os4 C41 1.890(12) . ? Os4 C42 1.934(12) . ? Os4 C43 1.936(11) . ? Os4 P4 2.350(3) . ? Os4 Os5 2.8769(8) . ? Os4 Os6 2.9230(7) . ? Os5 C51 1.871(14) . ? Os5 C53 1.899(13) . ? Os5 C52 1.947(14) . ? Os5 C54 1.945(15) . ? Os5 Os6 2.8888(9) . ? Os6 C61 1.884(13) . ? Os6 C63 1.928(14) . ? Os6 C62 1.936(12) . ? Os6 C64 1.974(14) . ? Cl1 C4 1.71(10) . ? Cl1 C4 1.81(15) 3_656 ? P1 C101 1.824(10) . ? P1 C701 1.844(10) . ? P1 P2 2.213(4) . ? P2 C201 1.841(10) . ? P2 P3 2.194(4) . ? P3 C702 1.824(11) . ? P3 C301 1.836(11) . ? P4 C801 1.846(10) . ? P4 C401 1.845(10) . ? P4 P5 2.213(4) . ? P5 C501 1.835(10) . ? P5 P6 2.200(4) . ? P6 C802 1.840(10) . ? P6 C601 1.846(12) . ? O11 C11 1.139(12) . ? O12 C12 1.133(11) . ? O13 C13 1.147(11) . ? O21 C21 1.135(13) . ? O22 C22 1.140(13) . ? O23 C23 1.156(13) . ? O24 C24 1.144(14) . ? O31 C31 1.137(13) . ? O32 C32 1.121(13) . ? O33 C33 1.137(13) . ? O34 C34 1.142(15) . ? O41 C41 1.141(13) . ? O42 C42 1.151(12) . ? O43 C43 1.143(12) . ? O51 C51 1.158(14) . ? O52 C52 1.137(13) . ? O53 C53 1.133(14) . ? O54 C54 1.124(14) . ? O61 C61 1.148(13) . ? O62 C62 1.130(13) . ? O63 C63 1.136(14) . ? O64 C64 1.120(14) . ? C1 C2 1.27(5) . ? C2 C3 1.27(5) . ? C3 C3 1.35(10) 3_766 ? C4 Cl1 1.81(15) 3_656 ? C101 C106 1.392(14) . ? C101 C102 1.393(14) . ? C102 C103 1.395(17) . ? C103 C104 1.37(2) . ? C104 C105 1.37(3) . ? C105 C106 1.36(2) . ? C201 C206 1.402(14) . ? C201 C202 1.400(14) . ? C202 C203 1.398(15) . ? C203 C204 1.360(18) . ? C204 C205 1.37(2) . ? C205 C206 1.39(2) . ? C301 C302 1.363(16) . ? C301 C306 1.410(16) . ? C302 C303 1.356(16) . ? C303 C304 1.362(18) . ? C304 C305 1.38(2) . ? C305 C306 1.39(2) . ? C401 C406 1.41(2) . ? C401 C402 1.391(15) . ? C402 C403 1.392(17) . ? C403 C404 1.39(3) . ? C404 C405 1.37(3) . ? C405 C406 1.38(2) . ? C501 C502 1.387(15) . ? C501 C506 1.381(14) . ? C502 C503 1.370(19) . ? C503 C504 1.396(16) . ? C504 C505 1.407(17) . ? C505 C506 1.351(16) . ? C601 C606 1.358(16) . ? C601 C602 1.380(16) . ? C602 C603 1.36(2) . ? C603 C604 1.34(2) . ? C604 C605 1.37(2) . ? C605 C606 1.361(19) . ? C701 C702 1.365(13) . ? C701 C706 1.395(14) . ? C702 C703 1.427(14) . ? C703 C704 1.381(19) . ? C704 C705 1.34(2) . ? C705 C706 1.406(18) . ? C801 C802 1.390(13) . ? C801 C806 1.399(14) . ? C802 C803 1.401(14) . ? C803 C804 1.391(16) . ? C804 C805 1.423(17) . ? C805 C806 1.372(15) . ? 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 C13 Os1 C12 88.7(4) . . ? C13 Os1 C11 90.3(5) . . ? C12 Os1 C11 178.6(4) . . ? C13 Os1 P1 103.7(3) . . ? C12 Os1 P1 88.7(3) . . ? C11 Os1 P1 90.6(3) . . ? C13 Os1 Os3 91.9(3) . . ? C12 Os1 Os3 94.3(3) . . ? C11 Os1 Os3 86.7(3) . . ? P1 Os1 Os3 164.13(6) . . ? C13 Os1 Os2 151.7(3) . . ? C12 Os1 Os2 90.9(3) . . ? C11 Os1 Os2 90.5(3) . . ? P1 Os1 Os2 104.51(7) . . ? Os3 Os1 Os2 59.92(2) . . ? C23 Os2 C22 98.7(5) . . ? C23 Os2 C21 90.6(5) . . ? C22 Os2 C21 91.1(5) . . ? C23 Os2 C24 89.1(5) . . ? C22 Os2 C24 95.3(6) . . ? C21 Os2 C24 173.5(5) . . ? C23 Os2 Os3 168.3(3) . . ? C22 Os2 Os3 93.0(4) . . ? C21 Os2 Os3 89.6(3) . . ? C24 Os2 Os3 89.3(4) . . ? C23 Os2 Os1 108.9(3) . . ? C22 Os2 Os1 152.3(4) . . ? C21 Os2 Os1 87.8(3) . . ? C24 Os2 Os1 86.2(4) . . ? Os3 Os2 Os1 59.419(19) . . ? C33 Os3 C31 102.3(5) . . ? C33 Os3 C34 90.0(6) . . ? C31 Os3 C34 90.9(6) . . ? C33 Os3 C32 92.1(5) . . ? C31 Os3 C32 90.2(5) . . ? C34 Os3 C32 177.4(5) . . ? C33 Os3 Os1 159.6(4) . . ? C31 Os3 Os1 97.8(3) . . ? C34 Os3 Os1 93.2(4) . . ? C32 Os3 Os1 84.3(3) . . ? C33 Os3 Os2 99.4(4) . . ? C31 Os3 Os2 158.3(3) . . ? C34 Os3 Os2 88.2(4) . . ? C32 Os3 Os2 90.0(3) . . ? Os1 Os3 Os2 60.66(2) . . ? C41 Os4 C42 88.3(5) . . ? C41 Os4 C43 91.7(5) . . ? C42 Os4 C43 178.4(4) . . ? C41 Os4 P4 101.3(4) . . ? C42 Os4 P4 88.7(3) . . ? C43 Os4 P4 89.7(3) . . ? C41 Os4 Os5 93.9(3) . . ? C42 Os4 Os5 89.6(3) . . ? C43 Os4 Os5 91.9(3) . . ? P4 Os4 Os5 164.70(7) . . ? C41 Os4 Os6 153.6(3) . . ? C42 Os4 Os6 89.9(3) . . ? C43 Os4 Os6 90.7(3) . . ? P4 Os4 Os6 105.04(7) . . ? Os5 Os4 Os6 59.74(2) . . ? C51 Os5 C53 102.8(6) . . ? C51 Os5 C52 89.6(6) . . ? C53 Os5 C52 89.3(5) . . ? C51 Os5 C54 91.4(6) . . ? C53 Os5 C54 92.6(6) . . ? C52 Os5 C54 177.7(5) . . ? C51 Os5 Os4 159.5(4) . . ? C53 Os5 Os4 97.6(4) . . ? C52 Os5 Os4 88.9(3) . . ? C54 Os5 Os4 89.5(4) . . ? C51 Os5 Os6 98.6(4) . . ? C53 Os5 Os6 158.5(4) . . ? C52 Os5 Os6 89.6(3) . . ? C54 Os5 Os6 88.2(4) . . ? Os4 Os5 Os6 60.92(2) . . ? C61 Os6 C63 98.1(5) . . ? C61 Os6 C62 93.1(5) . . ? C63 Os6 C62 89.6(5) . . ? C61 Os6 C64 93.5(5) . . ? C63 Os6 C64 89.5(6) . . ? C62 Os6 C64 173.4(5) . . ? C61 Os6 Os5 92.0(4) . . ? C63 Os6 Os5 169.7(4) . . ? C62 Os6 Os5 88.5(3) . . ? C64 Os6 Os5 91.3(4) . . ? C61 Os6 Os4 151.3(4) . . ? C63 Os6 Os4 110.5(4) . . ? C62 Os6 Os4 87.9(3) . . ? C64 Os6 Os4 86.3(3) . . ? Os5 Os6 Os4 59.338(18) . . ? C4 Cl1 C4 67(7) . 3_656 ? C101 P1 C701 101.3(4) . . ? C101 P1 P2 99.2(3) . . ? C701 P1 P2 99.2(3) . . ? C101 P1 Os1 116.3(3) . . ? C701 P1 Os1 120.4(3) . . ? P2 P1 Os1 116.87(13) . . ? C201 P2 P3 97.7(3) . . ? C201 P2 P1 103.5(3) . . ? P3 P2 P1 95.75(14) . . ? C702 P3 C301 104.3(5) . . ? C702 P3 P2 99.3(3) . . ? C301 P3 P2 102.7(3) . . ? C801 P4 C401 103.4(5) . . ? C801 P4 P5 99.8(3) . . ? C401 P4 P5 99.0(3) . . ? C801 P4 Os4 119.6(3) . . ? C401 P4 Os4 114.2(4) . . ? P5 P4 Os4 117.69(13) . . ? C501 P5 P6 98.7(3) . . ? C501 P5 P4 103.1(3) . . ? P6 P5 P4 96.24(14) . . ? C802 P6 C601 103.0(5) . . ? C802 P6 P5 99.2(3) . . ? C601 P6 P5 100.0(3) . . ? C1 C2 C3 120(5) . . ? C2 C3 C3 113(5) . 3_766 ? Cl1 C4 Cl1 113(7) . 3_656 ? O11 C11 Os1 173.8(10) . . ? O12 C12 Os1 175.1(9) . . ? O13 C13 Os1 176.3(9) . . ? O21 C21 Os2 174.9(10) . . ? O22 C22 Os2 178.5(13) . . ? O23 C23 Os2 177.0(10) . . ? O24 C24 Os2 175.1(11) . . ? O31 C31 Os3 176.6(12) . . ? O32 C32 Os3 174.7(11) . . ? O33 C33 Os3 178.8(14) . . ? O34 C34 Os3 172.5(13) . . ? O41 C41 Os4 173.7(11) . . ? O42 C42 Os4 174.8(10) . . ? O43 C43 Os4 174.3(10) . . ? O51 C51 Os5 178.9(14) . . ? O52 C52 Os5 177.7(11) . . ? O53 C53 Os5 175.8(14) . . ? O54 C54 Os5 174.1(13) . . ? O61 C61 Os6 178.5(12) . . ? O62 C62 Os6 175.3(10) . . ? O63 C63 Os6 176.8(12) . . ? O64 C64 Os6 175.2(11) . . ? C106 C101 C102 117.8(10) . . ? C106 C101 P1 120.8(8) . . ? C102 C101 P1 121.3(8) . . ? C103 C102 C101 121.3(12) . . ? C104 C103 C102 118.8(13) . . ? C105 C104 C103 120.4(14) . . ? C106 C105 C104 121.4(14) . . ? C105 C106 C101 120.2(12) . . ? C206 C201 C202 119.0(10) . . ? C206 C201 P2 125.4(8) . . ? C202 C201 P2 115.5(8) . . ? C203 C202 C201 120.6(11) . . ? C204 C203 C202 118.9(12) . . ? C203 C204 C205 121.8(13) . . ? C206 C205 C204 120.3(13) . . ? C205 C206 C201 119.4(10) . . ? C302 C301 C306 119.2(11) . . ? C302 C301 P3 125.5(9) . . ? C306 C301 P3 115.1(9) . . ? C301 C302 C303 122.3(12) . . ? C304 C303 C302 120.2(13) . . ? C303 C304 C305 118.7(13) . . ? C304 C305 C306 122.3(14) . . ? C305 C306 C301 117.2(13) . . ? C406 C401 C402 121.2(11) . . ? C406 C401 P4 120.3(10) . . ? C402 C401 P4 118.4(9) . . ? C401 C402 C403 120.2(13) . . ? C402 C403 C404 117.5(15) . . ? C405 C404 C403 122.4(15) . . ? C404 C405 C406 120.7(17) . . ? C405 C406 C401 117.8(17) . . ? C502 C501 C506 117.3(10) . . ? C502 C501 P5 125.6(9) . . ? C506 C501 P5 116.9(8) . . ? C503 C502 C501 122.2(11) . . ? C502 C503 C504 119.7(11) . . ? C505 C504 C503 118.1(11) . . ? C506 C505 C504 120.5(11) . . ? C505 C506 C501 122.2(10) . . ? C606 C601 C602 120.0(12) . . ? C606 C601 P6 124.3(9) . . ? C602 C601 P6 115.6(10) . . ? C603 C602 C601 119.7(13) . . ? C602 C603 C604 120.4(15) . . ? C603 C604 C605 119.8(16) . . ? C606 C605 C604 120.6(15) . . ? C601 C606 C605 119.4(13) . . ? C702 C701 C706 120.7(9) . . ? C702 C701 P1 119.0(7) . . ? C706 C701 P1 120.1(8) . . ? C701 C702 C703 119.0(10) . . ? C701 C702 P3 123.1(7) . . ? C703 C702 P3 117.7(9) . . ? C704 C703 C702 119.2(13) . . ? C705 C704 C703 121.6(12) . . ? C704 C705 C706 119.9(13) . . ? C705 C706 C701 119.5(12) . . ? C802 C801 C806 120.8(9) . . ? C802 C801 P4 118.8(7) . . ? C806 C801 P4 120.4(8) . . ? C801 C802 C803 119.7(9) . . ? C801 C802 P6 122.8(7) . . ? C803 C802 P6 117.3(8) . . ? C804 C803 C802 120.0(11) . . ? C803 C804 C805 119.3(11) . . ? C806 C805 C804 120.5(11) . . ? C805 C806 C801 119.7(11) . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 29.43 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 1.172 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.167 #============================================ data_2 _database_code_CSD 158407 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H21 Cl2 O22 Os6 P3' _chemical_formula_weight 2242.65 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' 'Os' 'Os' -1.2165 7.6030 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.9581(2) _cell_length_b 12.7231(2) _cell_length_c 26.7882(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.2830(10) _cell_angle_gamma 90.00 _cell_volume 5745.09(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15480 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not measured _exptl_crystal_density_diffrn 2.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4056 _exptl_absorpt_coefficient_mu 13.469 _exptl_absorpt_correction_type sadabs (Sheldrick) _exptl_absorpt_correction_T_min 0.082178 _exptl_absorpt_correction_T_max 0.261039 _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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36954 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 29.39 _reflns_number_total 14253 _reflns_number_gt 9477 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _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^)+(0.0342P)^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 SHELXL _refine_ls_extinction_coef 0.000062(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 14253 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.250 _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 0.22385(2) -0.66257(3) 0.008929(12) 0.04384(10) Uani 1 1 d . . . C11 C 0.2919(6) -0.7142(8) -0.0391(3) 0.055(3) Uani 1 1 d . . . O11 O 0.3347(5) -0.7374(7) -0.0675(3) 0.086(3) Uani 1 1 d . . . C12 C 0.1547(6) -0.6096(9) 0.0554(4) 0.061(3) Uani 1 1 d . . . O12 O 0.1161(5) -0.5707(7) 0.0832(3) 0.092(3) Uani 1 1 d . . . C13 C 0.2232(6) -0.5312(9) -0.0227(4) 0.067(3) Uani 1 1 d . . . O13 O 0.2180(6) -0.4500(7) -0.0431(3) 0.107(3) Uani 1 1 d . . . Os2 Os 0.09668(3) -0.74946(4) -0.058568(14) 0.06302(14) Uani 1 1 d . . . C21 C 0.0897(9) -0.6436(13) -0.1075(5) 0.113(6) Uani 1 1 d . . . O21 O 0.0862(8) -0.5797(11) -0.1388(4) 0.180(7) Uani 1 1 d . . . C22 C 0.0289(9) -0.6706(12) -0.0200(5) 0.095(5) Uani 1 1 d . . . O22 O -0.0171(6) -0.6243(9) 0.0006(4) 0.119(4) Uani 1 1 d . . . C23 C 0.1665(8) -0.8264(13) -0.0948(4) 0.091(5) Uani 1 1 d . . . C24 C 0.0124(7) -0.8367(11) -0.0841(4) 0.081(4) Uani 1 1 d . . . O23 O 0.2082(6) -0.8746(9) -0.1194(3) 0.111(3) Uani 1 1 d . . . O24 O -0.0402(6) -0.8879(9) -0.0991(3) 0.116(4) Uani 1 1 d . . . Os3 Os 0.16416(2) -0.87289(3) 0.025729(13) 0.04614(10) Uani 1 1 d . . . C31 C 0.0801(7) -0.8112(8) 0.0608(4) 0.059(3) Uani 1 1 d . . . O31 O 0.0320(5) -0.7819(7) 0.0830(3) 0.082(2) Uani 1 1 d . . . C32 C 0.2077(6) -0.9322(9) 0.0875(4) 0.062(3) Uani 1 1 d . . . O32 O 0.2303(5) -0.9748(7) 0.1245(3) 0.088(3) Uani 1 1 d . . . C33 C 0.1042(6) -0.9898(9) 0.0002(4) 0.060(3) Uani 1 1 d . . . O33 O 0.0726(4) -1.0659(7) -0.0153(3) 0.084(2) Uani 1 1 d . . . C34 C 0.2578(7) -0.9158(9) -0.0059(4) 0.061(3) Uani 1 1 d . . . O34 O 0.3121(5) -0.9500(7) -0.0215(3) 0.092(3) Uani 1 1 d . . . P1 P 0.33416(12) -0.65436(17) 0.06995(7) 0.0354(5) Uani 1 1 d . . . C101 C 0.4015(5) -0.7664(6) 0.0687(3) 0.0384(19) Uani 1 1 d . . . C102 C 0.3984(5) -0.8489(8) 0.1026(3) 0.050(2) Uani 1 1 d . . . H10A H 0.3639 -0.8448 0.1273 0.060 Uiso 1 1 calc R . . C103 C 0.4456(6) -0.9362(7) 0.1001(4) 0.059(3) Uani 1 1 d . . . H10B H 0.4421 -0.9912 0.1227 0.071 Uiso 1 1 calc R . . C104 C 0.4982(6) -0.9427(8) 0.0641(4) 0.066(3) Uani 1 1 d . . . H10C H 0.5312 -1.0009 0.0631 0.079 Uiso 1 1 calc R . . C105 C 0.5014(6) -0.8643(8) 0.0307(4) 0.060(3) Uani 1 1 d . . . H10D H 0.5356 -0.8700 0.0060 0.072 Uiso 1 1 calc R . . C106 C 0.4533(5) -0.7725(7) 0.0325(3) 0.050(2) Uani 1 1 d . . . H10E H 0.4568 -0.7180 0.0097 0.060 Uiso 1 1 calc R . . P2 P 0.41683(13) -0.52065(17) 0.06406(8) 0.0354(5) Uani 1 1 d . . . C201 C 0.3483(5) -0.4068(6) 0.0620(3) 0.041(2) Uani 1 1 d . . . C202 C 0.3594(6) -0.3322(9) 0.0250(4) 0.065(3) Uani 1 1 d . . . H20A H 0.3989 -0.3420 0.0040 0.078 Uiso 1 1 calc R . . C203 C 0.3121(9) -0.2448(9) 0.0198(5) 0.090(4) Uani 1 1 d . . . H20B H 0.3205 -0.1943 -0.0042 0.108 Uiso 1 1 calc R . . C204 C 0.2535(9) -0.2317(11) 0.0492(6) 0.099(5) Uani 1 1 d . . . H20C H 0.2217 -0.1721 0.0452 0.119 Uiso 1 1 calc R . . C205 C 0.2399(7) -0.3038(10) 0.0847(5) 0.086(4) Uani 1 1 d . . . H20D H 0.1983 -0.2948 0.1041 0.104 Uiso 1 1 calc R . . C206 C 0.2889(6) -0.3908(8) 0.0914(4) 0.061(3) Uani 1 1 d . . . H20E H 0.2811 -0.4390 0.1165 0.073 Uiso 1 1 calc R . . P3 P 0.46271(12) -0.52580(17) 0.14492(7) 0.0321(4) Uani 1 1 d . . . C301 C 0.5337(5) -0.6337(6) 0.1459(3) 0.041(2) Uani 1 1 d . . . C302 C 0.5920(5) -0.6318(8) 0.1127(3) 0.051(2) Uani 1 1 d . . . H30A H 0.5921 -0.5790 