Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Sergey Tunik' _publ_contact_author_address ; Department of Chemistry St. Petersburg State University Universitetskii pr., 26 St. Petersburg 198504 RUSSIAN FEDERATION ; _publ_contact_author_email STUNIK@CHEM.SPBU.RU _publ_section_title ; Reactions of 2,4-hexadiyne-1,6-diol with [H2Os3(CO)9(PR3)] Clusters. Cyclization of the Diyne and Reversible Exchange of the Phosphine Ligands between different positions of the Os3C3 framework. ; loop_ _publ_author_name 'Sergey Tunik' 'Matti Haukka' 'Vassily D. Khripun' 'Tapani A. Pakkanen' data_IV _database_code_depnum_ccdc_archive 'CCDC 228035' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common H2Os3(CO)9(P(C6H4MeF3)3) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H14 F9 O9 Os3 P' _chemical_formula_weight 1290.98 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' P P 0.1023 0.0942 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5872(3) _cell_length_b 11.7642(4) _cell_length_c 14.5257(4) _cell_angle_alpha 82.587(2) _cell_angle_beta 81.071(2) _cell_angle_gamma 77.165(2) _cell_volume 1734.18(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description black _exptl_crystal_colour block _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 11.108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.05194 _exptl_absorpt_correction_T_max 0.15756 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.12 (Bruker AXS, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19072 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 27.45 _reflns_number_total 7798 _reflns_number_gt 6999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Hydride hydrogen was located with XHYDEX program and not refined. Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0271P)^2^+2.8821P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7798 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2552(5) 0.1675(5) 0.4273(4) 0.0267(10) Uani 1 1 d . . . C2 C -0.3549(5) 0.3482(5) 0.5477(4) 0.0279(11) Uani 1 1 d . . . C3 C -0.4153(6) 0.3710(5) 0.3508(4) 0.0359(13) Uani 1 1 d . . . C4 C -0.2454(5) 0.4976(4) 0.4093(3) 0.0240(10) Uani 1 1 d . . . C5 C -0.0294(5) 0.1402(4) 0.5398(3) 0.0237(10) Uani 1 1 d . . . C6 C 0.1850(5) 0.2279(5) 0.4404(3) 0.0266(11) Uani 1 1 d . . . C7 C -0.0416(5) 0.3672(4) 0.5427(4) 0.0251(10) Uani 1 1 d . . . C10 C -0.1595(5) 0.2380(4) 0.2024(4) 0.0266(11) Uani 1 1 d . . . C12 C -0.1397(5) 0.4542(4) 0.2071(3) 0.0249(10) Uani 1 1 d . . . C20 C 0.1116(5) 0.2341(4) 0.0569(3) 0.0226(10) Uani 1 1 d . . . C21 C 0.0213(5) 0.3097(4) 0.0043(3) 0.0256(10) Uani 1 1 d . . . H21 H -0.0253 0.3815 0.0270 0.031 Uiso 1 1 calc R . . C22 C -0.0011(5) 0.2811(5) -0.0804(4) 0.0273(11) Uani 1 1 d . . . H22 H -0.0612 0.3340 -0.1160 0.033 Uiso 1 1 calc R . . C23 C 0.0641(5) 0.1754(5) -0.1134(3) 0.0259(10) Uani 1 1 d . . . C24 C 0.1530(6) 0.0995(5) -0.0622(4) 0.0343(13) Uani 1 1 d . . . H24 H 0.1979 0.0272 -0.0850 0.041 Uiso 1 1 calc R . . C25 C 0.1775(6) 0.1286(5) 0.0231(4) 0.0334(12) Uani 1 1 d . . . H25 H 0.2391 0.0762 0.0578 0.040 Uiso 1 1 calc R . . C26 C 0.2084(5) 0.4044(4) 0.1364(3) 0.0204(9) Uani 1 1 d . . . C27 C 0.0348(5) 0.1484(5) -0.2053(4) 0.0302(11) Uani 1 1 d . . . C28 C 0.2548(5) 0.4367(4) 0.0443(3) 0.0230(10) Uani 1 1 d . . . H28 H 0.2443 0.3941 -0.0043 0.028 Uiso 1 1 calc R . . C29 C 0.3170(5) 0.5318(4) 0.0230(4) 0.0280(11) Uani 1 1 d . . . H29 H 0.3472 0.5546 -0.0403 0.034 Uiso 1 1 calc R . . C30 C 0.3348(5) 0.5931(4) 0.0938(4) 0.0271(11) Uani 1 1 d . . . C31 C 0.2911(5) 0.5592(4) 0.1865(4) 0.0266(10) Uani 1 1 d . . . H31 H 0.3052 0.5994 0.2354 0.032 Uiso 1 1 calc R . . C32 C 0.2271(5) 0.4665(4) 0.2072(3) 0.0227(10) Uani 1 1 d . . . H32 H 0.1955 0.4448 0.2705 0.027 Uiso 1 1 calc R . . C33 C 0.2630(5) 0.1633(4) 0.2105(3) 0.0211(9) Uani 1 1 d . . . C34 C 0.4015(6) 0.6944(5) 0.0733(5) 0.0431(15) Uani 1 1 d . . . C35 C 0.3895(5) 0.1813(5) 0.2061(3) 0.0249(10) Uani 1 1 d . . . H35 H 0.4108 0.2538 0.1794 0.030 Uiso 1 1 calc R . . C36 C 0.4854(5) 0.0906(5) 0.2419(4) 0.0269(11) Uani 1 1 d . . . H36 H 0.5713 0.1030 0.2406 0.032 Uiso 1 1 calc R . . C37 C 0.4564(5) -0.0154(4) 0.2787(4) 0.0248(10) Uani 1 1 d . . . C38 C 0.3293(5) -0.0342(4) 0.2817(4) 0.0259(10) Uani 1 1 d . . . H38 H 0.3089 -0.1079 0.3060 0.031 Uiso 1 1 calc R . . C39 C 0.2345(5) 0.0555(4) 0.2490(4) 0.0253(10) Uani 1 1 d . . . H39 H 0.1479 0.0438 0.2527 0.030 Uiso 1 1 calc R . . C40 C 0.5560(5) -0.1119(5) 0.3180(4) 0.0321(12) Uani 1 1 d . . . P1 P 0.13077(12) 0.27765(11) 0.16924(8) 0.0192(2) Uani 1 1 d . . . O1 O -0.2472(4) 0.0688(3) 0.4325(3) 0.0374(9) Uani 1 1 d . . . O2 O -0.4035(4) 0.3588(4) 0.6229(3) 0.0429(10) Uani 1 1 d . . . O4 O -0.2317(4) 0.5921(3) 0.4040(3) 0.0352(9) Uani 1 1 d . . . O5 O -0.0464(4) 0.0652(3) 0.5943(2) 0.0295(8) Uani 1 1 d . . . O6 O 0.2938(4) 0.2077(4) 0.4408(3) 0.0383(10) Uani 1 1 d . . . O7 O -0.0692(4) 0.4299(3) 0.6001(2) 0.0307(8) Uani 1 1 d . . . O10 O -0.2186(4) 0.1949(3) 0.1626(3) 0.0337(9) Uani 1 1 d . . . O12 O -0.1856(4) 0.5437(3) 0.1718(3) 0.0374(9) Uani 1 1 d . . . O3 O -0.4999(5) 0.3882(4) 0.3079(4) 0.0594(15) Uani 1 1 d . . . F1 F -0.0936(3) 0.1632(4) -0.2078(3) 0.0579(12) Uani 1 1 d . . . F2 F 0.0768(4) 0.2190(3) -0.2769(2) 