0.0887 0.061 Uiso 1 1 calc R . . C303 C 0.6504(6) -0.7105(9) 0.1161(4) 0.068(3) Uani 1 1 d . . . H30B H 0.6884 -0.7112 0.0936 0.082 Uiso 1 1 calc R . . C304 C 0.6515(6) -0.7854(9) 0.1520(5) 0.075(3) Uani 1 1 d . . . H30C H 0.6918 -0.8352 0.1548 0.090 Uiso 1 1 calc R . . C305 C 0.5940(6) -0.7893(8) 0.1844(4) 0.067(3) Uani 1 1 d . . . H30D H 0.5948 -0.8425 0.2083 0.081 Uiso 1 1 calc R . . C306 C 0.5348(5) -0.7134(7) 0.1814(3) 0.050(2) Uani 1 1 d . . . H30E H 0.4958 -0.7160 0.2032 0.060 Uiso 1 1 calc R . . C401 C 0.3217(5) -0.6439(7) 0.1370(3) 0.0378(19) Uani 1 1 d . . . C402 C 0.3762(4) -0.5880(6) 0.1694(3) 0.0312(17) Uani 1 1 d . . . C403 C 0.3665(5) -0.5818(8) 0.2201(3) 0.048(2) Uani 1 1 d . . . H40A H 0.4032 -0.5448 0.2417 0.058 Uiso 1 1 calc R . . C404 C 0.3034(6) -0.6297(8) 0.2388(4) 0.057(3) Uani 1 1 d . . . H40B H 0.2973 -0.6244 0.2728 0.069 Uiso 1 1 calc R . . C405 C 0.2491(5) -0.6857(8) 0.2072(4) 0.056(3) Uani 1 1 d . . . H40C H 0.2064 -0.7183 0.2199 0.067 Uiso 1 1 calc R . . C406 C 0.2579(5) -0.6936(7) 0.1561(3) 0.046(2) Uani 1 1 d . . . H40D H 0.2215 -0.7319 0.1348 0.055 Uiso 1 1 calc R . . Os4 Os 0.517295(18) -0.37031(3) 0.181124(11) 0.03375(8) Uani 1 1 d . . . C41 C 0.5013(5) -0.2762(7) 0.1277(3) 0.049(2) Uani 1 1 d . . . O41 O 0.4940(5) -0.2139(6) 0.0954(3) 0.085(2) Uani 1 1 d . . . C42 C 0.4158(5) -0.3333(7) 0.2008(3) 0.046(2) Uani 1 1 d . . . O42 O 0.3532(4) -0.3099(6) 0.2089(3) 0.073(2) Uani 1 1 d . . . C43 C 0.6210(5) -0.4067(7) 0.1619(3) 0.044(2) Uani 1 1 d . . . O43 O 0.6792(4) -0.4278(6) 0.1471(3) 0.068(2) Uani 1 1 d . . . Os5 Os 0.60127(2) -0.22106(3) 0.247907(15) 0.04996(11) Uani 1 1 d . . . C51 C 0.7051(6) -0.2628(8) 0.2292(4) 0.055(2) Uani 1 1 d . . . O51 O 0.7656(5) -0.2833(7) 0.2186(3) 0.090(3) Uani 1 1 d . . . C52 C 0.4993(7) -0.1856(10) 0.2682(5) 0.087(4) Uani 1 1 d . . . O52 O 0.4415(6) -0.1538(10) 0.2814(6) 0.177(7) Uani 1 1 d . . . C53 C 0.6510(6) -0.1544(9) 0.3079(4) 0.065(3) Uani 1 1 d . . . O53 O 0.6794(5) -0.1143(8) 0.3429(3) 0.101(3) Uani 1 1 d . . . C54 C 0.6014(7) -0.1101(8) 0.2003(5) 0.079(4) Uani 1 1 d . . . O54 O 0.6021(7) -0.0446(8) 0.1710(4) 0.150(5) Uani 1 1 d . . . Os6 Os 0.57561(2) -0.42961(3) 0.284294(13) 0.04703(10) Uani 1 1 d . . . C61 C 0.6282(6) -0.3941(8) 0.3497(4) 0.058(3) Uani 1 1 d . . . O61 O 0.6576(5) -0.3758(8) 0.3882(3) 0.095(3) Uani 1 1 d . . . C62 C 0.6749(7) -0.4731(9) 0.2612(4) 0.072(3) Uani 1 1 d . . . O62 O 0.7324(6) -0.5057(8) 0.2495(4) 0.122(4) Uani 1 1 d . . . C63 C 0.4726(7) -0.3916(10) 0.3021(4) 0.071(3) Uani 1 1 d . . . O63 O 0.4107(5) -0.3737(9) 0.3140(3) 0.104(3) Uani 1 1 d . . . C64 C 0.5515(7) -0.5735(10) 0.2932(4) 0.067(3) Uani 1 1 d . . . O64 O 0.5389(6) -0.6605(7) 0.3006(3) 0.103(3) Uani 1 1 d . . . Cl1 Cl 0.4021(11) -0.8501(18) 0.3142(6) 0.543(13) Uani 1 1 d . . . C1 C 0.3383(17) -0.927(2) 0.2905(16) 0.33(2) Uani 1 1 d . . . H1A H 0.2856 -0.8970 0.2856 0.392 Uiso 1 1 calc R . . H1B H 0.3375 -0.9935 0.3086 0.392 Uiso 1 1 calc R . . Cl2 Cl 0.3886(14) -0.9383(13) 0.2287(4) 0.546(15) 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 0.0434(2) 0.0453(2) 0.04031(19) 0.00424(16) -0.00646(15) -0.01495(17) C11 0.064(6) 0.066(7) 0.033(5) 0.005(5) -0.005(5) -0.022(6) O11 0.083(6) 0.125(8) 0.054(4) -0.017(5) 0.027(4) -0.031(5) C12 0.048(6) 0.055(7) 0.076(7) 0.013(6) -0.015(5) -0.024(5) O12 0.065(5) 0.109(7) 0.103(6) -0.039(6) 0.016(5) 0.005(5) C13 0.071(7) 0.060(7) 0.065(7) 0.016(6) -0.022(5) -0.019(6) O13 0.137(8) 0.065(6) 0.105(7) 0.039(5) -0.048(6) -0.039(6) Os2 0.0627(3) 0.0749(3) 0.0462(2) 0.0095(2) -0.01809(19) -0.0280(2) C21 0.120(12) 0.111(12) 0.098(10) 0.048(9) -0.033(9) -0.044(10) O21 0.204(13) 0.177(13) 0.141(10) 0.085(10) -0.063(9) -0.090(11) C22 0.105(11) 0.089(11) 0.074(9) 0.012(8) -0.059(8) -0.013(9) O22 0.095(8) 0.119(9) 0.133(9) -0.016(7) -0.033(6) 0.021(7) C23 0.081(9) 0.151(14) 0.043(6) -0.022(8) 0.011(6) -0.044(9) C24 0.076(8) 0.121(11) 0.041(6) 0.009(6) -0.015(5) -0.044(8) O23 0.095(7) 0.158(10) 0.077(6) -0.031(6) -0.002(5) -0.027(7) O24 0.105(7) 0.156(10) 0.080(6) 0.003(6) -0.018(5) -0.074(7) Os3 0.0456(2) 0.0456(2) 0.0458(2) 0.00016(17) -0.00124(16) -0.01464(17) C31 0.070(7) 0.053(6) 0.055(6) 0.008(5) 0.004(5) -0.020(6) O31 0.077(5) 0.089(6) 0.086(6) -0.009(5) 0.031(5) -0.006(5) C32 0.057(6) 0.062(7) 0.065(7) 0.000(6) -0.007(5) -0.014(6) O32 0.088(6) 0.097(7) 0.074(5) 0.023(5) -0.015(4) -0.018(5) C33 0.051(6) 0.078(8) 0.052(6) -0.014(5) 0.010(5) -0.018(6) O33 0.071(5) 0.077(6) 0.103(6) -0.035(5) 0.008(4) -0.026(5) C34 0.063(7) 0.062(7) 0.057(6) 0.004(5) 0.003(5) -0.012(6) O34 0.062(5) 0.110(7) 0.108(7) -0.017(6) 0.025(5) -0.006(5) P1 0.0374(12) 0.0354(12) 0.0328(11) 0.0001(9) 0.0006(9) -0.0085(10) C101 0.040(5) 0.033(4) 0.041(5) -0.008(4) -0.001(4) -0.010(4) C102 0.051(6) 0.054(6) 0.043(5) 0.001(4) 0.003(4) -0.007(5) C103 0.080(7) 0.032(5) 0.063(6) 0.001(5) -0.005(6) 0.003(5) C104 0.062(7) 0.045(6) 0.087(8) -0.021(6) -0.011(6) 0.011(5) C105 0.059(6) 0.054(6) 0.069(7) -0.018(6) 0.013(5) 0.005(5) C106 0.058(6) 0.036(5) 0.055(6) 0.001(4) 0.000(5) -0.010(5) P2 0.0380(12) 0.0360(12) 0.0322(11) 0.0019(9) 0.0031(9) -0.0071(10) C201 0.042(5) 0.031(4) 0.047(5) 0.007(4) -0.012(4) -0.009(4) C202 0.070(7) 0.063(7) 0.058(6) 0.013(5) -0.014(5) 0.001(6) C203 0.112(11) 0.046(7) 0.102(10) 0.035(7) -0.026(9) -0.003(7) C204 0.103(11) 0.067(9) 0.122(12) 0.034(9) -0.017(9) 0.021(8) C205 0.077(8) 0.077(9) 0.103(10) 0.001(8) 0.001(7) 0.023(7) C206 0.070(7) 0.062(7) 0.052(6) 0.008(5) 0.012(5) 0.020(6) P3 0.0316(11) 0.0333(11) 0.0312(10) -0.0004(9) 0.0023(8) -0.0040(9) C301 0.035(4) 0.032(4) 0.053(5) -0.014(4) -0.005(4) -0.006(4) C302 0.038(5) 0.058(6) 0.055(5) -0.014(5) -0.001(4) -0.003(5) C303 0.050(6) 0.072(8) 0.082(8) -0.021(7) 0.003(6) 0.010(6) C304 0.048(6) 0.052(7) 0.119(10) -0.019(7) -0.017(7) 0.016(6) C305 0.059(7) 0.039(6) 0.097(8) 0.012(6) -0.022(6) 0.006(5) C306 0.047(5) 0.044(5) 0.059(6) 0.006(5) 0.001(5) -0.001(5) C401 0.038(4) 0.044(5) 0.033(4) 0.001(4) 0.005(3) -0.006(4) C402 0.031(4) 0.034(4) 0.029(4) -0.001(3) 0.008(3) -0.003(3) C403 0.050(5) 0.062(6) 0.033(4) -0.006(4) 0.006(4) -0.014(5) C404 0.053(6) 0.075(7) 0.046(5) 0.003(5) 0.016(5) -0.004(6) C405 0.039(5) 0.071(7) 0.059(6) 0.010(5) 0.012(5) -0.009(5) C406 0.040(5) 0.055(6) 0.042(5) -0.006(4) 0.005(4) -0.009(4) Os4 0.03260(17) 0.03229(17) 0.03583(17) -0.00349(14) 0.00131(13) -0.00239(14) C41 0.053(6) 0.035(5) 0.055(6) 0.002(4) -0.006(5) -0.004(4) O41 0.104(6) 0.063(5) 0.082(5) 0.028(4) -0.013(5) -0.011(5) C42 0.043(5) 0.052(6) 0.044(5) -0.018(4) 0.006(4) -0.002(5) O42 0.049(4) 0.095(6) 0.077(5) -0.034(4) 0.012(4) 0.004(4) C43 0.040(5) 0.042(5) 0.047(5) -0.006(4) -0.001(4) -0.004(4) O43 0.045(4) 0.079(5) 0.081(5) -0.019(4) 0.016(4) -0.003(4) Os5 0.0424(2) 0.0392(2) 0.0647(2) -0.01212(18) -0.01059(18) -0.00184(17) C51 0.057(6) 0.048(6) 0.056(6) -0.006(5) -0.008(5) -0.014(5) O51 0.047(4) 0.107(7) 0.116(7) -0.034(6) 0.011(5) -0.010(5) C52 0.062(8) 0.057(8) 0.140(11) -0.033(8) -0.002(8) -0.010(6) O52 0.059(6) 0.144(11) 0.329(18) -0.131(12) 0.028(8) 0.004(6) C53 0.058(6) 0.075(8) 0.060(7) -0.012(6) -0.001(5) 0.011(6) O53 0.081(6) 0.119(8) 0.095(6) -0.055(6) -0.025(5) 0.011(5) C54 0.083(8) 0.033(6) 0.109(10) -0.014(6) -0.039(7) -0.010(6) O54 0.191(11) 0.069(7) 0.171(11) 0.062(7) -0.067(8) -0.033(7) Os6 0.0484(2) 0.0545(2) 0.03727(19) 0.00066(17) 0.00047(16) -0.00086(19) C61 0.054(6) 0.065(7) 0.053(6) 0.003(5) -0.003(5) -0.003(5) O61 0.091(6) 0.132(8) 0.056(5) -0.013(5) -0.022(4) -0.027(6) C62 0.074(8) 0.072(8) 0.069(7) 0.029(6) 0.011(6) 0.018(7) O62 0.108(7) 0.142(9) 0.125(8) 0.057(7) 0.052(6) 0.086(7) C63 0.065(7) 0.107(10) 0.037(5) 0.002(6) -0.010(5) -0.032(7) O63 0.061(5) 0.181(11) 0.074(5) -0.010(6) 0.016(4) -0.009(6) C64 0.092(8) 0.063(8) 0.042(6) 0.008(5) -0.014(5) -0.005(7) O64 0.153(9) 0.073(6) 0.074(6) 0.010(5) -0.019(5) -0.031(6) Cl1 0.46(2) 0.71(4) 0.44(2) -0.03(2) -0.066(18) -0.20(2) C1 0.18(3) 0.19(3) 0.61(7) -0.03(4) 0.08(3) -0.13(2) Cl2 1.00(4) 0.43(2) 0.228(11) 0.132(13) 0.183(18) 0.24(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C13 1.873(11) . ? Os1 C11 1.935(11) . ? Os1 C12 1.924(13) . ? Os1 P1 2.348(2) . ? Os1 Os2 2.8790(5) . ? Os1 Os3 2.9133(5) . ? C11 O11 1.145(11) . ? C12 O12 1.155(12) . ? C13 O13 1.168(12) . ? Os2 C24 1.879(11) . ? Os2 C21 1.874(14) . ? Os2 C23 1.885(15) . ? Os2 C22 1.911(18) . ? Os2 Os3 2.8826(5) . ? C21 O21 1.165(14) . ? C22 O22 1.165(17) . ? C23 O23 1.190(15) . ? C24 O24 1.142(12) . ? Os3 C33 1.888(11) . ? Os3 C32 1.892(11) . ? Os3 C34 1.958(12) . ? Os3 C31 1.956(12) . ? C31 O31 1.125(12) . ? C32 O32 1.158(11) . ? C33 O33 1.161(11) . ? C34 O34 1.138(12) . ? P1 C101 1.829(9) . ? P1 C401 1.837(8) . ? P1 P2 2.221(3) . ? C101 C106 1.381(12) . ? C101 C102 1.393(12) . ? C102 C103 1.375(13) . ? C103 C104 1.387(14) . ? C104 C105 1.345(14) . ? C105 C106 1.428(13) . ? P2 C201 1.854(9) . ? P2 P3 2.221(3) . ? C201 C206 1.359(12) . ? C201 C202 1.401(12) . ? C202 C203 1.369(15) . ? C203 C204 1.344(18) . ? C204 C205 1.359(17) . ? C205 C206 1.384(14) . ? P3 C301 1.824(8) . ? P3 C402 1.848(7) . ? P3 Os4 2.348(2) . ? C301 C306 1.390(12) . ? C301 C302 1.400(12) . ? C302 C303 1.404(13) . ? C303 C304 1.352(15) . ? C304 C305 1.375(15) . ? C305 C306 1.389(13) . ? C401 C402 1.390(10) . ? C401 C406 1.397(11) . ? C402 C403 1.391(10) . ? C403 C404 1.373(12) . ? C404 C405 1.380(13) . ? C405 C406 1.397(11) . ? Os4 C41 1.864(9) . ? Os4 C42 1.912(9) . ? Os4 C43 1.942(9) . ? Os4 Os5 2.8769(5) . ? Os4 Os6 2.9304(5) . ? C41 O41 1.168(10) . ? C42 O42 1.146(10) . ? C43 O43 1.136(10) . ? Os5 C54 1.903(13) . ? Os5 C52 1.922(13) . ? Os5 C53 1.929(11) . ? Os5 C51 1.956(11) . ? Os5 Os6 2.8763(6) . ? C51 O51 1.124(11) . ? C52 O52 1.151(13) . ? C53 O53 1.127(11) . ? C54 O54 1.145(14) . ? Os6 C64 1.897(12) . ? Os6 C63 1.922(13) . ? Os6 C61 1.930(10) . ? Os6 C62 1.937(12) . ? C61 O61 1.120(10) . ? C62 O62 1.136(12) . ? C63 O63 1.154(13) . ? C64 O64 1.148(13) . ? Cl1 C1 1.55(3) . ? C1 Cl2 1.95(4) . ? 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 C13 Os1 C11 88.6(5) . . ? C13 Os1 C12 90.3(5) . . ? C11 Os1 C12 178.6(4) . . ? C13 Os1 P1 103.9(3) . . ? C11 Os1 P1 89.5(3) . . ? C12 Os1 P1 91.7(3) . . ? C13 Os1 Os2 95.3(3) . . ? C11 Os1 Os2 85.0(3) . . ? C12 Os1 Os2 94.2(3) . . ? P1 Os1 Os2 159.93(6) . . ? C13 Os1 Os3 154.8(3) . . ? C11 Os1 Os3 91.9(3) . . ? C12 Os1 Os3 88.6(3) . . ? P1 Os1 Os3 101.37(5) . . ? Os2 Os1 Os3 59.688(13) . . ? O11 C11 Os1 174.9(9) . . ? O12 C12 Os1 174.9(9) . . ? O13 C13 Os1 175.9(10) . . ? C24 Os2 C21 100.5(5) . . ? C24 Os2 C23 90.1(6) . . ? C21 Os2 C23 90.5(7) . . ? C24 Os2 C22 91.6(6) . . ? C21 Os2 C22 90.3(7) . . ? C23 Os2 C22 178.0(5) . . ? C24 Os2 Os1 160.6(3) . . ? C21 Os2 Os1 98.6(4) . . ? C23 Os2 Os1 93.0(3) . . ? C22 Os2 Os1 85.0(4) . . ? C24 Os2 Os3 100.6(4) . . ? C21 Os2 Os3 158.2(4) . . ? C23 Os2 Os3 84.4(4) . . ? C22 Os2 Os3 94.2(4) . . ? Os1 Os2 Os3 60.749(12) . . ? O21 C21 Os2 178.1(18) . . ? O22 C22 Os2 174.8(11) . . ? O23 C23 Os2 177.1(11) . . ? O24 C24 Os2 178.1(14) . . ? C33 Os3 C32 98.4(4) . . ? C33 Os3 C34 93.1(4) . . ? C32 Os3 C34 90.6(4) . . ? C33 Os3 C31 95.6(4) . . ? C32 Os3 C31 88.6(4) . . ? C34 Os3 C31 171.3(4) . . ? C33 Os3 Os2 89.6(3) . . ? C32 Os3 Os2 170.1(3) . . ? C34 Os3 Os2 94.8(3) . . ? C31 Os3 Os2 84.8(3) . . ? C33 Os3 Os1 148.3(3) . . ? C32 Os3 Os1 113.1(3) . . ? C34 Os3 Os1 83.0(3) . . ? C31 Os3 Os1 89.4(3) . . ? Os2 Os3 Os1 59.563(13) . . ? O31 C31 Os3 175.1(9) . . ? O32 C32 Os3 174.8(9) . . ? O33 C33 Os3 174.9(10) . . ? O34 C34 Os3 173.0(10) . . ? C101 P1 C401 102.3(4) . . ? C101 P1 P2 101.3(3) . . ? C401 P1 P2 98.9(3) . . ? C101 P1 Os1 113.8(3) . . ? C401 P1 Os1 121.1(3) . . ? P2 P1 Os1 116.46(10) . . ? C106 C101 C102 119.3(8) . . ? C106 C101 P1 120.2(7) . . ? C102 C101 P1 120.5(7) . . ? C103 C102 C101 120.9(9) . . ? C102 C103 C104 120.3(9) . . ? C105 C104 C103 119.6(10) . . ? C104 C105 C106 121.4(10) . . ? C101 C106 C105 118.6(9) . . ? C201 P2 P1 101.6(3) . . ? C201 P2 P3 101.7(3) . . ? P1 P2 P3 93.71(11) . . ? C206 C201 C202 118.3(9) . . ? C206 C201 P2 127.0(7) . . ? C202 C201 P2 114.7(8) . . ? C203 C202 C201 120.0(11) . . ? C204 C203 C202 120.2(12) . . ? C203 C204 C205 121.3(13) . . ? C204 C205 C206 119.1(13) . . ? C201 C206 C205 121.1(10) . . ? C301 P3 C402 102.8(4) . . ? C301 P3 P2 101.3(3) . . ? C402 P3 P2 98.7(2) . . ? C301 P3 Os4 113.5(3) . . ? C402 P3 Os4 120.5(3) . . ? P2 P3 Os4 117.26(11) . . ? C306 C301 C302 119.4(8) . . ? C306 C301 P3 121.2(7) . . ? C302 C301 P3 119.3(7) . . ? C303 C302 C301 119.2(10) . . ? C304 C303 C302 120.3(10) . . ? C303 C304 C305 121.3(10) . . ? C304 C305 C306 119.7(10) . . ? C305 C306 C301 120.2(9) . . ? C402 C401 C406 119.5(7) . . ? C402 C401 P1 120.4(6) . . ? C406 C401 P1 120.1(6) . . ? C403 C402 C401 119.8(7) . . ? C403 C402 P3 120.4(6) . . ? C401 C402 P3 119.8(5) . . ? C404 C403 C402 120.8(8) . . ? C403 C404 C405 120.0(8) . . ? C404 C405 C406 120.2(8) . . ? C405 C406 C401 119.7(8) . . ? C41 Os4 C42 89.6(4) . . ? C41 Os4 C43 90.6(4) . . ? C42 Os4 C43 179.2(4) . . ? C41 Os4 P3 101.9(3) . . ? C42 Os4 P3 89.7(3) . . ? C43 Os4 P3 91.0(3) . . ? C41 Os4 Os5 94.3(3) . . ? C42 Os4 Os5 93.7(3) . . ? C43 Os4 Os5 85.5(2) . . ? P3 Os4 