0.0416(8) Uani 1 1 d . . . F3 F 0.0882(4) 0.0394(3) -0.2242(2) 0.0427(9) Uani 1 1 d . . . F4 F 0.4446(4) 0.7151(3) -0.0174(3) 0.0528(10) Uani 1 1 d . . . F5 F 0.5109(5) 0.6736(4) 0.1153(3) 0.0698(13) Uani 1 1 d . . . F6 F 0.3294(6) 0.7907(4) 0.1017(5) 0.132(3) Uani 1 1 d . . . F7 F 0.6666(3) -0.0781(3) 0.3227(4) 0.0598(12) Uani 1 1 d . . . F8 F 0.5879(4) -0.2026(3) 0.2669(3) 0.0505(10) Uani 1 1 d . . . F9 F 0.5145(4) -0.1550(3) 0.4049(3) 0.0460(9) Uani 1 1 d . . . Os1 Os -0.269893(18) 0.336671(16) 0.421709(12) 0.01994(6) Uani 1 1 d . . . Os2 Os -0.067190(17) 0.310999(15) 0.270695(12) 0.01777(5) Uani 1 1 d . . . Os3 Os -0.004250(17) 0.265481(15) 0.446366(12) 0.01758(5) Uani 1 1 d . . . H01 H -0.0009 0.1801 0.3473 0.050 Uiso 1 1 d . . . H02 H 0.0103 0.3805 0.3480 0.050 Uiso 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 C1 0.026(3) 0.031(3) 0.024(2) 0.000(2) -0.008(2) -0.005(2) C2 0.030(3) 0.027(3) 0.029(3) -0.001(2) -0.005(2) -0.011(2) C3 0.036(3) 0.031(3) 0.040(3) -0.008(2) -0.010(3) -0.002(2) C4 0.018(2) 0.029(3) 0.023(2) -0.0010(19) -0.0034(19) -0.001(2) C5 0.029(3) 0.026(2) 0.018(2) -0.0090(19) -0.005(2) -0.005(2) C6 0.033(3) 0.033(3) 0.016(2) -0.0033(19) -0.009(2) -0.006(2) C7 0.023(2) 0.026(2) 0.026(2) 0.006(2) -0.006(2) -0.009(2) C10 0.023(2) 0.027(3) 0.027(3) 0.001(2) -0.003(2) 0.000(2) C12 0.028(3) 0.029(3) 0.019(2) -0.0049(19) -0.001(2) -0.008(2) C20 0.022(2) 0.024(2) 0.022(2) -0.0039(18) 0.0001(19) -0.006(2) C21 0.030(3) 0.023(2) 0.024(2) -0.0056(19) -0.006(2) -0.001(2) C22 0.029(3) 0.029(3) 0.024(2) -0.002(2) -0.006(2) -0.004(2) C23 0.024(2) 0.034(3) 0.020(2) -0.004(2) -0.003(2) -0.007(2) C24 0.043(3) 0.032(3) 0.028(3) -0.011(2) -0.010(2) -0.001(3) C25 0.040(3) 0.031(3) 0.028(3) -0.006(2) -0.011(2) 0.001(2) C26 0.024(2) 0.017(2) 0.021(2) -0.0013(17) -0.0073(19) -0.0036(19) C27 0.028(3) 0.038(3) 0.026(3) -0.010(2) -0.006(2) -0.004(2) C28 0.023(2) 0.025(2) 0.020(2) -0.0024(18) -0.0012(19) -0.005(2) C29 0.029(3) 0.027(3) 0.026(3) 0.000(2) 0.003(2) -0.007(2) C30 0.027(3) 0.021(2) 0.034(3) -0.003(2) -0.001(2) -0.008(2) C31 0.028(3) 0.023(2) 0.031(3) -0.003(2) -0.013(2) -0.005(2) C32 0.026(2) 0.022(2) 0.018(2) 0.0032(17) -0.003(2) -0.004(2) C33 0.023(2) 0.024(2) 0.016(2) -0.0015(17) -0.0034(19) -0.0046(19) C34 0.047(4) 0.035(3) 0.047(4) -0.009(3) 0.014(3) -0.018(3) C35 0.025(2) 0.029(3) 0.021(2) 0.0000(19) -0.004(2) -0.008(2) C36 0.020(2) 0.032(3) 0.030(3) -0.002(2) -0.004(2) -0.008(2) C37 0.021(2) 0.028(3) 0.026(2) -0.006(2) -0.005(2) -0.004(2) C38 0.028(3) 0.023(2) 0.029(3) 0.0009(19) -0.008(2) -0.008(2) C39 0.024(2) 0.028(3) 0.026(2) -0.0012(19) -0.006(2) -0.007(2) C40 0.024(3) 0.031(3) 0.042(3) -0.002(2) -0.012(2) -0.004(2) P1 0.0215(6) 0.0213(6) 0.0157(5) -0.0010(4) -0.0044(5) -0.0055(5) O1 0.039(2) 0.026(2) 0.049(2) -0.0033(17) -0.0072(19) -0.0094(17) O2 0.051(3) 0.051(3) 0.029(2) -0.0102(18) 0.011(2) -0.023(2) O4 0.039(2) 0.026(2) 0.041(2) -0.0034(16) -0.0076(18) -0.0047(17) O5 0.042(2) 0.0262(18) 0.0194(17) 0.0047(14) -0.0043(16) -0.0094(17) O6 0.022(2) 0.058(3) 0.035(2) -0.0080(19) -0.0077(17) -0.0024(18) O7 0.046(2) 0.0251(18) 0.0228(18) -0.0094(14) -0.0039(17) -0.0087(17) O10 0.037(2) 0.039(2) 0.033(2) -0.0033(17) -0.0153(17) -0.0150(18) O12 0.050(2) 0.029(2) 0.027(2) 0.0044(16) -0.0102(18) 0.0047(18) O3 0.053(3) 0.042(3) 0.093(4) -0.012(3) -0.055(3) 0.003(2) F1 0.0359(19) 0.100(3) 0.049(2) -0.043(2) -0.0099(17) -0.013(2) F2 0.060(2) 0.0423(19) 0.0232(16) -0.0029(14) -0.0141(16) -0.0056(17) F3 0.068(2) 0.0341(18) 0.0281(17) -0.0123(14) -0.0145(17) -0.0050(17) F4 0.061(2) 0.047(2) 0.053(2) 0.0087(17) 0.001(2) -0.029(2) F5 0.083(3) 0.091(3) 0.058(3) -0.008(2) -0.011(2) -0.062(3) F6 0.103(4) 0.033(2) 0.237(8) -0.054(3) 0.115(5) -0.036(3) F7 0.0255(18) 0.039(2) 0.119(4) 0.009(2) -0.033(2) -0.0070(16) F8 0.052(2) 0.0344(19) 0.061(2) -0.0121(17) -0.0189(19) 0.0119(17) F9 0.044(2) 0.046(2) 0.043(2) 0.0071(16) -0.0211(17) 0.0043(17) Os1 0.01973(10) 0.02172(10) 0.01860(10) -0.00226(7) -0.00402(7) -0.00355(7) Os2 0.02019(10) 0.01928(9) 0.01441(9) -0.00026(6) -0.00487(7) -0.00430(7) Os3 0.02067(10) 0.01830(9) 0.01451(9) -0.00072(6) -0.00496(7) -0.00422(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.138(6) . ? C1 Os1 1.954(5) . ? C2 O2 1.142(6) . ? C2 Os1 1.917(5) . ? C3 O3 1.137(7) . ? C3 Os1 1.924(6) . ? C4 O4 1.145(6) . ? C4 Os1 1.949(5) . ? C5 O5 1.133(6) . ? C5 Os3 1.905(5) . ? C6 O6 1.124(6) . ? C6 Os3 1.945(5) . ? C7 O7 1.145(6) . ? C7 Os3 1.897(5) . ? C10 O10 1.146(6) . ? C10 Os2 1.889(5) . ? C12 O12 1.148(6) . ? C12 Os2 1.878(5) . ? C20 C25 1.391(7) . ? C20 C21 1.401(7) . ? C20 P1 1.825(5) . ? C21 C22 1.383(7) . ? C21 H21 0.9500 . ? C22 C23 1.386(7) . ? C22 H22 0.9500 . ? C23 C24 1.381(8) . ? C23 C27 1.505(7) . ? C24 C25 1.404(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C28 1.386(7) . ? C26 C32 1.397(6) . ? C26 P1 1.835(5) . ? C27 F3 1.326(6) . ? C27 F2 1.329(7) . ? C27 F1 1.337(6) . ? C28 C29 1.400(7) . ? C28 H28 0.9500 . ? C29 C30 1.388(7) . ? C29 H29 0.9500 . ? C30 C31 1.391(7) . ? C30 C34 1.492(8) . ? C31 C32 1.385(7) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C35 1.393(7) . ? C33 C39 1.395(7) . ? C33 P1 1.828(5) . ? C34 F6 1.294(7) . ? C34 F4 1.335(7) . ? C34 F5 