Os5 163.49(5) . . ? C41 Os4 Os6 153.6(3) . . ? C42 Os4 Os6 91.4(3) . . ? C43 Os4 Os6 88.1(3) . . ? P3 Os4 Os6 104.46(5) . . ? Os5 Os4 Os6 59.368(13) . . ? O41 C41 Os4 176.6(8) . . ? O42 C42 Os4 174.9(8) . . ? O43 C43 Os4 174.8(8) . . ? C54 Os5 C52 94.7(6) . . ? C54 Os5 C53 101.6(5) . . ? C52 Os5 C53 89.2(5) . . ? C54 Os5 C51 87.8(5) . . ? C52 Os5 C51 177.5(5) . . ? C53 Os5 C51 90.5(4) . . ? C54 Os5 Os6 157.4(3) . . ? C52 Os5 Os6 87.0(4) . . ? C53 Os5 Os6 101.0(3) . . ? C51 Os5 Os6 90.6(3) . . ? C54 Os5 Os4 96.3(3) . . ? C52 Os5 Os4 86.1(3) . . ? C53 Os5 Os4 161.8(3) . . ? C51 Os5 Os4 93.4(3) . . ? Os6 Os5 Os4 61.242(12) . . ? O51 C51 Os5 177.7(9) . . ? O52 C52 Os5 172.7(11) . . ? O53 C53 Os5 179.1(11) . . ? O54 C54 Os5 178.7(13) . . ? C64 Os6 C63 89.8(5) . . ? C64 Os6 C61 101.3(4) . . ? C63 Os6 C61 93.3(4) . . ? C64 Os6 C62 88.4(5) . . ? C63 Os6 C62 175.1(5) . . ? C61 Os6 C62 91.5(4) . . ? C64 Os6 Os5 167.4(3) . . ? C63 Os6 Os5 91.6(4) . . ? C61 Os6 Os5 91.1(3) . . ? C62 Os6 Os5 89.2(3) . . ? C64 Os6 Os4 108.2(3) . . ? C63 Os6 Os4 87.0(3) . . ? C61 Os6 Os4 150.5(3) . . ? C62 Os6 Os4 89.3(3) . . ? Os5 Os6 Os4 59.390(12) . . ? O61 C61 Os6 178.1(10) . . ? O62 C62 Os6 174.7(10) . . ? O63 C63 Os6 176.5(12) . . ? O64 C64 Os6 177.1(10) . . ? Cl1 C1 Cl2 92.4(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Os1 C11 O11 35(10) . . . . ? C12 Os1 C11 O11 77(21) . . . . ? P1 Os1 C11 O11 -69(10) . . . . ? Os2 Os1 C11 O11 131(10) . . . . ? Os3 Os1 C11 O11 -170(10) . . . . ? C13 Os1 C12 O12 -34(11) . . . . ? C11 Os1 C12 O12 -76(21) . . . . ? P1 Os1 C12 O12 70(11) . . . . ? Os2 Os1 C12 O12 -130(11) . . . . ? Os3 Os1 C12 O12 171(11) . . . . ? C11 Os1 C13 O13 117(16) . . . . ? C12 Os1 C13 O13 -62(16) . . . . ? P1 Os1 C13 O13 -154(15) . . . . ? Os2 Os1 C13 O13 32(16) . . . . ? Os3 Os1 C13 O13 25(16) . . . . ? C13 Os1 Os2 C24 -159.5(13) . . . . ? C11 Os1 Os2 C24 112.3(13) . . . . ? C12 Os1 Os2 C24 -68.8(13) . . . . ? P1 Os1 Os2 C24 37.9(13) . . . . ? Os3 Os1 Os2 C24 17.1(13) . . . . ? C13 Os1 Os2 C21 10.6(7) . . . . ? C11 Os1 Os2 C21 -77.6(6) . . . . ? C12 Os1 Os2 C21 101.3(6) . . . . ? P1 Os1 Os2 C21 -152.0(6) . . . . ? Os3 Os1 Os2 C21 -172.8(6) . . . . ? C13 Os1 Os2 C23 101.5(6) . . . . ? C11 Os1 Os2 C23 13.4(5) . . . . ? C12 Os1 Os2 C23 -167.7(5) . . . . ? P1 Os1 Os2 C23 -61.0(5) . . . . ? Os3 Os1 Os2 C23 -81.8(4) . . . . ? C13 Os1 Os2 C22 -79.0(6) . . . . ? C11 Os1 Os2 C22 -167.1(5) . . . . ? C12 Os1 Os2 C22 11.8(5) . . . . ? P1 Os1 Os2 C22 118.5(4) . . . . ? Os3 Os1 Os2 C22 97.7(4) . . . . ? C13 Os1 Os2 Os3 -176.6(4) . . . . ? C11 Os1 Os2 Os3 95.2(3) . . . . ? C12 Os1 Os2 Os3 -85.9(3) . . . . ? P1 Os1 Os2 Os3 20.82(16) . . . . ? C24 Os2 C21 O21 -73(41) . . . . ? C23 Os2 C21 O21 18(41) . . . . ? C22 Os2 C21 O21 -164(41) . . . . ? Os1 Os2 C21 O21 111(41) . . . . ? Os3 Os2 C21 O21 94(41) . . . . ? C24 Os2 C22 O22 -31(16) . . . . ? C21 Os2 C22 O22 70(16) . . . . ? C23 Os2 C22 O22 -178(100) . . . . ? Os1 Os2 C22 O22 168(16) . . . . ? Os3 Os2 C22 O22 -131(16) . . . . ? C24 Os2 C23 O23 48(26) . . . . ? C21 Os2 C23 O23 -53(26) . . . . ? C22 Os2 C23 O23 -165(21) . . . . ? Os1 Os2 C23 O23 -151(26) . . . . ? Os3 Os2 C23 O23 149(26) . . . . ? C21 Os2 C24 O24 -78(33) . . . . ? C23 Os2 C24 O24 -169(100) . . . . ? C22 Os2 C24 O24 13(33) . . . . ? Os1 Os2 C24 O24 92(33) . . . . ? Os3 Os2 C24 O24 107(33) . . . . ? C24 Os2 Os3 C33 13.7(5) . . . . ? C21 Os2 Os3 C33 -152.4(15) . . . . ? C23 Os2 Os3 C33 -75.3(5) . . . . ? C22 Os2 Os3 C33 106.1(5) . . . . ? Os1 Os2 Os3 C33 -172.0(3) . . . . ? C24 Os2 Os3 C32 -130.4(18) . . . . ? C21 Os2 Os3 C32 63(2) . . . . ? C23 Os2 Os3 C32 140.6(18) . . . . ? C22 Os2 Os3 C32 -37.9(18) . . . . ? Os1 Os2 Os3 C32 43.9(18) . . . . ? C24 Os2 Os3 C34 106.8(5) . . . . ? C21 Os2 Os3 C34 -59.4(15) . . . . ? C23 Os2 Os3 C34 17.8(5) . . . . ? C22 Os2 Os3 C34 -160.8(5) . . . . ? Os1 Os2 Os3 C34 -78.9(3) . . . . ? C24 Os2 Os3 C31 -82.0(5) . . . . ? C21 Os2 Os3 C31 111.9(15) . . . . ? C23 Os2 Os3 C31 -171.0(5) . . . . ? C22 Os2 Os3 C31 10.5(5) . . . . ? Os1 Os2 Os3 C31 92.3(3) . . . . ? C24 Os2 Os3 Os1 -174.3(4) . . . . ? C21 Os2 Os3 Os1 19.5(15) . . . . ? C23 Os2 Os3 Os1 96.7(4) . . . . ? C22 Os2 Os3 Os1 -81.9(4) . . . . ? C13 Os1 Os3 C33 23.3(11) . . . . ? C11 Os1 Os3 C33 -67.6(6) . . . . ? C12 Os1 Os3 C33 111.1(6) . . . . ? P1 Os1 Os3 C33 -157.5(6) . . . . ? Os2 Os1 Os3 C33 15.4(6) . . . . ? C13 Os1 Os3 C32 -164.6(9) . . . . ? C11 Os1 Os3 C32 104.4(4) . . . . ? C12 Os1 Os3 C32 -76.8(5) . . . . ? P1 Os1 Os3 C32 14.6(4) . . . . ? Os2 Os1 Os3 C32 -172.6(4) . . . . ? C13 Os1 Os3 C34 107.8(9) . . . . ? C11 Os1 Os3 C34 16.8(4) . . . . ? C12 Os1 Os3 C34 -164.4(4) . . . . ? P1 Os1 Os3 C34 -73.0(3) . . . . ? Os2 Os1 Os3 C34 99.9(3) . . . . ? C13 Os1 Os3 C31 -76.5(9) . . . . ? C11 Os1 Os3 C31 -167.4(4) . . . . ? C12 Os1 Os3 C31 11.4(4) . . . . ? P1 Os1 Os3 C31 102.8(3) . . . . ? Os2 Os1 Os3 C31 -84.4(3) . . . . ? C13 Os1 Os3 Os2 7.9(9) . . . . ? C11 Os1 Os3 Os2 -83.0(3) . . . . ? C12 Os1 Os3 Os2 95.7(3) . . . . ? P1 Os1 Os3 Os2 -172.85(6) . . . . ? C33 Os3 C31 O31 63(11) . . . . ? C32 Os3 C31 O31 -35(11) . . . . ? C34 Os3 C31 O31 -120(11) . . . . ? Os2 Os3 C31 O31 152(11) . . . . ? Os1 Os3 C31 O31 -148(11) . . . . ? C33 Os3 C32 O32 -10(12) . . . . ? C34 Os3 C32 O32 -104(12) . . . . ? C31 Os3 C32 O32 85(12) . . . . ? Os2 Os3 C32 O32 133(11) . . . . ? Os1 Os3 C32 O32 174(12) . . . . ? C32 Os3 C33 O33 -59(10) . . . . ? C34 Os3 C33 O33 32(10) . . . . ? C31 Os3 C33 O33 -149(10) . . . . ? Os2 Os3 C33 O33 127(10) . . . . ? Os1 Os3 C33 O33 113(10) . . . . ? C33 Os3 C34 O34 -59(8) . . . . ? C32 Os3 C34 O34 39(8) . . . . ? C31 Os3 C34 O34 124(8) . . . . ? Os2 Os3 C34 O34 -149(8) . . . . ? Os1 Os3 C34 O34 153(8) . . . . ? C13 Os1 P1 C101 -129.4(5) . . . . ? C11 Os1 P1 C101 -40.9(4) . . . . ? C12 Os1 P1 C101 139.9(4) . . . . ? Os2 Os1 P1 C101 32.7(4) . . . . ? Os3 Os1 P1 C101 51.0(3) . . . . ? C13 Os1 P1 C401 108.1(5) . . . . ? C11 Os1 P1 C401 -163.5(4) . . . . ? C12 Os1 P1 C401 17.3(4) . . . . ? Os2 Os1 P1 C401 -89.8(4) . . . . ? Os3 Os1 P1 C401 -71.6(3) . . . . ? C13 Os1 P1 P2 -12.1(4) . . . . ? C11 Os1 P1 P2 76.4(3) . . . . ? C12 Os1 P1 P2 -102.8(3) . . . . ? Os2 Os1 P1 P2 150.05(11) . . . . ? Os3 Os1 P1 P2 168.29(10) . . . . ? C401 P1 C101 C106 -150.5(7) . . . . ? P2 P1 C101 C106 -48.6(7) . . . . ? Os1 P1 C101 C106 77.2(7) . . . . ? C401 P1 C101 C102 32.8(7) . . . . ? P2 P1 C101 C102 134.6(6) . . . . ? Os1 P1 C101 C102 -99.6(7) . . . . ? C106 C101 C102 C103 -0.6(13) . . . . ? P1 C101 C102 C103 176.2(7) . . . . ? C101 C102 C103 C104 1.1(14) . . . . ? C102 C103 C104 C105 -1.8(15) . . . . ? C103 C104 C105 C106 2.0(15) . . . . ? C102 C101 C106 C105 0.7(12) . . . . ? P1 C101 C106 C105 -176.1(7) . . . . ? C104 C105 C106 C101 -1.5(14) . . . . ? C101 P1 P2 C201 177.3(4) . . . . ? C401 P1 P2 C201 -78.2(4) . . . . ? Os1 P1 P2 C201 53.2(3) . . . . ? C101 P1 P2 P3 -80.0(3) . . . . ? C401 P1 P2 P3 24.6(3) . . . . ? Os1 P1 P2 P3 156.01(11) . . . . ? P1 P2 C201 C206 44.2(9) . . . . ? P3 P2 C201 C206 -52.1(9) . . . . ? P1 P2 C201 C202 -134.2(6) . . . . ? P3 P2 C201 C202 129.5(6) . . . . ? C206 C201 C202 C203 1.3(15) . . . . ? P2 C201 C202 C203 179.8(9) . . . . ? C201 C202 C203 C204 -1.8(19) . . . . ? C202 C203 C204 C205 0(2) . . . . ? C203 C204 C205 C206 2(2) . . . . ? C202 C201 C206 C205 0.8(15) . . . . ? P2 C201 C206 C205 -177.5(8) . . . . ? C204 C205 C206 C201 -2.4(18) . . . . ? C201 P2 P3 C301 -177.3(4) . . . . ? P1 P2 P3 C301 80.0(3) . . . . ? C201 P2 P3 C402 77.7(4) . . . . ? P1 P2 P3 C402 -24.9(3) . . . . ? C201 P2 P3 Os4 -53.2(3) . . . . ? P1 P2 P3 Os4 -155.90(10) . . . . ? C402 P3 C301 C306 -30.6(7) . . . . ? P2 P3 C301 C306 -132.3(6) . . . . ? Os4 P3 C301 C306 101.1(7) . . . . ? C402 P3 C301 C302 154.3(6) . . . . ? P2 P3 C301 C302 52.6(7) . . . . ? Os4 P3 C301 C302 -74.0(7) . . . . ? C306 C301 C302 C303 -0.1(13) . . . . ? P3 C301 C302 C303 175.0(7) . . . . ? C301 C302 C303 C304 -1.9(14) . . . . ? C302 C303 C304 C305 2.9(17) . . . . ? C303 C304 C305 C306 -1.8(16) . . . . ? C304 C305 C306 C301 -0.2(15) . . . . ? C302 C301 C306 C305 1.1(13) . . . . ? P3 C301 C306 C305 -173.9(7) . . . . ? C101 P1 C401 C402 85.1(7) . . . . ? P2 P1 C401 C402 -18.6(7) . . . . ? Os1 P1 C401 C402 -147.0(6) . . . . ? C101 P1 C401 C406 -93.8(8) . . . . ? P2 P1 C401 C406 162.5(7) . . . . ? Os1 P1 C401 C406 34.1(8) . . . . ? C406 C401 C402 C403 -0.3(12) . . . . ? P1 C401 C402 C403 -179.2(7) . . . . ? C406 C401 C402 P3 177.9(7) . . . . ? P1 C401 C402 P3 -1.1(10) . . . . ? C301 P3 C402 C403 94.5(7) . . . . ? P2 P3 C402 C403 -161.7(7) . . . . ? Os4 P3 C402 C403 -32.9(8) . . . . ? C301 P3 C402 C401 -83.7(7) . . . . ? P2 P3 C402 C401 20.1(7) . . . . ? Os4 P3 C402 C401 148.9(6) . . . . ? C401 C402 C403 C404 -0.4(13) . . . . ? P3 C402 C403 C404 -178.6(8) . . . . ? C402 C403 C404 C405 0.6(15) . . . . ? C403 C404 C405 C406 -0.2(15) . . . . ? C404 C405 C406 C401 -0.5(15) . . . . ? C402 C401 C406 C405 0.8(13) . . . . ? P1 C401 C406 C405 179.7(7) . . . . ? C301 P3 Os4 C41 120.3(4) . . . . ? C402 P3 Os4 C41 -117.4(4) . . . . ? P2 P3 Os4 C41 2.6(3) . . . . ? C301 P3 Os4 C42 -150.2(4) . . . . ? C402 P3 Os4 C42 -27.8(4) . . . . ? P2 P3 Os4 C42 92.2(3) . . . . ? C301 P3 Os4 C43 29.5(4) . . . . ? C402 P3 Os4 C43 151.8(4) . . . . ? P2 P3 Os4 C43 -88.2(3) . . . . ? C301 P3 Os4 Os5 -47.8(4) . . . . ? C402 P3 Os4 Os5 74.5(3) . . . . ? P2 P3 Os4 Os5 -165.48(12) . . . . ? C301 P3 Os4 Os6 -58.8(3) . . . . ? C402 P3 Os4 Os6 63.6(3) . . . . ? P2 P3 Os4 Os6 -176.43(9) . . . . ? C42 Os4 C41 O41 108(16) . . . . ? C43 Os4 C41 O41 -71(16) . . . . ? P3 Os4 C41 O41 -163(16) . . . . ? Os5 Os4 C41 O41 14(16) . . . . ? Os6 Os4 C41 O41 15(17) . . . . ? C41 Os4 C42 O42 32(10) . . . . ? C43 Os4 C42 O42 137(28) . . . . ? P3 Os4 C42 O42 -70(10) . . . . ? Os5 Os4 C42 O42 127(10) . . . . ? Os6 Os4 C42 O42 -174(10) . . . . ? C41 Os4 C43 O43 -40(9) . . . . ? C42 Os4 C43 O43 -144(28) . . . . ? P3 Os4 C43 O43 62(9) . . . . ? Os5 Os4 C43 O43 -134(9) . . . . ? Os6 Os4 C43 O43 166(9) . . . . ? C41 Os4 Os5 C54 -3.7(5) . . . . ? C42 Os4 Os5 C54 -93.6(5) . . . . ? C43 Os4 Os5 C54 86.5(5) . . . . ? P3 Os4 Os5 C54 164.6(4) . . . . ? Os6 Os4 Os5 C54 177.0(4) . . . . ? C41 Os4 Os5 C52 90.6(5) . . . . ? C42 Os4 Os5 C52 0.7(5) . . . . ? C43 Os4 Os5 C52 -179.1(5) . . . . ? P3 Os4 Os5 C52 -101.0(5) . . . . ? Os6 Os4 Os5 C52 -88.7(4) . . . . ? C41 Os4 Os5 C53 165.9(10) . . . . ? C42 Os4 Os5 C53 75.9(10) . . . . ? C43 Os4 Os5 C53 -103.9(10) . . . . ? P3 Os4 Os5 C53 -25.8(10) . . . . ? Os6 Os4 Os5 C53 -13.5(10) . . . . ? C41 Os4 Os5 C51 -91.9(4) . . . . ? C42 Os4 Os5 C51 178.2(4) . . . . ? C43 Os4 Os5 C51 -1.6(4) . . . . ? P3 Os4 Os5 C51 76.5(3) . . . . ? Os6 Os4 Os5 C51 88.8(3) . . . . ? C41 Os4 Os5 Os6 179.3(3) . . . . ? C42 Os4 Os5 Os6 89.4(3) . . . . ? C43 Os4 Os5 Os6 -90.4(3) . . . . ? P3 Os4 Os5 Os6 -12.34(18) . . . . ? C54 Os5 C51 O51 48(23) . . . . ? C52 Os5 C51 O51 -137(22) . . . . ? C53 Os5 C51 O51 -53(23) . . . . ? Os6 Os5 C51 O51 -154(23) . . . . ? Os4 Os5 C51 O51 144(23) . . . . ? C54 Os5 C52 O52 -55(12) . . . . ? C53 Os5 C52 O52 46(12) . . . . ? C51 Os5 C52 O52 130(12) . . . . ? Os6 Os5 C52 O52 147(12) . . . . ? Os4 Os5 C52 O52 -151(12) . . . . ? C54 Os5 C53 O53 45(75) . . . . ? C52 Os5 C53 O53 -50(75) . . . . ? C51 Os5 C53 O53 133(75) . . . . ? Os6 Os5 C53 O53 -137(75) . . . . ? Os4 Os5 C53 O53 -125(75) . . . . ? C52 Os5 C54 O54 -138(52) . . . . ? C53 Os5 C54 O54 132(52) . . . . ? C51 Os5 C54 O54 42(52) . . . . ? Os6 Os5 C54 O54 -45(53) . . . . ? Os4 Os5 C54 O54 -52(52) . . . . ? C54 Os5 Os6 C64 3(2) . . . . ? C52 Os5 Os6 C64 97.8(17) . . . . ? C53 Os5 Os6 C64 -173.6(17) . . . . ? C51 Os5 Os6 C64 -82.9(17) . . . . ? Os4 Os5 Os6 C64 10.7(17) . . . . ? C54 Os5 Os6 C63 -93.3(10) . . . . ? C52 Os5 Os6 C63 1.6(5) . . . . ? C53 Os5 Os6 C63 90.2(4) . . . . ? C51 Os5 Os6 C63 -179.1(4) . . . . ? Os4 Os5 Os6 C63 -85.5(3) . . . . ? C54 Os5 Os6 C61 173.3(11) . . . . ? C52 Os5 Os6 C61 -91.7(5) . . . . ? C53 Os5 Os6 C61 -3.1(4) . . . . ? C51 Os5 Os6 C61 87.5(4) . . . . ? Os4 Os5 Os6 C61 -178.9(3) . . . . ? C54 Os5 Os6 C62 81.8(11) . . . . ? C52 Os5 Os6 C62 176.8(5) . . . . ? C53 Os5 Os6 C62 -94.6(5) . . . . ? C51 Os5 Os6 C62 -3.9(4) . . . . ? Os4 Os5 Os6 C62 89.6(3) . . . . ? C54 Os5 Os6 Os4 -7.8(10) . . . . ? C52 Os5 Os6 Os4 87.2(4) . . . . ? C53 Os5 Os6 Os4 175.8(3) . . . . ? C51 Os5 Os6 Os4 -93.6(3) . . . . ? C41 Os4 Os6 C64 -179.1(8) . . . . ? C42 Os4 Os6 C64 88.9(5) . . . . ? C43 Os4 Os6 C64 -91.7(5) . . . . ? P3 Os4 Os6 C64 -1.2(4) . . . . ? Os5 Os4 Os6 C64 -177.6(4) . . . . ? C41 Os4 Os6 C63 92.1(8) . . . . ? C42 Os4 Os6 C63 0.1(5) . . . . ? C43 Os4 Os6 C63 179.5(4) . . . . ? P3 Os4 Os6 C63 -90.0(4) . . . . ? Os5 Os4 Os6 C63 93.6(4) . . . . ? C41 Os4 Os6 C61 0.7(9) . . . . ? C42 Os4 Os6 C61 -91.3(7) . . . . ? C43 Os4 Os6 C61 88.1(7) . . . . ? P3 Os4 Os6 C61 178.6(6) . . . . ? Os5 Os4 Os6 C61 2.2(6) . . . . ? C41 Os4 Os6 C62 -91.0(7) . . . . ? C42 Os4 Os6 C62 177.0(5) . . . . ? C43 Os4 Os6 C62 -3.6(4) . . . . ? P3 Os4 Os6 C62 86.9(4) . . . . ? Os5 Os4 Os6 C62 -89.5(4) . . . . ? C41 Os4 Os6 Os5 -1.5(7) . . . . ? C42 Os4 Os6 Os5 -93.5(3) . . . . ? C43 Os4 Os6 Os5 85.9(3) . . . . ? P3 Os4 Os6 Os5 176.40(5) . . . . ? C64 Os6 C61 O61 -23(32) . . . . ? C63 Os6 C61 O61 67(32) . . . . ? C62 Os6 C61 O61 -112(32) . . . . ? Os5 Os6 C61 O61 159(32) . . . . ? Os4 Os6 C61 O61 157(31) . . . . ? C64 Os6 C62 O62 -20(13) . . . . ? C63 Os6 C62 O62 -89(14) . . . . ? C61 Os6 C62 O62 81(13) . . . . ? Os5 Os6 C62 O62 172(13) . . . . ? Os4 Os6 C62 O62 -128(13) . . . . ? C64 Os6 C63 O63 24(16) . . . . ? C61 Os6 C63 O63 -78(16) . . . . ? C62 Os6 C63 O63 92(16) . . . . ? Os5 Os6 C63 O63 -169(16) . . . . ? Os4 Os6 C63 O63 132(16) . . . . ? C63 Os6 C64 O64 -103(25) . . . . ? C61 Os6 C64 O64 -10(25) . . . . ? C62 Os6 C64 O64 81(25) . . . . ? Os5 Os6 C64 O64 160(23) . . . . ? Os4 Os6 C64 O64 170(25) . . . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 29.39 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 2.031 _refine_diff_density_min -1.892 _refine_diff_density_rms 0.193 #============================================== data_3 _database_code_CSD 158408 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H35 Cl2 O10 Os3 P3' _chemical_formula_weight 1422.10 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' 'Os' 'Os' -1.2165 7.6030 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.8812(19) _cell_length_b 17.490(3) _cell_length_c 12.7076(19) _cell_angle_alpha 90.00 _cell_angle_beta 107.135(17) _cell_angle_gamma 90.00 _cell_volume 2311.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7290 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas not measured _exptl_crystal_density_diffrn 2.044 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 8.498 _exptl_absorpt_correction_type sadabs (Sheldrick) _exptl_absorpt_correction_T_min 0.171022 _exptl_absorpt_correction_T_max 0.350329 _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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14824 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 29.35 _reflns_number_total 5875 _reflns_number_gt 3985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _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^)+(0.0452P)^2^+5.1475P] 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 SHELXL _refine_ls_extinction_coef 0.00079(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5875 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 2.95725(3) 0.332996(18) 2.09208(3) 0.03783(12) Uani 1 1 d . . . C11 C 3.0010(9) 0.4364(5) 2.1230(7) 0.050(2) Uani 1 1 d . . . O11 O 3.0247(9) 0.5000(4) 2.1422(7) 0.085(2) Uani 1 1 d . . . C12 C 2.8393(9) 0.3331(5) 2.1802(7) 0.046(2) Uani 1 1 d . . . O12 O 2.7663(8) 0.3386(4) 2.2286(6) 0.069(2) Uani 1 1 d . . . C13 C 3.0743(9) 0.3329(5) 2.0024(8) 0.049(2) Uani 1 1 d . . . O13 O 3.1416(7) 0.3363(4) 1.9490(6) 0.067(2) Uani 1 1 d . . . Os2 Os 3.14225(5) 0.2500 2.26233(4) 0.04562(15) Uani 1 2 d S . . C21 C 3.2284(11) 0.3359(7) 2.3414(9) 0.067(3) Uani 1 1 d . . . O21 O 3.2766(9) 0.3892(6) 2.3903(8) 0.105(3) Uani 1 1 d . . . C22 C 3.0233(14) 0.2500 2.3492(11) 0.061(4) Uani 1 2 d S . . O22 O 2.9615(11) 0.2500 2.4087(9) 0.085(4) Uani 1 2 d S . . C23 C 3.2579(14) 0.2500 2.1730(11) 0.058(4) Uani 1 2 d S . . O23 O 3.3374(10) 0.2500 2.1287(9) 0.073(3) Uani 1 2 d S . . P1 P 2.7853(2) 0.33442(12) 1.93183(18) 0.0395(5) Uani 1 1 d . . . C101 C 2.6951(9) 0.4217(5) 1.8862(8) 0.048(2) Uani 1 1 d . . . C102 C 2.6288(11) 0.4345(7) 1.7751(10) 0.077(3) Uani 1 1 d . . . H10A H 2.6329 0.3982 1.7227 0.092 Uiso 1 1 calc R . . C103 C 2.5581(15) 0.4995(8) 1.7425(12) 0.099(5) Uani 1 1 d . . . H10B H 2.5162 0.5079 1.6683 0.119 Uiso 1 1 calc R . . C104 C 2.5494(13) 0.5520(8) 1.8191(14) 0.097(5) Uani 1 1 d . . . H10C H 2.5001 0.5959 1.7975 0.117 Uiso 1 1 calc R . . C105 C 2.6129(13) 0.5401(7) 1.9274(13) 0.086(4) Uani 1 1 d . . . H10D H 2.6067 0.5758 1.9797 0.103 Uiso 1 1 calc R . . C106 C 2.6864(11) 0.4752(6) 1.9598(10) 0.068(3) Uani 1 1 d . . . H10E H 2.7307 0.4683 2.0339 0.081 Uiso 1 1 calc R . . P2 P 2.6441(3) 0.2500 1.9549(2) 0.0403(7) Uani 1 2 d S . . C201 C 2.5060(11) 0.2500 1.8305(9) 0.039(3) Uani 1 2 d S . . C202 C 2.3909(12) 0.2500 1.8509(11) 0.061(4) Uani 1 2 d S . . H20A H 2.3891 0.2500 1.9236 0.074 Uiso 1 2 calc SR . . C203 C 2.2759(16) 0.2500 1.7676(13) 0.100(7) Uani 1 2 d S . . H20B H 2.1976 0.2500 1.7831 0.120 Uiso 1 2 calc SR . . C204 C 2.2812(16) 0.2500 1.6602(12) 0.078(5) Uani 1 2 d S . . H20C H 2.2046 0.2500 1.6031 0.094 Uiso 1 2 calc SR . . C205 C 2.3921(15) 0.2500 1.6355(12) 0.069(4) Uani 1 2 d S . . H20D H 2.3935 0.2500 1.5627 0.083 Uiso 1 2 calc SR . . C206 C 2.5040(13) 0.2500 1.7206(10) 0.060(4) Uani 1 2 d S . . H20E H 2.5818 0.2500 1.7042 0.072 Uiso 1 2 calc SR . . C301 C 2.8254(8) 0.2897(5) 1.8157(6) 0.0396(19) Uani 1 1 d . . . C302 C 2.8692(9) 0.3296(5) 1.7402(8) 0.052(2) Uani 1 1 d . . . H30B H 2.8705 0.3828 1.7413 0.063 Uiso 1 1 calc R . . C303 C 2.9116(9) 0.2895(6) 1.6617(7) 0.054(2) Uani 1 1 d . . . H30C H 2.9397 0.3161 1.6098 0.065 Uiso 1 1 calc R . . Cl1 Cl 3.5961(6) 0.3321(4) 2.4552(5) 0.178(3) Uani 1 1 d . . . C4 C 3.639(3) 0.2500 2.400(2) 0.142(10) Uani 1 2 d S . . H4A H 3.7318 0.2500 2.4134 0.171 Uiso 1 2 calc SR . . H4B H 3.5992 0.2500 2.3214 0.171 Uiso 1 2 calc SR . . C2 C 2.148(3) 0.4624(18) 1.5961(19) 0.232(15) Uani 1 1 d . . . H2A H 2.2111 0.4845 1.5652 0.278 Uiso 1 1 calc R . . H2B H 2.1357 0.4100 1.5702 0.278 Uiso 1 1 calc R . . C3 C 2.207(3) 0.4581(15) 1.710(2) 0.231(14) Uani 1 1 d . . . H3A H 2.2878 0.4322 1.7237 0.346 Uiso 1 1 calc R . . H3B H 2.1523 0.4303 1.7436 0.346 Uiso 1 1 calc R . . H3C H 2.2206 0.5087 1.7401 0.346 Uiso 1 1 calc R . . C1 C 2.032(5) 0.500(2) 1.545(3) 0.31(2) Uani 1 1 d . . . H1A H 1.9752 0.4849 1.5871 0.370 Uiso 1 1 calc R . . H1B H 2.0512 0.5535 1.5617 0.370 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0369(2) 0.03971(18) 0.03697(18) -0.00230(13) 0.01099(14) -0.00164(15) C11 0.043(6) 0.054(5) 0.050(5) -0.007(4) 0.011(4) -0.006(4) O11 0.097(7) 0.052(4) 0.109(6) -0.020(4) 0.035(6) -0.015(4) C12 0.050(6) 0.051(5) 0.041(5) -0.007(4) 0.019(4) -0.004(4) O12 0.069(5) 0.080(5) 0.071(5) -0.002(4) 0.042(4) 0.012(4) C13 0.037(5) 0.059(5) 0.054(5) -0.007(4) 0.017(4) -0.002(4) O13 0.061(5) 0.085(5) 0.063(5) 0.006(4) 0.034(4) 0.002(4) Os2 0.0378(3) 0.0608(3) 0.0360(3) 0.000 0.0073(2) 0.000 C21 0.055(7) 0.080(8) 0.062(7) -0.005(6) 0.012(6) -0.008(6) O21 0.099(7) 0.112(7) 0.111(7) -0.051(6) 0.038(6) -0.045(6) C22 0.041(8) 0.097(11) 0.037(7) 0.000 0.000(6) 0.000 O22 0.068(8) 0.147(11) 0.052(6) 0.000 0.034(6) 0.000 C23 0.040(8) 0.092(11) 0.039(7) 0.000 0.010(6) 0.000 O23 0.049(7) 0.105(9) 0.069(7) 0.000 0.024(6) 0.000 P1 0.0357(12) 0.0430(11) 0.0388(11) -0.0002(9) 0.0095(9) 0.0018(10) C101 0.033(5) 0.052(5) 0.059(6) 0.011(4) 0.013(4) 0.006(4) C102 0.070(8) 0.082(8) 0.077(8) 0.031(6) 0.020(7) 0.016(7) C103 0.111(13) 0.088(10) 0.093(10) 0.033(8) 0.021(9) 0.029(9) C104 0.073(9) 0.073(8) 0.129(13) 0.030(9) 0.002(9) 0.024(7) C105 0.070(9) 0.059(7) 0.129(12) -0.009(7) 0.031(8) 0.014(6) C106 0.067(8) 0.051(6) 0.086(8) -0.002(5) 0.024(6) 0.009(5) P2 0.0333(18) 0.0541(18) 0.0350(16) 0.000 0.0123(13) 0.000 C201 0.030(7) 0.044(6) 0.041(6) 0.000 0.009(5) 0.000 C202 0.027(7) 0.115(12) 0.045(7) 0.000 0.015(6) 0.000 C203 0.034(9) 0.20(2) 0.055(10) 0.000 -0.004(8) 0.000 C204 0.041(9) 0.137(16) 0.047(9) 0.000 -0.002(7) 0.000 C205 0.058(11) 0.095(12) 0.047(8) 0.000 0.003(8) 0.000 C206 0.034(8) 0.100(11) 0.039(7) 0.000 0.000(6) 0.000 C301 0.031(5) 0.050(5) 0.038(4) -0.002(3) 0.012(4) 0.001(4) C302 0.047(6) 0.057(5) 0.051(5) 0.000(4) 0.012(5) -0.014(5) C303 0.051(6) 0.079(6) 0.037(5) 0.002(4) 0.019(4) -0.005(5) Cl1 0.174(6) 0.218(7) 0.160(5) 0.071(5) 0.077(5) 0.079(5) C4 0.13(2) 0.19(3) 0.109(19) 0.000 0.049(18) 0.000 C2 0.36(5) 0.23(3) 0.112(18) -0.03(2) 0.07(3) -0.02(3) C3 0.29(4) 0.20(2) 0.24(3) -0.13(2) 0.13(3) -0.04(2) C1 0.33(6) 0.27(3) 0.24(5) 0.12(4) -0.04(4) 0.10(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C11 1.883(10) . ? Os1 C12 1.936(9) . ? Os1 C13 1.944(9) . ? Os1 P1 2.324(2) . ? Os1 Os2 2.8764(7) . ? Os1 Os1 2.9033(8) 4_565 ? C11 O11 1.151(10) . ? C12 O12 1.144(10) . ? C13 O13 1.137(11) . ? Os2 C21 1.895(12) . ? Os2 C21 1.895(12) 4_565 ? Os2 C23 1.927(14) . ? Os2 C22 1.933(15) . ? Os2 Os1 2.8764(7) 4_565 ? C21 O21 1.156(12) . ? C22 O22 1.150(17) . ? C23 O23 1.162(16) . ? P1 C101 1.816(9) . ? P1 C301 1.833(8) . ? P1 P2 2.212(3) . ? C101 C106 1.346(13) . ? C101 C102 1.402(14) . ? C102 C103 1.367(16) . ? C103 C104 1.362(18) . ? C104 C105 1.362(19) . ? C105 C106 1.380(15) . ? P2 C201 1.833(12) . ? P2 P1 2.212(3) 4_565 ? C201 C202 1.352(17) . ? C201 C206 1.389(17) . ? C202 C203 1.38(2) . ? C203 C204 1.38(2) . ? C204 C205 1.33(2) . ? C205 C206 1.370(19) . ? C301 C302 1.380(12) . ? C301 C301 1.388(16) 4_565 ? C302 C303 1.403(12) . ? C303 C303 1.382(19) 4_565 ? Cl1 C4 1.721(14) . ? C4 Cl1 1.721(14) 4_565 ? C2 C1 1.40(5) . ? C2 C3 1.40(3) . ? C1 C1 1.15(5) 3_968 ? 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 C11 Os1 C12 92.8(4) . . ? C11 Os1 C13 87.4(4) . . ? C12 Os1 C13 179.5(4) . . ? C11 Os1 P1 105.1(3) . . ? C12 Os1 P1 90.4(3) . . ? C13 Os1 P1 89.1(3) . . ? C11 Os1 Os2 104.5(3) . . ? C12 Os1 Os2 90.1(3) . . ? C13 Os1 Os2 90.4(3) . . ? P1 Os1 Os2 150.30(6) . . ? C11 Os1 Os1 164.0(3) . 4_565 ? C12 Os1 Os1 90.0(3) . 4_565 ? C13 Os1 Os1 90.0(3) . 4_565 ? P1 Os1 Os1 90.61(5) . 4_565 ? Os2 Os1 Os1 59.691(11) . 4_565 ? O11 C11 Os1 178.3(9) . . ? O12 C12 Os1 174.6(8) . . ? O13 C13 Os1 176.9(9) . . ? C21 Os2 C21 104.9(7) . 4_565 ? C21 Os2 C23 90.3(4) . . ? C21 Os2 C23 90.3(4) 4_565 . ? C21 Os2 C22 90.4(4) . . ? C21 Os2 C22 90.4(4) 4_565 . ? C23 Os2 C22 178.8(6) . . ? C21 Os2 Os1 157.8(3) . 4_565 ? C21 Os2 Os1 97.2(4) 4_565 4_565 ? C23 Os2 Os1 89.5(4) . 4_565 ? C22 Os2 Os1 89.5(3) . 4_565 ? C21 Os2 Os1 97.2(3) . . ? C21 Os2 Os1 157.8(4) 4_565 . ? C23 Os2 Os1 89.5(3) . . ? C22 Os2 Os1 89.5(3) . . ? Os1 Os2 Os1 60.62(2) 4_565 . ? O21 C21 Os2 177.4(11) . . ? O22 C22 Os2 174.2(12) . . ? O23 C23 Os2 173.3(12) . . ? C101 P1 C301 109.7(4) . . ? C101 P1 P2 105.8(3) . . ? C301 P1 P2 99.3(3) . . ? C101 P1 Os1 120.6(3) . . ? C301 P1 Os1 112.3(3) . . ? P2 P1 Os1 106.74(12) . . ? C106 C101 C102 118.0(10) . . ? C106 C101 P1 120.3(8) . . ? C102 C101 P1 121.7(8) . . ? C103 C102 C101 120.9(13) . . ? C104 C103 C102 119.8(13) . . ? C105 C104 C103 119.8(12) . . ? C104 C105 C106 120.4(13) . . ? C101 C106 C105 121.1(12) . . ? C201 P2 P1 108.1(3) . . ? C201 P2 P1 108.1(3) . 4_565 ? P1 P2 P1 83.75(16) . 4_565 ? C202 C201 C206 116.9(12) . . ? C202 C201 P2 113.9(9) . . ? C206 C201 P2 129.3(10) . . ? C201 C202 C203 122.2(13) . . ? C202 C203 C204 117.8(15) . . ? C205 C204 C203 122.4(15) . . ? C204 C205 C206 118.0(15) . . ? C205 C206 C201 122.8(14) . . ? C302 C301 C301 120.4(5) . 4_565 ? C302 C301 P1 123.8(7) . . ? C301 C301 P1 115.3(3) 4_565 . ? C301 C302 C303 119.6(9) . . ? C303 C303 C302 120.0(5) 4_565 . ? Cl1 C4 Cl1 113.1(14) . 4_565 ? C1 C2 C3 126(3) . . ? C1 C1 C2 132(7) 3_968 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Os1 C11 O11 -29(31) . . . . ? C13 Os1 C11 O11 150(31) . . . . ? P1 Os1 C11 O11 62(31) . . . . ? Os2 Os1 C11 O11 -120(31) . . . . ? Os1 Os1 C11 O11 -129(31) 4_565 . . . ? C11 Os1 C12 O12 43(9) . . . . ? C13 Os1 C12 O12 -64(44) . . . . ? P1 Os1 C12 O12 -62(9) . . . . ? Os2 Os1 C12 O12 148(9) . . . . ? Os1 Os1 C12 O12 -152(9) 4_565 . . . ? C11 Os1 C13 O13 -29(16) . . . . ? C12 Os1 C13 O13 78(46) . . . . ? P1 Os1 C13 O13 76(16) . . . . ? Os2 Os1 C13 O13 -134(16) . . . . ? Os1 Os1 C13 O13 166(16) 4_565 . . . ? C11 Os1 Os2 C21 2.8(5) . . . . ? C12 Os1 Os2 C21 -90.1(4) . . . . ? C13 Os1 Os2 C21 90.2(4) . . . . ? P1 Os1 Os2 C21 179.0(4) . . . . ? Os1 Os1 Os2 C21 179.9(4) 4_565 . . . ? C11 Os1 Os2 C21 -177.0(10) . . . 4_565 ? C12 Os1 Os2 C21 90.2(10) . . . 4_565 ? C13 Os1 Os2 C21 -89.6(10) . . . 4_565 ? P1 Os1 Os2 C21 -0.8(9) . . . 4_565 ? Os1 Os1 Os2 C21 0.2(9) 4_565 . . 4_565 ? C11 Os1 Os2 C23 -87.4(4) . . . . ? C12 Os1 Os2 C23 179.7(3) . . . . ? C13 Os1 Os2 C23 0.0(3) . . . . ? P1 Os1 Os2 C23 88.7(2) . . . . ? Os1 Os1 Os2 C23 89.7(2) 4_565 . . . ? C11 Os1 Os2 C22 93.2(4) . . . . ? C12 Os1 Os2 C22 0.3(3) . . . . ? C13 Os1 Os2 C22 -179.5(3) . . . . ? P1 Os1 Os2 C22 -90.7(2) . . . . ? Os1 Os1 Os2 C22 -89.7(2) 4_565 . . . ? C11 Os1 Os2 Os1 -177.1(3) . . . 4_565 ? C12 Os1 Os2 Os1 90.0(3) . . . 4_565 ? C13 Os1 Os2 Os1 -89.7(3) . . . 4_565 ? P1 Os1 Os2 Os1 -0.99(12) . . . 4_565 ? C21 Os2 C21 O21 -118(25) 4_565 . . . ? C23 Os2 C21 O21 151(25) . . . . ? C22 Os2 C21 O21 -28(25) . . . . ? Os1 Os2 C21 O21 62(25) 4_565 . . . ? Os1 Os2 C21 O21 62(25) . . . . ? C21 Os2 C22 O22 -52.5(4) . . . . ? C21 Os2 C22 O22 52.5(4) 4_565 . . . ? C23 Os2 C22 O22 180.0(3) . . . . ? Os1 Os2 C22 O22 149.69(13) 4_565 . . . ? Os1 Os2 C22 O22 -149.69(14) . . . . ? C21 Os2 C23 O23 52.5(4) . . . . ? C21 Os2 C23 O23 -52.5(4) 4_565 . . . ? C22 Os2 C23 O23 180.0(3) . . . . ? Os1 Os2 C23 O23 -149.69(11) 4_565 . . . ? Os1 Os2 C23 O23 149.69(11) . . . . ? C11 Os1 P1 C101 -17.0(5) . . . . ? C12 Os1 P1 C101 76.0(4) . . . . ? C13 Os1 P1 C101 -104.0(4) . . . . ? Os2 Os1 P1 C101 166.9(3) . . . . ? Os1 Os1 P1 C101 166.1(3) 4_565 . . . ? C11 Os1 P1 C301 114.7(4) . . . . ? C12 Os1 P1 C301 -152.3(4) . . . . ? C13 Os1 P1 C301 27.7(4) . . . . ? Os2 Os1 P1 C301 -61.4(3) . . . . ? Os1 Os1 P1 C301 -62.2(3) 4_565 . . . ? C11 Os1 P1 P2 -137.5(3) . . . . ? C12 Os1 P1 P2 -44.5(3) . . . . ? C13 Os1 P1 P2 135.5(3) . . . . ? Os2 Os1 P1 P2 46.40(17) . . . . ? Os1 Os1 P1 P2 45.55(9) 4_565 . . . ? C301 P1 C101 C106 -161.0(8) . . . . ? P2 P1 C101 C106 92.8(8) . . . . ? Os1 P1 C101 C106 -28.2(9) . . . . ? C301 P1 C101 C102 21.4(10) . . . . ? P2 P1 C101 C102 -84.8(9) . . . . ? Os1 P1 C101 C102 154.2(8) . . . . ? C106 C101 C102 C103 0.4(17) . . . . ? P1 C101 C102 C103 178.0(10) . . . . ? C101 C102 C103 C104 -2(2) . . . . ? C102 C103 C104 C105 1(2) . . . . ? C103 C104 C105 C106 0(2) . . . . ? C102 C101 C106 C105 1.0(16) . . . . ? P1 C101 C106 C105 -176.7(9) . . . . ? C104 C105 C106 C101 -1(2) . . . . ? C101 P1 P2 C201 49.9(4) . . . . ? C301 P1 P2 C201 -63.7(4) . . . . ? Os1 P1 P2 C201 179.5(3) . . . . ? C101 P1 P2 P1 156.9(3) . . . 4_565 ? C301 P1 P2 P1 43.4(3) . . . 4_565 ? Os1 P1 P2 P1 -73.46(13) . . . 4_565 ? P1 P2 C201 C202 -135.39(13) . . . . ? P1 P2 C201 C202 135.39(13) 4_565 . . . ? P1 P2 C201 C206 44.61(13) . . . . ? P1 P2 C201 C206 -44.61(13) 4_565 . . . ? C206 C201 C202 C203 0.000(15) . . . . ? P2 C201 C202 C203 180.000(13) . . . . ? C201 C202 C203 C204 0.000(15) . . . . ? C202 C203 C204 C205 0.000(18) . . . . ? C203 C204 C205 C206 0.000(16) . . . . ? C204 C205 C206 C201 0.000(13) . . . . ? C202 C201 C206 C205 0.000(14) . . . . ? P2 C201 C206 C205 180.000(13) . . . . ? C101 P1 C301 C302 43.3(9) . . . . ? P2 P1 C301 C302 153.8(7) . . . . ? Os1 P1 C301 C302 -93.7(8) . . . . ? C101 P1 C301 C301 -145.0(3) . . . 4_565 ? P2 P1 C301 C301 -34.4(2) . . . 4_565 ? Os1 P1 C301 C301 78.1(2) . . . 4_565 ? C301 C301 C302 C303 1.2(11) 4_565 . . . ? P1 C301 C302 C303 172.5(7) . . . . ? C301 C302 C303 C303 -1.2(11) . . . 4_565 ? C3 C2 C1 C1 -170(7) . . . 3_968 ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 29.35 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 1.629 _refine_diff_density_min -1.248 _refine_diff_density_rms 0.205 #============================================== data_4a _database_code_CSD 158409 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H26 O17 Os5 P3' _chemical_formula_weight 1870.56 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' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8065(2) _cell_length_b 13.7544(2) _cell_length_c 19.6895(3) _cell_angle_alpha 100.5680(10) _cell_angle_beta 94.87 _cell_angle_gamma 109.5980(10) _cell_volume 2428.57(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13407 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not measured _exptl_crystal_density_diffrn 2.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1702 _exptl_absorpt_coefficient_mu 13.202 _exptl_absorpt_correction_type sadabs (Sheldrick, 1996) _exptl_absorpt_correction_T_min 0.073079 _exptl_absorpt_correction_T_max 0.185315 _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 22961 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0960 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 29.34 _reflns_number_total 11757 _reflns_number_gt 8029 _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^)+(0.0292P)^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 SHELXL _refine_ls_extinction_coef 0.00054(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11757 _refine_ls_number_parameters 665 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 0.819 _refine_ls_restrained_S_all 0.819 _refine_ls_shift/su_max 3.646 _refine_ls_shift/su_mean 0.069 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 1.47229(3) 0.54655(2) -0.164628(17) 0.03073(9) Uani 1 1 d . . . Os2 Os 1.36372(4) 0.65183(2) -0.253508(17) 0.03135(9) Uani 1 1 d . . . Os3 Os 1.06150(4) 0.17471(2) -0.284509(18) 0.03306(9) Uani 1 1 d . . . Os4 Os 0.98472(4) 0.11020(2) -0.155654(19) 0.03902(10) Uani 1 1 d . . . Os5 Os 0.97855(4) -0.04486(2) -0.27691(2) 0.04681(11) Uani 1 1 d . . . P1 P 1.3119(2) 0.46680(14) -0.27314(11) 0.0294(4) Uani 1 1 d . . . P2 P 1.0877(2) 0.35428(14) -0.27609(11) 0.0287(4) Uani 1 1 d . . . P3 P 1.2734(2) 0.60498(14) -0.15123(11) 0.0295(4) Uani 1 1 d . . . O11 O 1.7314(8) 0.5389(6) -0.2397(4) 0.067(2) Uani 1 1 d . . . O12 O 1.6862(8) 0.7343(6) -0.0530(4) 0.074(2) Uani 1 1 d . . . O13 O 1.4279(9) 0.3853(6) -0.0737(4) 0.077(2) Uani 1 1 d . . . O21 O 1.1329(10) 0.7107(6) -0.3332(5) 0.085(3) Uani 1 1 d . . . O22 O 1.5463(8) 0.8765(5) -0.1708(4) 0.072(2) Uani 1 1 d . . . O23 O 1.5817(10) 0.6668(5) -0.3565(4) 0.082(3) Uani 1 1 d . . . O31 O 1.1444(10) 0.1183(6) -0.4259(4) 0.077(2) Uani 1 1 d . . . O32 O 1.3769(8) 0.2299(5) -0.2128(4) 0.0597(19) Uani 1 1 d . . . O33 O 0.7449(8) 0.1256(6) -0.3509(4) 0.067(2) Uani 1 1 d . . . O41 O 0.8671(10) -0.0442(6) -0.0629(5) 0.088(3) Uani 1 1 d . . . O42 O 1.0560(10) 0.3217(6) -0.0510(4) 0.083(3) Uani 1 1 d . . . O43 O 1.2887(9) 0.1119(7) -0.1017(5) 0.087(3) Uani 1 1 d . . . O44 O 0.6752(8) 0.1051(5) -0.2055(4) 0.0613(19) Uani 1 1 d . . . O51 O 0.9046(12) -0.2288(7) -0.2035(6) 0.121(4) Uani 1 1 d . . . O52 O 0.9760(13) -0.1551(8) -0.4251(5) 0.116(4) Uani 1 1 d . . . O53 O 1.3037(11) -0.0083(7) -0.2424(6) 0.115(4) Uani 1 1 d . . . O54 O 0.6520(9) -0.0882(5) -0.3154(5) 0.075(2) Uani 1 1 d . . . H10A H 1.290(15) 0.448(10) -0.410(7) 0.090 Uiso 1 1 d . . . H10B H 1.325(15) 0.372(11) -0.505(7) 0.090 Uiso 1 1 d . . . H10C H 1.468(13) 0.280(9) -0.511(6) 0.090 Uiso 1 1 d . . . H10D H 1.557(12) 0.259(9) -0.398(6) 0.090 Uiso 1 1 d . . . H10E H 1.494(12) 0.342(9) -0.296(6) 0.090 Uiso 1 1 d . . . H20A H 1.037(12) 0.265(8) -0.421(6) 0.090 Uiso 1 1 d . . . H20B H 0.900(12) 0.274(8) -0.529(6) 0.090 Uiso 1 1 d . . . H20C H 0.793(12) 0.433(8) -0.524(6) 0.090 Uiso 1 1 d . . . H20D H 0.830(12) 0.542(9) -0.386(6) 0.090 Uiso 1 1 d . . . H20E H 0.960(12) 0.514(8) -0.281(6) 0.090 Uiso 1 1 d . . . H30A H 0.832(12) 0.301(9) -0.243(6) 0.090 Uiso 1 1 d . . . H30B H 0.698(12) 0.349(8) -0.151(6) 0.090 Uiso 1 1 d . . . H30C H 0.827(13) 0.490(9) -0.069(7) 0.090 Uiso 1 1 d . . . H30D H 1.074(12) 0.596(9) -0.063(6) 0.090 Uiso 1 1 d . . . H40A H 1.185(12) 0.763(8) -0.149(6) 0.090 Uiso 1 1 d . . . H40B H 1.260(15) 0.923(9) -0.042(7) 0.090 Uiso 1 1 d . . . H40C H 1.349(12) 0.951(9) 0.063(6) 0.090 Uiso 1 1 d . . . H40D H 1.430(13) 0.819(9) 0.085(6) 0.090 Uiso 1 1 d . . . H40E H 1.394(13) 0.666(9) -0.011(6) 0.090 Uiso 1 1 d . . . C1 C 0.513(5) 0.032(3) -0.509(3) 0.101(14) Uiso 0.50 1 d P . . C2 C 0.635(4) 0.055(3) -0.571(2) 0.124(13) Uiso 0.50 1 d P . . C3 C 1.605(5) 0.038(3) -0.529(3) 0.137(15) Uiso 0.50 1 d P . . C11 C 1.6370(11) 0.5382(6) -0.2111(5) 0.045(2) Uani 1 1 d . . . C12 C 1.6067(10) 0.6654(7) -0.0930(5) 0.043(2) Uani 1 1 d . . . C13 C 1.4433(11) 0.4446(7) -0.1086(5) 0.048(2) Uani 1 1 d . . . C21 C 1.2178(12) 0.6854(7) -0.3044(5) 0.054(3) Uani 1 1 d . . . C22 C 1.4745(11) 0.7950(6) -0.2016(5) 0.049(2) Uani 1 1 d . . . C23 C 1.4976(11) 0.6618(6) -0.3199(5) 0.050(2) Uani 1 1 d . . . C31 C 1.1147(11) 0.1436(7) -0.3734(5) 0.049(2) Uani 1 1 d . . . C32 C 1.2553(11) 0.2077(6) -0.2381(5) 0.043(2) Uani 1 1 d . . . C33 C 0.8617(11) 0.1406(6) -0.3262(5) 0.044(2) Uani 1 1 d . . . C41 C 0.9094(11) 0.0122(7) -0.0981(6) 0.051(2) Uani 1 1 d . . . C42 C 1.0287(12) 0.2437(9) -0.0908(6) 0.059(3) Uani 1 1 d . . . C43 C 1.1795(12) 0.1127(8) -0.1246(6) 0.055(3) Uani 1 1 d . . . C44 C 0.7893(12) 0.1065(7) -0.1898(5) 0.048(2) Uani 1 1 d . . . C51 C 0.9300(13) -0.1613(8) -0.2317(7) 0.076(4) Uani 1 1 d . . . C52 C 0.9765(13) -0.1130(8) -0.3687(7) 0.069(3) Uani 1 1 d . . . C53 C 1.1851(13) -0.0168(8) -0.2528(8) 0.076(4) Uani 1 1 d . . . C54 C 0.7733(13) -0.0673(7) -0.3007(6) 0.056(3) Uani 1 1 d . . . C101 C 1.3672(9) 0.4034(6) -0.3490(5) 0.037(2) Uani 1 1 d . . . C102 C 1.3253(13) 0.4178(8) -0.4142(6) 0.050(3) Uani 1 1 d . . . C103 C 1.3667(16) 0.3706(11) -0.4732(6) 0.069(4) Uani 1 1 d . . . C104 C 1.4536(16) 0.3122(9) -0.4663(8) 0.079(4) Uani 1 1 d . . . C105 C 1.4995(13) 0.2990(8) -0.4036(7) 0.061(3) Uani 1 1 d . . . C106 C 1.4572(11) 0.3442(6) -0.3440(5) 0.046(2) Uani 1 1 d . . . C201 C 0.9873(9) 0.3781(6) -0.3504(4) 0.0339(18) Uani 1 1 d . . . C202 C 0.9686(12) 0.3175(8) -0.4176(5) 0.052(2) Uani 1 1 d . . . C203 C 0.9025(13) 0.3390(8) -0.4766(6) 0.063(3) Uani 1 1 d . . . C204 C 0.8465(12) 0.4218(10) -0.4632(7) 0.069(3) Uani 1 1 d . . . C205 C 0.8634(12) 0.4825(9) -0.3971(6) 0.059(3) Uani 1 1 d . . . C206 C 0.9346(10) 0.4612(7) -0.3396(5) 0.041(2) Uani 1 1 d . . . C301 C 1.0177(8) 0.4163(6) -0.2027(4) 0.0298(17) Uani 1 1 d . . . C302 C 0.8725(10) 0.3563(6) -0.1999(5) 0.038(2) Uani 1 1 d . . . C303 C 0.7995(10) 0.3854(7) -0.1473(5) 0.046(2) Uani 1 1 d . . . C304 C 0.8703(12) 0.4751(8) -0.0977(6) 0.051(3) Uani 1 1 d . . . C305 C 1.0107(10) 0.5368(7) -0.0992(5) 0.044(2) Uani 1 1 d . . . C306 C 1.0884(8) 0.5114(5) -0.1518(4) 0.0275(16) Uani 1 1 d . . . C401 C 1.2955(9) 0.7154(6) -0.0804(4) 0.0330(18) Uani 1 1 d . . . C402 C 1.2518(13) 0.7977(7) -0.0926(6) 0.057(3) Uani 1 1 d . . . C403 C 1.276(2) 0.8846(9) -0.0374(9) 0.092(5) Uani 1 1 d . . . C404 C 1.3482(15) 0.8910(9) 0.0276(7) 0.074(4) Uani 1 1 d . . . C405 C 1.3809(12) 0.8081(11) 0.0395(6) 0.069(3) Uani 1 1 d . . . C406 C 1.3594(11) 0.7202(8) -0.0128(6) 0.052(3) 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 0.03534(18) 0.03050(15) 0.02708(19) 0.00751(13) 0.00392(14) 0.01244(13) Os2 0.0461(2) 0.02416(14) 0.02370(18) 0.00707(12) 0.00687(15) 0.01125(13) Os3 0.0427(2) 0.02418(14) 0.0297(2) 0.00542(13) 0.00265(15) 0.00977(13) Os4 0.0462(2) 0.03334(16) 0.0331(2) 0.01037(15) 0.00158(16) 0.00820(15) Os5 0.0604(3) 0.02416(15) 0.0494(3) 0.00502(15) 0.0006(2) 0.01057(15) P1 0.0375(12) 0.0251(9) 0.0251(12) 0.0055(8) 0.0055(9) 0.0104(8) P2 0.0367(12) 0.0261(9) 0.0233(11) 0.0063(8) 0.0050(9) 0.0108(8) P3 0.0385(12) 0.0277(9) 0.0218(11) 0.0041(8) 0.0051(9) 0.0121(9) O11 0.054(4) 0.070(4) 0.079(6) 0.006(4) 0.029(4) 0.027(4) O12 0.070(5) 0.065(4) 0.054(5) -0.004(4) -0.007(4) -0.005(4) O13 0.109(7) 0.068(5) 0.060(5) 0.039(4) 0.009(5) 0.026(5) O21 0.103(7) 0.068(5) 0.086(7) 0.017(5) -0.022(5) 0.041(5) O22 0.082(5) 0.034(3) 0.068(6) -0.007(4) 0.011(4) -0.009(3) O23 0.112(7) 0.054(4) 0.072(6) 0.012(4) 0.052(5) 0.011(4) O31 0.113(7) 0.077(5) 0.047(5) 0.004(4) 0.031(5) 0.041(5) O32 0.057(5) 0.055(4) 0.070(5) 0.026(4) 0.006(4) 0.018(3) O33 0.055(5) 0.067(5) 0.065(5) 0.020(4) -0.008(4) 0.007(4) O41 0.100(7) 0.074(5) 0.094(7) 0.051(5) 0.021(6) 0.017(5) O42 0.125(7) 0.060(4) 0.052(5) -0.017(4) -0.021(5) 0.042(5) O43 0.056(5) 0.109(7) 0.095(7) 0.052(6) -0.008(5) 0.019(5) O44 0.052(4) 0.066(4) 0.071(6) 0.026(4) 0.014(4) 0.020(4) O51 0.143(9) 0.064(5) 0.147(10) 0.062(6) -0.016(7) 0.014(6) O52 0.163(10) 0.116(7) 0.060(7) -0.028(6) -0.012(7) 0.072(7) O53 0.085(7) 0.080(6) 0.168(11) -0.005(6) -0.009(7) 0.038(6) O54 0.066(5) 0.050(4) 0.091(7) 0.010(4) -0.001(5) 0.003(4) C11 0.053(6) 0.040(4) 0.047(6) 0.010(4) 0.002(5) 0.023(4) C12 0.039(5) 0.047(5) 0.040(6) 0.016(5) 0.002(5) 0.012(4) C13 0.063(6) 0.056(5) 0.036(6) 0.020(5) 0.006(5) 0.030(5) C21 0.073(7) 0.042(5) 0.044(6) 0.008(4) -0.014(5) 0.021(5) C22 0.058(6) 0.031(4) 0.054(7) 0.011(4) 0.020(5) 0.009(4) C23 0.068(7) 0.032(4) 0.046(6) 0.007(4) 0.025(5) 0.010(4) C31 0.068(7) 0.041(5) 0.035(6) -0.003(4) 0.002(5) 0.024(5) C32 0.057(6) 0.035(4) 0.037(6) 0.016(4) 0.006(5) 0.014(4) C33 0.052(6) 0.032(4) 0.037(6) 0.009(4) -0.004(5) 0.003(4) C41 0.051(6) 0.047(5) 0.052(7) 0.014(5) 0.005(5) 0.011(4) C42 0.066(7) 0.069(7) 0.047(7) 0.021(6) 0.006(6) 0.026(6) C43 0.055(7) 0.053(6) 0.052(7) 0.028(5) 0.008(6) 0.006(5) C44 0.056(6) 0.035(4) 0.050(7) 0.023(4) 0.009(5) 0.006(4) C51 0.080(8) 0.042(5) 0.091(10) 0.016(6) -0.012(7) 0.009(5) C52 0.087(9) 0.056(6) 0.055(8) -0.007(6) -0.012(7) 0.030(6) C53 0.055(7) 0.043(5) 0.123(12) 0.015(6) -0.012(8) 0.018(5) C54 0.059(7) 0.032(4) 0.071(8) 0.018(5) 0.006(6) 0.005(5) C101 0.048(5) 0.030(4) 0.035(5) 0.010(4) 0.012(4) 0.013(4) C102 0.066(7) 0.049(6) 0.036(6) 0.005(5) 0.014(5) 0.023(5) C103 0.091(10) 0.068(7) 0.044(8) 0.010(6) 0.018(7) 0.025(7) C104 0.105(10) 0.062(7) 0.067(10) -0.002(7) 0.046(9) 0.026(7) C105 0.071(8) 0.050(6) 0.067(9) 0.007(6) 0.032(7) 0.026(5) C106 0.058(6) 0.033(4) 0.047(6) 0.003(4) 0.012(5) 0.018(4) C201 0.039(5) 0.036(4) 0.027(5) 0.012(4) 0.006(4) 0.011(4) C202 0.074(7) 0.057(6) 0.030(6) 0.014(5) 0.004(5) 0.028(5) C203 0.083(8) 0.060(6) 0.041(7) 0.011(5) -0.005(6) 0.023(6) C204 0.056(7) 0.096(9) 0.059(8) 0.054(7) -0.005(6) 0.019(6) C205 0.071(7) 0.075(7) 0.042(7) 0.017(6) -0.001(6) 0.041(6) C206 0.044(5) 0.046(5) 0.038(6) 0.015(4) 0.003(4) 0.020(4) C301 0.033(4) 0.034(4) 0.023(4) 0.009(3) 0.008(4) 0.011(3) C302 0.041(5) 0.038(4) 0.042(6) 0.015(4) 0.015(5) 0.017(4) C303 0.037(5) 0.046(5) 0.051(7) 0.006(5) 0.012(5) 0.013(4) C304 0.053(7) 0.051(5) 0.046(7) 0.003(5) 0.018(5) 0.015(5) C305 0.047(6) 0.049(5) 0.036(6) 0.004(4) 0.011(5) 0.020(4) C306 0.032(4) 0.028(3) 0.022(4) 0.005(3) 0.003(3) 0.010(3) C401 0.042(5) 0.031(4) 0.024(5) 0.004(3) 0.009(4) 0.010(3) C402 0.095(8) 0.043(5) 0.040(6) 0.009(5) 0.017(6) 0.034(5) C403 0.161(14) 0.047(6) 0.101(12) 0.030(7) 0.073(12) 0.060(8) C404 0.103(10) 0.045(6) 0.043(8) -0.017(5) 0.027(7) -0.003(6) C405 0.051(7) 0.091(9) 0.038(7) -0.015(6) 0.011(5) 0.006(6) C406 0.046(6) 0.063(6) 0.043(7) 0.002(5) 0.011(5) 0.017(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 C13 1.903(9) . ? Os1 C12 1.947(10) . ? Os1 C11 1.949(10) . ? Os1 P3 2.363(2) . ? Os1 P1 2.378(2) . ? Os1 Os2 2.8178(4) . ? Os2 C21 1.906(10) . ? Os2 C23 1.921(10) . ? Os2 C22 1.934(9) . ? Os2 P1 2.3712(18) . ? Os2 P3 2.377(2) . ? Os3 C32 1.905(10) . ? Os3 C31 1.884(10) . ? Os3 C33 1.924(10) . ? Os3 P2 2.3688(18) . ? Os3 Os5 2.8884(4) . ? Os3 Os4 2.9142(5) . ? Os4 C41 1.920(10) . ? Os4 C43 1.942(12) . ? Os4 C42 1.924(12) . ? Os4 C44 1.957(11) . ? Os4 Os5 2.8764(5) . ? Os5 C52 1.872(12) . ? Os5 C53 1.929(12) . ? Os5 C51 1.915(11) . ? Os5 C54 1.933(12) . ? P1 C101 1.805(8) . ? P1 P2 2.213(3) . ? P2 C201 1.835(8) . ? P2 C301 1.843(8) . ? P3 C401 1.803(8) . ? P3 C306 1.836(8) . ? O11 C11 1.121(10) . ? O12 C12 1.118(10) . ? O13 C13 1.140(10) . ? O21 C21 1.151(11) . ? O22 C22 1.127(10) . ? O23 C23 1.133(10) . ? O31 C31 1.124(11) . ? O32 C32 1.167(11) . ? O33 C33 1.140(10) . ? O41 C41 1.133(11) . ? O42 C42 1.141(12) . ? O43 C43 1.130(11) . ? O44 C44 1.128(11) . ? O51 C51 1.135(12) . ? O52 C52 1.154(13) . ? O53 C53 1.126(12) . ? O54 C54 1.125(12) . ? C1 C3 1.01(6) 1_455 ? C1 C1 0.96(7) 2_654 ? C1 C2 1.79(7) . ? C1 C3 1.58(7) 2_754 ? C2 C3 0.94(6) 1_455 ? C3 C1 1.01(6) 1_655 ? C3 C2 0.94(6) 1_655 ? C3 C1 1.58(7) 2_754 ? C101 C102 1.384(14) . ? C101 C106 1.396(11) . ? C102 C103 1.385(16) . ? C103 C104 1.368(18) . ? C104 C105 1.342(17) . ? C105 C106 1.387(14) . ? C201 C202 1.389(12) . ? C201 C206 1.394(10) . ? C202 C203 1.408(13) . ? C203 C204 1.415(15) . ? C204 C205 1.374(16) . ? C205 C206 1.407(13) . ? C301 C302 1.397(11) . ? C301 C306 1.410(10) . ? C302 C303 1.382(12) . ? C303 C304 1.352(13) . ? C304 C305 1.360(13) . ? C305 C306 1.399(11) . ? C401 C402 1.390(11) . ? C401 C406 1.401(13) . ? C402 C403 1.398(16) . ? C403 C404 1.38(2) . ? C404 C405 1.337(17) . ? C405 C406 1.379(14) . ? 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 C13 Os1 C12 96.1(4) . . ? C13 Os1 C11 104.7(4) . . ? C12 Os1 C11 89.5(4) . . ? C13 Os1 P3 103.2(3) . . ? C12 Os1 P3 93.2(3) . . ? C11 Os1 P3 151.4(3) . . ? C13 Os1 P1 108.7(3) . . ? C12 Os1 P1 154.5(3) . . ? C11 Os1 P1 89.8(3) . . ? P3 Os1 P1 75.79(7) . . ? C13 Os1 Os2 151.4(3) . . ? C12 Os1 Os2 101.4(2) . . ? C11 Os1 Os2 97.8(3) . . ? P3 Os1 Os2 53.76(5) . . ? P1 Os1 Os2 53.50(4) . . ? C21 Os2 C23 98.7(5) . . ? C21 Os2 C22 96.3(4) . . ? C23 Os2 C22 91.6(4) . . ? C21 Os2 P1 112.5(3) . . ? C23 Os2 P1 89.8(2) . . ? C22 Os2 P1 150.7(3) . . ? C21 Os2 P3 107.2(3) . . ? C23 Os2 P3 153.6(3) . . ? C22 Os2 P3 90.8(3) . . ? P1 Os2 P3 75.65(7) . . ? C21 Os2 Os1 156.2(3) . . ? C23 Os2 Os1 100.3(3) . . ? C22 Os2 Os1 97.3(3) . . ? P1 Os2 Os1 53.72(5) . . ? P3 Os2 Os1 53.29(5) . . ? C32 Os3 C31 92.4(4) . . ? C32 Os3 C33 176.6(4) . . ? C31 Os3 C33 90.8(4) . . ? C32 Os3 P2 94.2(2) . . ? C31 Os3 P2 100.0(3) . . ? C33 Os3 P2 86.3(2) . . ? C32 Os3 Os5 92.1(2) . . ? C31 Os3 Os5 90.7(3) . . ? C33 Os3 Os5 86.9(2) . . ? P2 Os3 Os5 167.39(5) . . ? C32 Os3 Os4 82.2(3) . . ? C31 Os3 Os4 149.2(3) . . ? C33 Os3 Os4 94.5(3) . . ? P2 Os3 Os4 110.62(5) . . ? Os5 Os3 Os4 59.430(12) . . ? C41 Os4 C43 88.3(4) . . ? C41 Os4 C42 101.3(4) . . ? C43 Os4 C42 89.3(4) . . ? C41 Os4 C44 92.6(4) . . ? C43 Os4 C44 178.3(4) . . ? C42 Os4 C44 91.8(4) . . ? C41 Os4 Os5 96.6(3) . . ? C43 Os4 Os5 86.3(3) . . ? C42 Os4 Os5 161.4(3) . . ? C44 Os4 Os5 92.2(3) . . ? C41 Os4 Os3 156.1(3) . . ? C43 Os4 Os3 93.8(3) . . ? C42 Os4 Os3 102.5(3) . . ? C44 Os4 Os3 84.8(3) . . ? Os5 Os4 Os3 59.840(11) . . ? C52 Os5 C53 91.6(6) . . ? C52 Os5 C51 101.4(5) . . ? C53 Os5 C51 91.1(5) . . ? C52 Os5 C54 89.2(5) . . ? C53 Os5 C54 177.8(4) . . ? C51 Os5 C54 90.8(4) . . ? C52 Os5 Os4 163.0(3) . . ? C53 Os5 Os4 91.5(4) . . ? C51 Os5 Os4 95.2(4) . . ? C54 Os5 Os4 87.2(3) . . ? C52 Os5 Os3 102.8(3) . . ? C53 Os5 Os3 86.7(3) . . ? C51 Os5 Os3 155.8(4) . . ? C54 Os5 Os3 91.2(2) . . ? Os4 Os5 Os3 60.730(11) . . ? C101 P1 P2 102.0(3) . . ? C101 P1 Os2 118.3(3) . . ? P2 P1 Os2 121.30(10) . . ? C101 P1 Os1 122.2(3) . . ? P2 P1 Os1 119.99(11) . . ? Os2 P1 Os1 72.79(6) . . ? C201 P2 C301 100.7(4) . . ? C201 P2 P1 101.1(3) . . ? C301 P2 P1 105.1(3) . . ? C201 P2 Os3 114.5(3) . . ? C301 P2 Os3 116.7(2) . . ? P1 P2 Os3 116.47(10) . . ? C401 P3 C306 104.0(4) . . ? C401 P3 Os1 118.7(3) . . ? C306 P3 Os1 121.2(2) . . ? C401 P3 Os2 115.0(3) . . ? C306 P3 Os2 123.7(3) . . ? Os1 P3 Os2 72.95(6) . . ? C3 C1 C1 107(8) 1_455 2_654 ? C3 C1 C2 23(4) 1_455 . ? C1 C1 C2 122(7) 2_654 . ? C3 C1 C3 144(4) 1_455 2_754 ? C1 C1 C3 38(5) 2_654 2_754 ? C2 C1 C3 155(3) . 2_754 ? C3 C2 C1 24(4) 1_455 . ? C1 C3 C2 133(7) 1_655 1_655 ? C1 C3 C1 36(4) 1_655 2_754 ? C2 C3 C1 149(5) 1_655 2_754 ? O11 C11 Os1 175.3(8) . . ? O12 C12 Os1 178.3(9) . . ? O13 C13 Os1 178.4(9) . . ? O21 C21 Os2 176.6(9) . . ? O22 C22 Os2 175.8(9) . . ? O23 C23 Os2 176.2(10) . . ? O31 C31 Os3 175.4(8) . . ? O32 C32 Os3 176.3(8) . . ? O33 C33 Os3 176.6(7) . . ? O41 C41 Os4 178.5(10) . . ? O42 C42 Os4 178.1(10) . . ? O43 C43 Os4 174.4(9) . . ? O44 C44 Os4 176.0(9) . . ? O51 C51 Os5 178.1(11) . . ? O52 C52 Os5 179.6(11) . . ? O53 C53 Os5 174.3(11) . . ? O54 C54 Os5 174.8(8) . . ? C102 C101 C106 118.3(8) . . ? C102 C101 P1 119.3(6) . . ? C106 C101 P1 122.3(7) . . ? C101 C102 C103 120.6(9) . . ? C104 C103 C102 119.3(11) . . ? C105 C104 C103 121.6(11) . . ? C104 C105 C106 119.9(11) . . ? C105 C106 C101 120.2(10) . . ? C202 C201 C206 119.6(8) . . ? C202 C201 P2 121.0(6) . . ? C206 C201 P2 119.3(7) . . ? C201 C202 C203 122.5(9) . . ? C204 C203 C202 116.0(10) . . ? C205 C204 C203 122.3(9) . . ? C206 C205 C204 120.0(9) . . ? C205 C206 C201 119.4(9) . . ? C302 C301 C306 118.4(7) . . ? C302 C301 P2 111.8(6) . . ? C306 C301 P2 129.7(6) . . ? C303 C302 C301 121.9(9) . . ? C304 C303 C302 118.9(9) . . ? C303 C304 C305 121.1(9) . . ? C304 C305 C306 122.0(9) . . ? C305 C306 C301 117.5(7) . . ? C305 C306 P3 118.0(6) . . ? C301 C306 P3 124.4(6) . . ? C402 C401 C406 119.3(8) . . ? C402 C401 P3 120.1(7) . . ? C406 C401 P3 120.5(6) . . ? C401 C402 C403 119.1(11) . . ? C404 C403 C402 120.5(11) . . ? C405 C404 C403 119.3(10) . . ? C404 C405 C406 122.3(12) . . ? C405 C406 C401 119.0(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Os1 Os2 C21 2.3(9) . . . . ? C12 Os1 Os2 C21 -124.3(8) . . . . ? C11 Os1 Os2 C21 144.5(8) . . . . ? P3 Os1 Os2 C21 -38.8(7) . . . . ? P1 Os1 Os2 C21 60.6(7) . . . . ? C13 Os1 Os2 C23 -140.3(7) . . . . ? C12 Os1 Os2 C23 93.0(4) . . . . ? C11 Os1 Os2 C23 1.9(4) . . . . ? P3 Os1 Os2 C23 178.5(3) . . . . ? P1 Os1 Os2 C23 -82.0(3) . . . . ? C13 Os1 Os2 C22 126.7(7) . . . . ? C12 Os1 Os2 C22 0.1(4) . . . . ? C11 Os1 Os2 C22 -91.1(4) . . . . ? P3 Os1 Os2 C22 85.6(3) . . . . ? P1 Os1 Os2 C22 -175.0(3) . . . . ? C13 Os1 Os2 P1 -58.3(6) . . . . ? C12 Os1 Os2 P1 175.0(3) . . . . ? C11 Os1 Os2 P1 83.9(3) . . . . ? P3 Os1 Os2 P1 -99.43(9) . . . . ? C13 Os1 Os2 P3 41.2(6) . . . . ? C12 Os1 Os2 P3 -85.5(3) . . . . ? C11 Os1 Os2 P3 -176.6(3) . . . . ? P1 Os1 Os2 P3 99.43(9) . . . . ? C32 Os3 Os4 C41 -108.0(8) . . . . ? C31 Os3 Os4 C41 -26.4(9) . . . . ? C33 Os3 Os4 C41 72.8(8) . . . . ? P2 Os3 Os4 C41 160.5(7) . . . . ? Os5 Os3 Os4 C41 -10.9(7) . . . . ? C32 Os3 Os4 C43 -13.6(4) . . . . ? C31 Os3 Os4 C43 68.0(7) . . . . ? C33 Os3 Os4 C43 167.2(4) . . . . ? P2 Os3 Os4 C43 -105.1(3) . . . . ? Os5 Os3 Os4 C43 83.5(3) . . . . ? C32 Os3 Os4 C42 76.6(4) . . . . ? C31 Os3 Os4 C42 158.1(7) . . . . ? C33 Os3 Os4 C42 -102.6(4) . . . . ? P2 Os3 Os4 C42 -14.9(3) . . . . ? Os5 Os3 Os4 C42 173.7(3) . . . . ? C32 Os3 Os4 C44 167.3(4) . . . . ? C31 Os3 Os4 C44 -111.2(7) . . . . ? C33 Os3 Os4 C44 -11.9(4) . . . . ? P2 Os3 Os4 C44 75.8(3) . . . . ? Os5 Os3 Os4 C44 -95.6(3) . . . . ? C32 Os3 Os4 Os5 -97.1(2) . . . . ? C31 Os3 Os4 Os5 -15.5(6) . . . . ? C33 Os3 Os4 Os5 83.7(2) . . . . ? P2 Os3 Os4 Os5 171.40(6) . . . . ? C41 Os4 Os5 C52 160.4(13) . . . . ? C43 Os4 Os5 C52 -111.7(13) . . . . ? C42 Os4 Os5 C52 -34.9(16) . . . . ? C44 Os4 Os5 C52 67.5(13) . . . . ? Os3 Os4 Os5 C52 -15.1(13) . . . . ? C41 Os4 Os5 C53 -99.1(5) . . . . ? C43 Os4 Os5 C53 -11.2(4) . . . . ? C42 Os4 Os5 C53 65.5(10) . . . . ? C44 Os4 Os5 C53 168.0(4) . . . . ? Os3 Os4 Os5 C53 85.3(3) . . . . ? C41 Os4 Os5 C51 -7.9(5) . . . . ? C43 Os4 Os5 C51 80.0(4) . . . . ? C42 Os4 Os5 C51 156.7(10) . . . . ? C44 Os4 Os5 C51 -100.8(4) . . . . ? Os3 Os4 Os5 C51 176.5(4) . . . . ? C41 Os4 Os5 C54 82.6(4) . . . . ? C43 Os4 Os5 C54 170.5(4) . . . . ? C42 Os4 Os5 C54 -112.8(10) . . . . ? C44 Os4 Os5 C54 -10.3(4) . . . . ? Os3 Os4 Os5 C54 -93.0(3) . . . . ? C41 Os4 Os5 Os3 175.6(3) . . . . ? C43 Os4 Os5 Os3 -96.5(3) . . . . ? C42 Os4 Os5 Os3 -19.8(10) . . . . ? C44 Os4 Os5 Os3 82.7(2) . . . . ? C32 Os3 Os5 C52 -104.8(5) . . . . ? C31 Os3 Os5 C52 -12.4(5) . . . . ? C33 Os3 Os5 C52 78.4(5) . . . . ? P2 Os3 Os5 C52 135.6(4) . . . . ? Os4 Os3 Os5 C52 175.5(4) . . . . ? C32 Os3 Os5 C53 -13.9(5) . . . . ? C31 Os3 Os5 C53 78.5(5) . . . . ? C33 Os3 Os5 C53 169.3(5) . . . . ? P2 Os3 Os5 C53 -133.5(5) . . . . ? Os4 Os3 Os5 C53 -93.6(4) . . . . ? C32 Os3 Os5 C51 71.2(9) . . . . ? C31 Os3 Os5 C51 163.6(9) . . . . ? C33 Os3 Os5 C51 -105.6(9) . . . . ? P2 Os3 Os5 C51 -48.4(9) . . . . ? Os4 Os3 Os5 C51 -8.5(9) . . . . ? C32 Os3 Os5 C54 165.8(4) . . . . ? C31 Os3 Os5 C54 -101.8(5) . . . . ? C33 Os3 Os5 C54 -11.0(5) . . . . ? P2 Os3 Os5 C54 46.2(4) . . . . ? Os4 Os3 Os5 C54 86.1(3) . . . . ? C32 Os3 Os5 Os4 79.7(3) . . . . ? C31 Os3 Os5 Os4 172.1(3) . . . . ? C33 Os3 Os5 Os4 -97.1(3) . . . . ? P2 Os3 Os5 Os4 -39.9(2) . . . . ? C21 Os2 P1 C101 84.5(5) . . . . ? C23 Os2 P1 C101 -14.8(5) . . . . ? C22 Os2 P1 C101 -107.7(6) . . . . ? P3 Os2 P1 C101 -172.6(3) . . . . ? Os1 Os2 P1 C101 -117.9(3) . . . . ? C21 Os2 P1 P2 -42.6(4) . . . . ? C23 Os2 P1 P2 -141.9(3) . . . . ? C22 Os2 P1 P2 125.3(6) . . . . ? P3 Os2 P1 P2 60.37(12) . . . . ? Os1 Os2 P1 P2 115.09(13) . . . . ? C21 Os2 P1 Os1 -157.7(4) . . . . ? C23 Os2 P1 Os1 103.0(3) . . . . ? C22 Os2 P1 Os1 10.2(6) . . . . ? P3 Os2 P1 Os1 -54.71(6) . . . . ? C13 Os1 P1 C101 -92.4(4) . . . . ? C12 Os1 P1 C101 101.7(7) . . . . ? C11 Os1 P1 C101 13.1(4) . . . . ? P3 Os1 P1 C101 168.2(3) . . . . ? Os2 Os1 P1 C101 113.0(3) . . . . ? C13 Os1 P1 P2 37.9(3) . . . . ? C12 Os1 P1 P2 -128.0(6) . . . . ? C11 Os1 P1 P2 143.4(3) . . . . ? P3 Os1 P1 P2 -61.53(11) . . . . ? Os2 Os1 P1 P2 -116.69(12) . . . . ? C13 Os1 P1 Os2 154.6(3) . . . . ? C12 Os1 P1 Os2 -11.4(6) . . . . ? C11 Os1 P1 Os2 -99.9(2) . . . . ? P3 Os1 P1 Os2 55.16(6) . . . . ? C101 P1 P2 C201 -72.6(4) . . . . ? Os2 P1 P2 C201 61.5(3) . . . . ? Os1 P1 P2 C201 148.6(3) . . . . ? C101 P1 P2 C301 -177.0(4) . . . . ? Os2 P1 P2 C301 -42.9(3) . . . . ? Os1 P1 P2 C301 44.3(3) . . . . ? C101 P1 P2 Os3 52.1(3) . . . . ? Os2 P1 P2 Os3 -173.85(8) . . . . ? Os1 P1 P2 Os3 -86.66(12) . . . . ? C32 Os3 P2 C201 146.1(4) . . . . ? C31 Os3 P2 C201 53.0(4) . . . . ? C33 Os3 P2 C201 -37.2(4) . . . . ? Os5 Os3 P2 C201 -94.5(4) . . . . ? Os4 Os3 P2 C201 -130.6(3) . . . . ? C32 Os3 P2 C301 -96.7(4) . . . . ? C31 Os3 P2 C301 170.1(4) . . . . ? C33 Os3 P2 C301 79.9(4) . . . . ? Os5 Os3 P2 C301 22.7(4) . . . . ? Os4 Os3 P2 C301 -13.5(3) . . . . ? C32 Os3 P2 P1 28.5(3) . . . . ? C31 Os3 P2 P1 -64.6(3) . . . . ? C33 Os3 P2 P1 -154.8(3) . . . . ? Os5 Os3 P2 P1 147.94(19) . . . . ? Os4 Os3 P2 P1 111.78(10) . . . . ? C13 Os1 P3 C401 89.2(4) . . . . ? C12 Os1 P3 C401 -7.8(4) . . . . ? C11 Os1 P3 C401 -102.6(6) . . . . ? P1 Os1 P3 C401 -164.5(3) . . . . ? Os2 Os1 P3 C401 -109.6(3) . . . . ? C13 Os1 P3 C306 -41.6(4) . . . . ? C12 Os1 P3 C306 -138.6(4) . . . . ? C11 Os1 P3 C306 126.5(6) . . . . ? P1 Os1 P3 C306 64.7(3) . . . . ? Os2 Os1 P3 C306 119.5(3) . . . . ? C13 Os1 P3 Os2 -161.1(3) . . . . ? C12 Os1 P3 Os2 101.8(3) . . . . ? C11 Os1 P3 Os2 7.0(6) . . . . ? P1 Os1 P3 Os2 -54.88(6) . . . . ? C21 Os2 P3 C401 -81.0(4) . . . . ? C23 Os2 P3 C401 111.1(7) . . . . ? C22 Os2 P3 C401 15.8(4) . . . . ? P1 Os2 P3 C401 169.5(3) . . . . ? Os1 Os2 P3 C401 114.3(3) . . . . ? C21 Os2 P3 C306 48.1(4) . . . . ? C23 Os2 P3 C306 -119.8(7) . . . . ? C22 Os2 P3 C306 144.9(4) . . . . ? P1 Os2 P3 C306 -61.4(3) . . . . ? Os1 Os2 P3 C306 -116.6(3) . . . . ? C21 Os2 P3 Os1 164.7(3) . . . . ? C23 Os2 P3 Os1 -3.2(6) . . . . ? C22 Os2 P3 Os1 -98.5(3) . . . . ? P1 Os2 P3 Os1 55.17(6) . . . . ? C1 C1 C2 C3 -53(10) 2_654 . . 1_455 ? C3 C1 C2 C3 -81(12) 2_754 . . 1_455 ? C13 Os1 C11 O11 -176(11) . . . . ? C12 Os1 C11 O11 -80(11) . . . . ? P3 Os1 C11 O11 16(11) . . . . ? P1 Os1 C11 O11 75(11) . . . . ? Os2 Os1 C11 O11 21(11) . . . . ? C13 Os1 C12 O12 132(29) . . . . ? C11 Os1 C12 O12 27(29) . . . . ? P3 Os1 C12 O12 -124(29) . . . . ? P1 Os1 C12 O12 -61(29) . . . . ? Os2 Os1 C12 O12 -71(29) . . . . ? C12 Os1 C13 O13 5(34) . . . . ? C11 Os1 C13 O13 96(34) . . . . ? P3 Os1 C13 O13 -90(34) . . . . ? P1 Os1 C13 O13 -169(34) . . . . ? Os2 Os1 C13 O13 -123(34) . . . . ? C23 Os2 C21 O21 -97(17) . . . . ? C22 Os2 C21 O21 -4(17) . . . . ? P1 Os2 C21 O21 170(17) . . . . ? P3 Os2 C21 O21 88(17) . . . . ? Os1 Os2 C21 O21 120(17) . . . . ? C21 Os2 C22 O22 -158(12) . . . . ? C23 Os2 C22 O22 -59(12) . . . . ? P1 Os2 C22 O22 33(12) . . . . ? P3 Os2 C22 O22 94(12) . . . . ? Os1 Os2 C22 O22 41(12) . . . . ? C21 Os2 C23 O23 176(12) . . . . ? C22 Os2 C23 O23 79(12) . . . . ? P1 Os2 C23 O23 -72(12) . . . . ? P3 Os2 C23 O23 -16(12) . . . . ? Os1 Os2 C23 O23 -19(12) . . . . ? C32 Os3 C31 O31 88(12) . . . . ? C33 Os3 C31 O31 -91(12) . . . . ? P2 Os3 C31 O31 -177(12) . . . . ? Os5 Os3 C31 O31 -4(12) . . . . ? Os4 Os3 C31 O31 10(13) . . . . ? C31 Os3 C32 O32 32(12) . . . . ? C33 Os3 C32 O32 -165(10) . . . . ? P2 Os3 C32 O32 -68(12) . . . . ? Os5 Os3 C32 O32 123(12) . . . . ? Os4 Os3 C32 O32 -178(100) . . . . ? C32 Os3 C33 O33 103(15) . . . . ? C31 Os3 C33 O33 -95(15) . . . . ? P2 Os3 C33 O33 5(15) . . . . ? Os5 Os3 C33 O33 175(100) . . . . ? Os4 Os3 C33 O33 116(15) . . . . ? C43 Os4 C41 O41 53(37) . . . . ? C42 Os4 C41 O41 -36(37) . . . . ? C44 Os4 C41 O41 -128(37) . . . . ? Os5 Os4 C41 O41 140(37) . . . . ? Os3 Os4 C41 O41 149(37) . . . . ? C41 Os4 C42 O42 38(33) . . . . ? C43 Os4 C42 O42 -50(33) . . . . ? C44 Os4 C42 O42 131(33) . . . . ? Os5 Os4 C42 O42 -126(32) . . . . ? Os3 Os4 C42 O42 -144(33) . . . . ? C41 Os4 C43 O43 -25(10) . . . . ? C42 Os4 C43 O43 76(10) . . . . ? C44 Os4 C43 O43 -150(11) . . . . ? Os5 Os4 C43 O43 -122(10) . . . . ? Os3 Os4 C43 O43 178(100) . . . . ? C41 Os4 C44 O44 47(11) . . . . ? C43 Os4 C44 O44 171(11) . . . . ? C42 Os4 C44 O44 -54(11) . . . . ? Os5 Os4 C44 O44 144(11) . . . . ? Os3 Os4 C44 O44 -157(11) . . . . ? C52 Os5 C51 O51 129(39) . . . . ? C53 Os5 C51 O51 37(39) . . . . ? C54 Os5 C51 O51 -142(39) . . . . ? Os4 Os5 C51 O51 -55(39) . . . . ? Os3 Os5 C51 O51 -47(40) . . . . ? C53 Os5 C52 O52 17(100) . . . . ? C51 Os5 C52 O52 -75(100) . . . . ? C54 Os5 C52 O52 -165(100) . . . . ? Os4 Os5 C52 O52 117(100) . . . . ? Os3 Os5 C52 O52 104(100) . . . . ? C52 Os5 C53 O53 -34(13) . . . . ? C51 Os5 C53 O53 67(13) . . . . ? C54 Os5 C53 O53 -145(12) . . . . ? Os4 Os5 C53 O53 162(13) . . . . ? Os3 Os5 C53 O53 -137(13) . . . . ? C52 Os5 C54 O54 64(12) . . . . ? C53 Os5 C54 O54 175(33) . . . . ? C51 Os5 C54 O54 -37(12) . . . . ? Os4 Os5 C54 O54 -133(12) . . . . ? Os3 Os5 C54 O54 167(12) . . . . ? P2 P1 C101 C102 83.2(8) . . . . ? Os2 P1 C101 C102 -52.7(9) . . . . ? Os1 P1 C101 C102 -139.3(7) . . . . ? P2 P1 C101 C106 -100.0(7) . . . . ? Os2 P1 C101 C106 124.2(6) . . . . ? Os1 P1 C101 C106 37.5(8) . . . . ? C106 C101 C102 C103 2.7(16) . . . . ? P1 C101 C102 C103 179.7(9) . . . . ? C101 C102 C103 C104 -2.0(19) . . . . ? C102 C103 C104 C105 0(2) . . . . ? C103 C104 C105 C106 1(2) . . . . ? C104 C105 C106 C101 -0.1(16) . . . . ? C102 C101 C106 C105 -1.7(14) . . . . ? P1 C101 C106 C105 -178.5(7) . . . . ? C301 P2 C201 C202 -159.4(7) . . . . ? P1 P2 C201 C202 92.7(7) . . . . ? Os3 P2 C201 C202 -33.4(8) . . . . ? C301 P2 C201 C206 23.4(7) . . . . ? P1 P2 C201 C206 -84.5(7) . . . . ? Os3 P2 C201 C206 149.4(6) . . . . ? C206 C201 C202 C203 2.4(15) . . . . ? P2 C201 C202 C203 -174.8(8) . . . . ? C201 C202 C203 C204 -4.2(16) . . . . ? C202 C203 C204 C205 4.0(17) . . . . ? C203 C204 C205 C206 -2.0(18) . . . . ? C204 C205 C206 C201 -0.1(16) . . . . ? C202 C201 C206 C205 -0.1(13) . . . . ? P2 C201 C206 C205 177.1(7) . . . . ? C201 P2 C301 C302 72.3(6) . . . . ? P1 P2 C301 C302 177.0(5) . . . . ? Os3 P2 C301 C302 -52.2(6) . . . . ? C201 P2 C301 C306 -107.9(7) . . . . ? P1 P2 C301 C306 -3.1(8) . . . . ? Os3 P2 C301 C306 127.6(6) . . . . ? C306 C301 C302 C303 -2.7(12) . . . . ? P2 C301 C302 C303 177.3(7) . . . . ? C301 C302 C303 C304 0.7(14) . . . . ? C302 C303 C304 C305 0.6(16) . . . . ? C303 C304 C305 C306 0.3(16) . . . . ? C304 C305 C306 C301 -2.3(13) . . . . ? C304 C305 C306 P3 176.4(8) . . . . ? C302 C301 C306 C305 3.3(11) . . . . ? P2 C301 C306 C305 -176.5(6) . . . . ? C302 C301 C306 P3 -175.2(6) . . . . ? P2 C301 C306 P3 4.9(11) . . . . ? C401 P3 C306 C305 -4.3(7) . . . . ? Os1 P3 C306 C305 132.6(6) . . . . ? Os2 P3 C306 C305 -137.8(6) . . . . ? C401 P3 C306 C301 174.3(6) . . . . ? Os1 P3 C306 C301 -48.9(7) . . . . ? Os2 P3 C306 C301 40.7(7) . . . . ? C306 P3 C401 C402 -88.8(8) . . . . ? Os1 P3 C401 C402 133.0(7) . . . . ? Os2 P3 C401 C402 49.5(8) . . . . ? C306 P3 C401 C406 92.4(8) . . . . ? Os1 P3 C401 C406 -45.8(8) . . . . ? Os2 P3 C401 C406 -129.2(7) . . . . ? C406 C401 C402 C403 1.5(15) . . . . ? P3 C401 C402 C403 -177.3(10) . . . . ? C401 C402 C403 C404 3(2) . . . . ? C402 C403 C404 C405 -7(2) . . . . ? C403 C404 C405 C406 7.2(19) . . . . ? C404 C405 C406 C401 -2.8(17) . . . . ? C402 C401 C406 C405 -1.7(14) . . . . ? P3 C401 C406 C405 177.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.882 _diffrn_reflns_theta_full 29.34 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 2.214 _refine_diff_density_min -2.305 _refine_diff_density_rms 0.237 #=============================================== data_5 _database_code_CSD 158410 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H19 O9 Os3 P3' _chemical_formula_weight 1222.99 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' '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 16.17700(10) _cell_length_b 11.9969(2) _cell_length_c 19.4553(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.9670(10) _cell_angle_gamma 90.00 _cell_volume 3450.21(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 14122 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not measured _exptl_crystal_density_diffrn 2.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 11.213 _exptl_absorpt_correction_type sadabs (Sheldrick) _exptl_absorpt_correction_T_min 0.107563 _exptl_absorpt_correction_T_max 0.203296 _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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21779 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 29.32 _reflns_number_total 8461 _reflns_number_gt 6884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _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^)+(0.0193P)^2^+2.4368P] 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 SHELXL _refine_ls_extinction_coef 0.00035(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8461 _refine_ls_number_parameters 434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0543 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.005 _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 0.291413(11) 0.785668(14) 0.219415(10) 0.03465(5) Uani 1 1 d . . . C11 C 0.3310(3) 0.7773(5) 0.1400(3) 0.0505(13) Uani 1 1 d . . . O11 O 0.3570(3) 0.7724(4) 0.0938(3) 0.0836(14) Uani 1 1 d . . . C12 C 0.3974(3) 0.8670(4) 0.2825(3) 0.0472(12) Uani 1 1 d . . . O12 O 0.4614(3) 0.9141(4) 0.3189(3) 0.0772(13) Uani 1 1 d . . . C13 C 0.2151(3) 0.9142(4) 0.1955(3) 0.0495(12) Uani 1 1 d . . . O13 O 0.1689(3) 0.9903(3) 0.1830(2) 0.0800(13) Uani 1 1 d . . . P1 P 0.34803(7) 0.63252(9) 0.30201(6) 0.0326(2) Uani 1 1 d . . . C101 C 0.4700(3) 0.6132(3) 0.3483(3) 0.0369(10) Uani 1 1 d . . . C102 C 0.5131(3) 0.6074(5) 0.4254(3) 0.0542(13) Uani 1 1 d . . . H10A H 0.4793 0.6087 0.4543 0.065 Uiso 1 1 calc R . . C103 C 0.6059(4) 0.5995(6) 0.4601(3) 0.0700(17) Uani 1 1 d . . . H10B H 0.6346 0.5961 0.5123 0.084 Uiso 1 1 calc R . . C104 C 0.6557(4) 0.5967(5) 0.4178(4) 0.0697(18) Uani 1 1 d . . . H10C H 0.7184 0.5911 0.4415 0.084 Uiso 1 1 calc R . . C105 C 0.6147(4) 0.6020(5) 0.3411(4) 0.0612(15) Uani 1 1 d . . . H10D H 0.6491 0.5999 0.3127 0.073 Uiso 1 1 calc R . . C106 C 0.5213(3) 0.6107(4) 0.3060(3) 0.0478(12) Uani 1 1 d . . . H10E H 0.4930 0.6149 0.2538 0.057 Uiso 1 1 calc R . . P2 P 0.26896(7) 0.48434(9) 0.24860(6) 0.0317(2) Uani 1 1 d . . . C201 C 0.3127(3) 0.3529(4) 0.2960(2) 0.0360(10) Uani 1 1 d . . . C202 C 0.2505(4) 0.2710(4) 0.2923(3) 0.0569(14) Uani 1 1 d . . . H20A H 0.1891 0.2835 0.2645 0.068 Uiso 1 1 calc R . . C203 C 0.2793(4) 0.1711(5) 0.3294(4) 0.0699(17) Uani 1 1 d . . . H20B H 0.2374 0.1162 0.3263 0.084 Uiso 1 1 calc R . . C204 C 0.3695(4) 0.1527(5) 0.3709(3) 0.0659(16) Uani 1 1 d . . . H20C H 0.3889 0.0858 0.3966 0.079 Uiso 1 1 calc R . . C205 C 0.4302(4) 0.2319(5) 0.3743(4) 0.0676(17) Uani 1 1 d . . . H20D H 0.4915 0.2189 0.4023 0.081 Uiso 1 1 calc R . . C206 C 0.4027(3) 0.3325(4) 0.3368(3) 0.0518(13) Uani 1 1 d . . . H20E H 0.4454 0.3861 0.3394 0.062 Uiso 1 1 calc R . . Os2 Os 0.252108(11) 0.722303(15) 0.346309(10) 0.03560(5) Uani 1 1 d . . . C21 C 0.1606(3) 0.8338(5) 0.3227(3) 0.0527(13) Uani 1 1 d . . . O21 O 0.1091(3) 0.9057(4) 0.3072(3) 0.0817(13) Uani 1 1 d . . . C22 C 0.2351(3) 0.6380(4) 0.4217(3) 0.0470(12) Uani 1 1 d . . . O22 O 0.2257(3) 0.5899(4) 0.4684(2) 0.0728(12) Uani 1 1 d . . . C23 C 0.3445(4) 0.8141(4) 0.4142(3) 0.0493(12) Uani 1 1 d . . . O23 O 0.4014(3) 0.8680(4) 0.4571(2) 0.0716(11) Uani 1 1 d . . . Os3 Os 0.129217(11) 0.557253(14) 0.240597(9) 0.03307(5) Uani 1 1 d . . . C31 C 0.1235(4) 0.4673(5) 0.3212(3) 0.0514(13) Uani 1 1 d . . . O31 O 0.1190(4) 0.4125(4) 0.3667(3) 0.0978(17) Uani 1 1 d . . . C32 C 0.0316(3) 0.6515(5) 0.2401(3) 0.0533(13) Uani 1 1 d . . . O32 O -0.0269(3) 0.7045(4) 0.2391(3) 0.0836(14) Uani 1 1 d . . . C33 C 0.0586(3) 0.4554(4) 0.1629(3) 0.0435(11) Uani 1 1 d . . . O33 O 0.0160(3) 0.3965(4) 0.1163(2) 0.0712(12) Uani 1 1 d . . . P3 P 0.16385(7) 0.66543(10) 0.15143(6) 0.0323(2) Uani 1 1 d . . . C301 C 0.0689(3) 0.7292(4) 0.0738(2) 0.0385(10) Uani 1 1 d . . . C302 C 0.0836(3) 0.8131(4) 0.0312(3) 0.0505(13) Uani 1 1 d . . . H30A H 0.1423 0.8378 0.0431 0.061 Uiso 1 1 calc R . . C303 C 0.0131(4) 0.8611(5) -0.0287(3) 0.0618(15) Uani 1 1 d . . . H30B H 0.0243 0.9172 -0.0568 0.074 Uiso 1 1 calc R . . C304 C -0.0743(4) 0.8249(5) -0.0463(3) 0.0669(16) Uani 1 1 d . . . H30C H -0.1222 0.8560 -0.0869 0.080 Uiso 1 1 calc R . . C305 C -0.0904(4) 0.7435(5) -0.0043(3) 0.0672(17) Uani 1 1 d . . . H30D H -0.1494 0.7207 -0.0156 0.081 Uiso 1 1 calc R . . C306 C -0.0191(3) 0.6943(4) 0.0554(3) 0.0506(13) Uani 1 1 d . . . H30E H -0.0307 0.6378 0.0830 0.061 Uiso 1 1 calc R . . C401 C 0.2088(3) 0.5605(4) 0.1058(2) 0.0346(9) Uani 1 1 d . . . C402 C 0.2645(3) 0.4788(4) 0.1538(2) 0.0357(9) Uani 1 1 d . . . C403 C 0.3128(3) 0.4053(4) 0.1285(3) 0.0426(11) Uani 1 1 d . . . H40A H 0.3505 0.3520 0.1609 0.051 Uiso 1 1 calc R . . C404 C 0.3043(4) 0.4123(5) 0.0560(3) 0.0531(13) Uani 1 1 d . . . H40B H 0.3371 0.3641 0.0391 0.064 Uiso 1 1 calc R . . C405 C 0.2475(4) 0.4901(5) 0.0072(3) 0.0546(13) Uani 1 1 d . . . H40C H 0.2412 0.4922 -0.0425 0.066 Uiso 1 1 calc R . . C406 C 0.2005(3) 0.5642(4) 0.0312(3) 0.0446(11) Uani 1 1 d . . . H40D H 0.1631 0.6169 -0.0019 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.02965(9) 0.03231(9) 0.03892(10) 0.00705(7) 0.01078(7) 0.00134(7) C11 0.036(3) 0.059(3) 0.052(3) 0.011(3) 0.013(2) 0.001(2) O11 0.075(3) 0.118(4) 0.076(3) 0.013(3) 0.050(3) 0.007(3) C12 0.043(3) 0.038(3) 0.055(3) 0.008(2) 0.015(2) -0.002(2) O12 0.053(2) 0.069(3) 0.092(3) 0.001(2) 0.011(2) -0.021(2) C13 0.053(3) 0.039(3) 0.048(3) 0.010(2) 0.011(2) 0.006(2) O13 0.091(3) 0.051(3) 0.084(3) 0.014(2) 0.021(3) 0.034(2) P1 0.0285(5) 0.0319(6) 0.0354(6) 0.0036(4) 0.0109(5) 0.0033(4) C101 0.030(2) 0.028(2) 0.048(3) 0.0044(19) 0.0103(19) 0.0025(17) C102 0.041(3) 0.066(4) 0.048(3) 0.009(3) 0.012(2) 0.007(2) C103 0.044(3) 0.087(5) 0.058(4) 0.012(3) -0.001(3) 0.008(3) C104 0.030(3) 0.074(4) 0.090(5) 0.013(3) 0.009(3) 0.004(3) C105 0.047(3) 0.054(3) 0.093(5) 0.007(3) 0.039(3) 0.009(3) C106 0.039(3) 0.044(3) 0.060(3) 0.001(2) 0.019(2) 0.004(2) P2 0.0282(5) 0.0316(6) 0.0341(6) 0.0046(4) 0.0115(4) 0.0033(4) C201 0.038(2) 0.034(2) 0.036(2) 0.0063(18) 0.0145(19) 0.0054(18) C202 0.046(3) 0.041(3) 0.073(4) 0.011(3) 0.013(3) -0.001(2) C203 0.065(4) 0.045(3) 0.097(5) 0.017(3) 0.030(4) -0.010(3) C204 0.079(4) 0.045(3) 0.076(4) 0.023(3) 0.034(3) 0.013(3) C205 0.051(3) 0.057(4) 0.079(4) 0.022(3) 0.010(3) 0.014(3) C206 0.040(3) 0.042(3) 0.066(3) 0.016(2) 0.014(2) 0.004(2) Os2 0.03302(9) 0.03806(10) 0.03451(9) -0.00009(7) 0.01246(7) 0.00562(7) C21 0.049(3) 0.054(3) 0.058(3) 0.001(3) 0.024(3) 0.010(3) O21 0.071(3) 0.075(3) 0.104(4) 0.009(3) 0.041(3) 0.039(2) C22 0.046(3) 0.055(3) 0.040(3) 0.001(2) 0.018(2) 0.003(2) O22 0.095(3) 0.076(3) 0.057(2) 0.009(2) 0.041(2) 0.001(2) C23 0.053(3) 0.046(3) 0.044(3) 0.000(2) 0.014(2) 0.010(2) O23 0.067(3) 0.067(3) 0.063(2) -0.014(2) 0.009(2) -0.013(2) Os3 0.02701(8) 0.03731(10) 0.03613(9) 0.00325(7) 0.01410(7) 0.00092(7) C31 0.065(3) 0.051(3) 0.046(3) 0.000(2) 0.030(3) -0.009(3) O31 0.159(5) 0.082(3) 0.074(3) 0.007(3) 0.069(3) -0.032(3) C32 0.044(3) 0.062(4) 0.054(3) -0.003(3) 0.020(2) 0.002(3) O32 0.049(2) 0.099(4) 0.109(4) -0.006(3) 0.038(2) 0.030(2) C33 0.033(2) 0.051(3) 0.048(3) 0.001(2) 0.017(2) -0.002(2) O33 0.061(2) 0.077(3) 0.068(3) -0.024(2) 0.018(2) -0.015(2) P3 0.0279(5) 0.0342(6) 0.0332(6) 0.0055(4) 0.0106(4) 0.0033(4) C301 0.031(2) 0.041(3) 0.036(2) 0.0067(19) 0.0070(19) 0.0099(19) C302 0.041(3) 0.055(3) 0.049(3) 0.015(2) 0.011(2) 0.007(2) C303 0.071(4) 0.054(3) 0.050(3) 0.022(3) 0.013(3) 0.010(3) C304 0.058(4) 0.068(4) 0.055(3) 0.016(3) 0.003(3) 0.019(3) C305 0.037(3) 0.073(4) 0.068(4) 0.012(3) -0.003(3) 0.006(3) C306 0.039(3) 0.052(3) 0.049(3) 0.012(2) 0.006(2) 0.001(2) C401 0.034(2) 0.038(2) 0.034(2) -0.0014(18) 0.0161(18) -0.0010(18) C402 0.030(2) 0.038(2) 0.038(2) 0.0000(18) 0.0123(18) -0.0005(18) C403 0.038(2) 0.043(3) 0.049(3) 0.002(2) 0.020(2) 0.008(2) C404 0.057(3) 0.060(3) 0.053(3) -0.006(3) 0.034(3) 0.007(3) C405 0.067(3) 0.064(4) 0.041(3) -0.002(2) 0.030(3) 0.000(3) C406 0.045(3) 0.049(3) 0.040(3) 0.001(2) 0.018(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C11 1.900(6) . ? Os1 C13 1.910(5) . ? Os1 C12 1.920(5) . ? Os1 P1 2.3667(11) . ? Os1 P3 2.4231(11) . ? Os1 Os2 2.8900(2) . ? C11 O11 1.137(6) . ? C12 O12 1.139(6) . ? C13 O13 1.143(6) . ? P1 C101 1.821(4) . ? P1 P2 2.1900(16) . ? P1 Os2 2.3232(11) . ? C101 C102 1.376(6) . ? C101 C106 1.386(6) . ? C102 C103 1.376(7) . ? C103 C104 1.367(8) . ? C104 C105 1.367(8) . ? C105 C106 1.385(7) . ? P2 C402 1.818(4) . ? P2 C201 1.819(4) . ? P2 Os3 2.3693(11) . ? C201 C206 1.367(6) . ? C201 C202 1.386(6) . ? C202 C203 1.379(7) . ? C203 C204 1.368(8) . ? C204 C205 1.348(8) . ? C205 C206 1.387(7) . ? Os2 C23 1.894(5) . ? Os2 C22 1.892(5) . ? Os2 C21 1.907(5) . ? Os2 Os3 2.9633(2) . ? C21 O21 1.151(6) . ? C22 O22 1.136(6) . ? C23 O23 1.157(6) . ? Os3 C33 1.918(5) . ? Os3 C31 1.937(5) . ? Os3 C32 1.939(5) . ? Os3 P3 2.4078(11) . ? C31 O31 1.129(6) . ? C32 O32 1.134(6) . ? C33 O33 1.135(6) . ? P3 C301 1.827(4) . ? P3 C401 1.851(4) . ? C301 C306 1.384(6) . ? C301 C302 1.386(7) . ? C302 C303 1.381(7) . ? C303 C304 1.383(8) . ? C304 C305 1.365(8) . ? C305 C306 1.392(7) . ? C401 C402 1.400(6) . ? C401 C406 1.402(6) . ? C402 C403 1.393(6) . ? C403 C404 1.365(7) . ? C404 C405 1.380(7) . ? C405 C406 1.370(7) . ? 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 C11 Os1 C13 104.0(2) . . ? C11 Os1 C12 92.2(2) . . ? C13 Os1 C12 93.8(2) . . ? C11 Os1 P1 110.22(16) . . ? C13 Os1 P1 145.62(16) . . ? C12 Os1 P1 87.82(14) . . ? C11 Os1 P3 91.06(16) . . ? C13 Os1 P3 91.41(16) . . ? C12 Os1 P3 173.02(14) . . ? P1 Os1 P3 85.26(4) . . ? C11 Os1 Os2 160.80(16) . . ? C13 Os1 Os2 94.34(16) . . ? C12 Os1 Os2 92.11(15) . . ? P1 Os1 Os2 51.28(3) . . ? P3 Os1 Os2 82.86(3) . . ? O11 C11 Os1 178.3(5) . . ? O12 C12 Os1 178.2(5) . . ? O13 C13 Os1 178.0(5) . . ? C101 P1 P2 115.99(15) . . ? C101 P1 Os2 128.96(16) . . ? P2 P1 Os2 101.71(5) . . ? C101 P1 Os1 118.49(15) . . ? P2 P1 Os1 108.52(5) . . ? Os2 P1 Os1 76.08(3) . . ? C102 C101 C106 119.1(4) . . ? C102 C101 P1 120.8(4) . . ? C106 C101 P1 120.0(3) . . ? C101 C102 C103 120.4(5) . . ? C104 C103 C102 120.0(5) . . ? C103 C104 C105 120.8(5) . . ? C104 C105 C106 119.3(5) . . ? C105 C106 C101 120.4(5) . . ? C402 P2 C201 109.3(2) . . ? C402 P2 P1 106.60(15) . . ? C201 P2 P1 115.55(15) . . ? C402 P2 Os3 107.67(14) . . ? C201 P2 Os3 121.15(14) . . ? P1 P2 Os3 95.12(5) . . ? C206 C201 C202 118.9(4) . . ? C206 C201 P2 123.5(4) . . ? C202 C201 P2 117.6(3) . . ? C203 C202 C201 120.3(5) . . ? C204 C203 C202 120.1(5) . . ? C205 C204 C203 119.7(5) . . ? C204 C205 C206 121.1(5) . . ? C201 C206 C205 119.9(5) . . ? C23 Os2 C22 95.3(2) . . ? C23 Os2 C21 94.3(2) . . ? C22 Os2 C21 102.6(2) . . ? C23 Os2 P1 94.10(15) . . ? C22 Os2 P1 111.70(16) . . ? C21 Os2 P1 143.70(16) . . ? C23 Os2 Os1 93.29(16) . . ? C22 Os2 Os1 162.74(16) . . ? C21 Os2 Os1 91.64(16) . . ? P1 Os2 Os1 52.64(3) . . ? C23 Os2 Os3 171.66(15) . . ? C22 Os2 Os3 85.02(15) . . ? C21 Os2 Os3 93.75(17) . . ? P1 Os2 Os3 78.09(3) . . ? Os1 Os2 Os3 84.333(7) . . ? O21 C21 Os2 175.4(5) . . ? O22 C22 Os2 178.1(5) . . ? O23 C23 Os2 178.1(5) . . ? C33 Os3 C31 94.3(2) . . ? C33 Os3 C32 98.3(2) . . ? C31 Os3 C32 91.3(2) . . ? C33 Os3 P2 93.62(14) . . ? C31 Os3 P2 95.69(17) . . ? C32 Os3 P2 165.71(16) . . ? C33 Os3 P3 90.79(15) . . ? C31 Os3 P3 170.21(16) . . ? C32 Os3 P3 96.29(17) . . ? P2 Os3 P3 75.60(4) . . ? C33 Os3 Os2 171.63(14) . . ? C31 Os3 Os2 92.83(16) . . ? C32 Os3 Os2 85.97(16) . . ? P2 Os3 Os2 81.25(3) . . ? P3 Os3 Os2 81.55(3) . . ? O31 C31 Os3 178.0(5) . . ? O32 C32 Os3 178.4(5) . . ? O33 C33 Os3 178.9(5) . . ? C301 P3 C401 104.5(2) . . ? C301 P3 Os3 117.21(15) . . ? C401 P3 Os3 103.33(14) . . ? C301 P3 Os1 116.46(16) . . ? C401 P3 Os1 104.67(14) . . ? Os3 P3 Os1 108.87(4) . . ? C306 C301 C302 118.2(4) . . ? C306 C301 P3 121.2(4) . . ? C302 C301 P3 120.5(3) . . ? C303 C302 C301 121.6(5) . . ? C302 C303 C304 119.3(5) . . ? C305 C304 C303 120.0(5) . . ? C304 C305 C306 120.6(5) . . ? C301 C306 C305 120.3(5) . . ? C402 C401 C406 118.5(4) . . ? C402 C401 P3 115.4(3) . . ? C406 C401 P3 125.7(3) . . ? C403 C402 C401 120.6(4) . . ? C403 C402 P2 125.8(4) . . ? C401 C402 P2 113.6(3) . . ? C404 C403 C402 119.4(5) . . ? C403 C404 C405 120.7(5) . . ? C406 C405 C404 120.7(5) . . ? C405 C406 C401 120.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Os1 C11 O11 122(16) . . . . ? C12 Os1 C11 O11 28(16) . . . . ? P1 Os1 C11 O11 -60(16) . . . . ? P3 Os1 C11 O11 -146(16) . . . . ? Os2 Os1 C11 O11 -75(17) . . . . ? C11 Os1 C12 O12 -25(16) . . . . ? C13 Os1 C12 O12 -129(16) . . . . ? P1 Os1 C12 O12 85(16) . . . . ? P3 Os1 C12 O12 93(16) . . . . ? Os2 Os1 C12 O12 137(16) . . . . ? C11 Os1 C13 O13 175(100) . . . . ? C12 Os1 C13 O13 -91(15) . . . . ? P1 Os1 C13 O13 0(15) . . . . ? P3 Os1 C13 O13 84(15) . . . . ? Os2 Os1 C13 O13 1(15) . . . . ? C11 Os1 P1 C101 58.9(2) . . . . ? C13 Os1 P1 C101 -126.1(3) . . . . ? C12 Os1 P1 C101 -32.6(2) . . . . ? P3 Os1 P1 C101 148.31(18) . . . . ? Os2 Os1 P1 C101 -127.05(18) . . . . ? C11 Os1 P1 P2 -76.12(17) . . . . ? C13 Os1 P1 P2 98.8(3) . . . . ? C12 Os1 P1 P2 -167.64(16) . . . . ? P3 Os1 P1 P2 13.27(5) . . . . ? Os2 Os1 P1 P2 97.90(5) . . . . ? C11 Os1 P1 Os2 -174.02(16) . . . . ? C13 Os1 P1 Os2 0.9(3) . . . . ? C12 Os1 P1 Os2 94.46(15) . . . . ? P3 Os1 P1 Os2 -84.64(3) . . . . ? P2 P1 C101 C102 -104.3(4) . . . . ? Os2 P1 C101 C102 28.9(5) . . . . ? Os1 P1 C101 C102 123.9(4) . . . . ? P2 P1 C101 C106 79.4(4) . . . . ? Os2 P1 C101 C106 -147.4(3) . . . . ? Os1 P1 C101 C106 -52.4(4) . . . . ? C106 C101 C102 C103 0.2(8) . . . . ? P1 C101 C102 C103 -176.1(5) . . . . ? C101 C102 C103 C104 -0.5(9) . . . . ? C102 C103 C104 C105 0.3(10) . . . . ? C103 C104 C105 C106 0.2(9) . . . . ? C104 C105 C106 C101 -0.4(8) . . . . ? C102 C101 C106 C105 0.2(7) . . . . ? P1 C101 C106 C105 176.5(4) . . . . ? C101 P1 P2 C402 -87.3(2) . . . . ? Os2 P1 P2 C402 128.05(15) . . . . ? Os1 P1 P2 C402 48.99(15) . . . . ? C101 P1 P2 C201 34.3(2) . . . . ? Os2 P1 P2 C201 -110.32(16) . . . . ? Os1 P1 P2 C201 170.62(16) . . . . ? C101 P1 P2 Os3 162.52(17) . . . . ? Os2 P1 P2 Os3 17.89(5) . . . . ? Os1 P1 P2 Os3 -61.18(5) . . . . ? C402 P2 C201 C206 89.5(4) . . . . ? P1 P2 C201 C206 -30.6(5) . . . . ? Os3 P2 C201 C206 -144.5(4) . . . . ? C402 P2 C201 C202 -92.6(4) . . . . ? P1 P2 C201 C202 147.2(4) . . . . ? Os3 P2 C201 C202 33.3(5) . . . . ? C206 C201 C202 C203 0.4(8) . . . . ? P2 C201 C202 C203 -177.6(5) . . . . ? C201 C202 C203 C204 0.6(10) . . . . ? C202 C203 C204 C205 -1.0(10) . . . . ? C203 C204 C205 C206 0.4(10) . . . . ? C202 C201 C206 C205 -0.9(8) . . . . ? P2 C201 C206 C205 176.9(4) . . . . ? C204 C205 C206 C201 0.6(10) . . . . ? C101 P1 Os2 C23 24.6(2) . . . . ? P2 P1 Os2 C23 162.56(16) . . . . ? Os1 P1 Os2 C23 -91.01(16) . . . . ? C101 P1 Os2 C22 -72.8(2) . . . . ? P2 P1 Os2 C22 65.19(17) . . . . ? Os1 P1 Os2 C22 171.62(16) . . . . ? C101 P1 Os2 C21 127.5(3) . . . . ? P2 P1 Os2 C21 -94.4(3) . . . . ? Os1 P1 Os2 C21 12.0(3) . . . . ? C101 P1 Os2 Os1 115.57(19) . . . . ? P2 P1 Os2 Os1 -106.43(5) . . . . ? C101 P1 Os2 Os3 -152.48(19) . . . . ? P2 P1 Os2 Os3 -14.48(4) . . . . ? Os1 P1 Os2 Os3 91.95(2) . . . . ? C11 Os1 Os2 C23 109.9(5) . . . . ? C13 Os1 Os2 C23 -86.8(2) . . . . ? C12 Os1 Os2 C23 7.1(2) . . . . ? P1 Os1 Os2 C23 92.65(15) . . . . ? P3 Os1 Os2 C23 -177.71(15) . . . . ? C11 Os1 Os2 C22 -9.9(7) . . . . ? C13 Os1 Os2 C22 153.4(5) . . . . ? C12 Os1 Os2 C22 -112.7(5) . . . . ? P1 Os1 Os2 C22 -27.2(5) . . . . ? P3 Os1 Os2 C22 62.5(5) . . . . ? C11 Os1 Os2 C21 -155.7(5) . . . . ? C13 Os1 Os2 C21 7.6(2) . . . . ? C12 Os1 Os2 C21 101.6(2) . . . . ? P1 Os1 Os2 C21 -172.94(17) . . . . ? P3 Os1 Os2 C21 -83.30(17) . . . . ? C11 Os1 Os2 P1 17.3(5) . . . . ? C13 Os1 Os2 P1 -179.48(16) . . . . ? C12 Os1 Os2 P1 -85.51(15) . . . . ? P3 Os1 Os2 P1 89.64(4) . . . . ? C11 Os1 Os2 Os3 -62.0(5) . . . . ? C13 Os1 Os2 Os3 101.20(15) . . . . ? C12 Os1 Os2 Os3 -164.83(15) . . . . ? P1 Os1 Os2 Os3 -79.33(3) . . . . ? P3 Os1 Os2 Os3 10.31(3) . . . . ? C23 Os2 C21 O21 55(6) . . . . ? C22 Os2 C21 O21 151(6) . . . . ? P1 Os2 C21 O21 -48(7) . . . . ? Os1 Os2 C21 O21 -38(6) . . . . ? Os3 Os2 C21 O21 -123(6) . . . . ? C23 Os2 C22 O22 27(14) . . . . ? C21 Os2 C22 O22 -68(14) . . . . ? P1 Os2 C22 O22 124(14) . . . . ? Os1 Os2 C22 O22 147(14) . . . . ? Os3 Os2 C22 O22 -161(14) . . . . ? C22 Os2 C23 O23 24(15) . . . . ? C21 Os2 C23 O23 127(15) . . . . ? P1 Os2 C23 O23 -88(15) . . . . ? Os1 Os2 C23 O23 -141(15) . . . . ? Os3 Os2 C23 O23 -68(15) . . . . ? C402 P2 Os3 C33 50.3(2) . . . . ? C201 P2 Os3 C33 -76.4(2) . . . . ? P1 P2 Os3 C33 159.54(15) . . . . ? C402 P2 Os3 C31 145.0(2) . . . . ? C201 P2 Os3 C31 18.3(2) . . . . ? P1 P2 Os3 C31 -105.80(16) . . . . ? C402 P2 Os3 C32 -96.2(7) . . . . ? C201 P2 Os3 C32 137.1(7) . . . . ? P1 P2 Os3 C32 13.0(7) . . . . ? C402 P2 Os3 P3 -39.59(15) . . . . ? C201 P2 Os3 P3 -166.28(18) . . . . ? P1 P2 Os3 P3 69.65(5) . . . . ? C402 P2 Os3 Os2 -123.05(15) . . . . ? C201 P2 Os3 Os2 110.27(17) . . . . ? P1 P2 Os3 Os2 -13.80(4) . . . . ? C23 Os2 Os3 C33 -60.2(15) . . . . ? C22 Os2 Os3 C33 -152.8(10) . . . . ? C21 Os2 Os3 C33 104.9(10) . . . . ? P1 Os2 Os3 C33 -39.4(10) . . . . ? Os1 Os2 Os3 C33 13.6(10) . . . . ? C23 Os2 Os3 C31 87.7(11) . . . . ? C22 Os2 Os3 C31 -4.9(2) . . . . ? C21 Os2 Os3 C31 -107.2(2) . . . . ? P1 Os2 Os3 C31 108.56(17) . . . . ? Os1 Os2 Os3 C31 161.53(17) . . . . ? C23 Os2 Os3 C32 179(14) . . . . ? C22 Os2 Os3 C32 86.2(2) . . . . ? C21 Os2 Os3 C32 -16.1(2) . . . . ? P1 Os2 Os3 C32 -160.36(17) . . . . ? Os1 Os2 Os3 C32 -107.39(17) . . . . ? C23 Os2 Os3 P2 -7.6(11) . . . . ? C22 Os2 Os3 P2 -100.20(15) . . . . ? C21 Os2 Os3 P2 157.48(16) . . . . ? P1 Os2 Os3 P2 13.23(4) . . . . ? Os1 Os2 Os3 P2 66.20(3) . . . . ? C23 Os2 Os3 P3 -84.2(11) . . . . ? C22 Os2 Os3 P3 -176.81(15) . . . . ? C21 Os2 Os3 P3 80.87(16) . . . . ? P1 Os2 Os3 P3 -63.38(4) . . . . ? Os1 Os2 Os3 P3 -10.41(3) . . . . ? C33 Os3 C31 O31 6(17) . . . . ? C32 Os3 C31 O31 105(17) . . . . ? P2 Os3 C31 O31 -88(17) . . . . ? P3 Os3 C31 O31 -115(16) . . . . ? Os2 Os3 C31 O31 -169(16) . . . . ? C33 Os3 C32 O32 25(19) . . . . ? C31 Os3 C32 O32 -70(19) . . . . ? P2 Os3 C32 O32 171(100) . . . . ? P3 Os3 C32 O32 116(19) . . . . ? Os2 Os3 C32 O32 -163(19) . . . . ? C31 Os3 C33 O33 127(24) . . . . ? C32 Os3 C33 O33 35(24) . . . . ? P2 Os3 C33 O33 -137(24) . . . . ? P3 Os3 C33 O33 -62(24) . . . . ? Os2 Os3 C33 O33 -85(24) . . . . ? C33 Os3 P3 C301 61.7(2) . . . . ? C31 Os3 P3 C301 -177.2(9) . . . . ? C32 Os3 P3 C301 -36.8(2) . . . . ? P2 Os3 P3 C301 155.19(18) . . . . ? Os2 Os3 P3 C301 -121.74(17) . . . . ? C33 Os3 P3 C401 -52.6(2) . . . . ? C31 Os3 P3 C401 68.5(10) . . . . ? C32 Os3 P3 C401 -151.1(2) . . . . ? P2 Os3 P3 C401 40.89(14) . . . . ? Os2 Os3 P3 C401 123.96(14) . . . . ? C33 Os3 P3 Os1 -163.50(14) . . . . ? C31 Os3 P3 Os1 -42.4(9) . . . . ? C32 Os3 P3 Os1 98.06(16) . . . . ? P2 Os3 P3 Os1 -69.97(4) . . . . ? Os2 Os3 P3 Os1 13.10(3) . . . . ? C11 Os1 P3 C301 -76.5(2) . . . . ? C13 Os1 P3 C301 27.6(2) . . . . ? C12 Os1 P3 C301 165.9(13) . . . . ? P1 Os1 P3 C301 173.34(17) . . . . ? Os2 Os1 P3 C301 121.82(17) . . . . ? C11 Os1 P3 C401 38.4(2) . . . . ? C13 Os1 P3 C401 142.4(2) . . . . ? C12 Os1 P3 C401 -79.3(13) . . . . ? P1 Os1 P3 C401 -71.83(15) . . . . ? Os2 Os1 P3 C401 -123.36(14) . . . . ? C11 Os1 P3 Os3 148.33(16) . . . . ? C13 Os1 P3 Os3 -107.60(16) . . . . ? C12 Os1 P3 Os3 30.7(13) . . . . ? P1 Os1 P3 Os3 38.13(4) . . . . ? Os2 Os1 P3 Os3 -13.40(3) . . . . ? C401 P3 C301 C306 97.2(4) . . . . ? Os3 P3 C301 C306 -16.5(5) . . . . ? Os1 P3 C301 C306 -147.9(4) . . . . ? C401 P3 C301 C302 -82.0(5) . . . . ? Os3 P3 C301 C302 164.4(4) . . . . ? Os1 P3 C301 C302 32.9(5) . . . . ? C306 C301 C302 C303 -0.5(8) . . . . ? P3 C301 C302 C303 178.7(4) . . . . ? C301 C302 C303 C304 0.3(9) . . . . ? C302 C303 C304 C305 0.8(10) . . . . ? C303 C304 C305 C306 -1.6(10) . . . . ? C302 C301 C306 C305 -0.4(8) . . . . ? P3 C301 C306 C305 -179.5(4) . . . . ? C304 C305 C306 C301 1.4(9) . . . . ? C301 P3 C401 C402 -162.4(3) . . . . ? Os3 P3 C401 C402 -39.2(3) . . . . ? Os1 P3 C401 C402 74.7(3) . . . . ? C301 P3 C401 C406 25.6(4) . . . . ? Os3 P3 C401 C406 148.7(4) . . . . ? Os1 P3 C401 C406 -97.4(4) . . . . ? C406 C401 C402 C403 2.0(6) . . . . ? P3 C401 C402 C403 -170.6(3) . . . . ? C406 C401 C402 P2 179.9(3) . . . . ? P3 C401 C402 P2 7.2(4) . . . . ? C201 P2 C402 C403 -19.8(5) . . . . ? P1 P2 C402 C403 105.8(4) . . . . ? Os3 P2 C402 C403 -153.1(4) . . . . ? C201 P2 C402 C401 162.5(3) . . . . ? P1 P2 C402 C401 -71.9(3) . . . . ? Os3 P2 C402 C401 29.2(3) . . . . ? C401 C402 C403 C404 -1.0(7) . . . . ? P2 C402 C403 C404 -178.6(4) . . . . ? C402 C403 C404 C405 -1.0(8) . . . . ? C403 C404 C405 C406 1.9(8) . . . . ? C404 C405 C406 C401 -0.9(8) . . . . ? C402 C401 C406 C405 -1.1(7) . . . . ? P3 C401 C406 C405 170.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 29.32 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.918 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.118 END