1.351(8) . ? C35 C36 1.406(7) . ? C35 H35 0.9500 . ? C36 C37 1.372(7) . ? C36 H36 0.9500 . ? C37 C38 1.405(7) . ? C37 C40 1.488(7) . ? C38 C39 1.376(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 F8 1.331(6) . ? C40 F7 1.332(6) . ? C40 F9 1.343(7) . ? P1 Os2 2.3544(12) . ? Os1 Os3 2.8157(3) . ? Os1 Os2 2.8161(3) . ? Os2 Os3 2.6942(3) . ? Os2 H01 1.8503 . ? Os2 H02 1.8504 . ? Os3 H01 1.8502 . ? Os3 H02 1.8504 . ? 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 O1 C1 Os1 178.7(5) . . ? O2 C2 Os1 177.4(5) . . ? O3 C3 Os1 178.0(5) . . ? O4 C4 Os1 178.6(4) . . ? O5 C5 Os3 178.5(4) . . ? O6 C6 Os3 176.9(4) . . ? O7 C7 Os3 177.2(5) . . ? O10 C10 Os2 178.1(5) . . ? O12 C12 Os2 177.1(4) . . ? C25 C20 C21 118.8(4) . . ? C25 C20 P1 123.6(4) . . ? C21 C20 P1 117.6(3) . . ? C22 C21 C20 120.9(4) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 120.1(5) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 119.9(5) . . ? C24 C23 C27 122.3(5) . . ? C22 C23 C27 117.8(5) . . ? C23 C24 C25 120.4(5) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C20 C25 C24 120.0(5) . . ? C20 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C28 C26 C32 119.2(4) . . ? C28 C26 P1 122.1(3) . . ? C32 C26 P1 118.7(4) . . ? F3 C27 F2 107.1(4) . . ? F3 C27 F1 107.0(5) . . ? F2 C27 F1 105.2(5) . . ? F3 C27 C23 112.9(5) . . ? F2 C27 C23 112.2(4) . . ? F1 C27 C23 112.0(4) . . ? C26 C28 C29 120.1(4) . . ? C26 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.3(5) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 119.7(5) . . ? C29 C30 C34 121.5(5) . . ? C31 C30 C34 118.7(5) . . ? C32 C31 C30 119.8(5) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C26 120.9(5) . . ? C31 C32 H32 119.5 . . ? C26 C32 H32 119.5 . . ? C35 C33 C39 119.4(5) . . ? C35 C33 P1 122.2(4) . . ? C39 C33 P1 118.4(4) . . ? F6 C34 F4 108.1(6) . . ? F6 C34 F5 106.6(6) . . ? F4 C34 F5 103.8(5) . . ? F6 C34 C30 113.3(5) . . ? F4 C34 C30 113.2(5) . . ? F5 C34 C30 111.2(5) . . ? C33 C35 C36 119.1(5) . . ? C33 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C37 C36 C35 120.9(5) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C38 120.0(5) . . ? C36 C37 C40 121.7(5) . . ? C38 C37 C40 118.3(5) . . ? C39 C38 C37 119.2(5) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C33 121.4(5) . . ? C38 C39 H39 119.3 . . ? C33 C39 H39 119.3 . . ? F8 C40 F7 106.6(5) . . ? F8 C40 F9 105.8(5) . . ? F7 C40 F9 106.8(5) . . ? F8 C40 C37 112.2(5) . . ? F7 C40 C37 112.3(5) . . ? F9 C40 C37 112.7(4) . . ? C20 P1 C33 103.9(2) . . ? C20 P1 C26 103.6(2) . . ? C33 P1 C26 103.0(2) . . ? C20 P1 Os2 112.66(16) . . ? C33 P1 Os2 116.64(16) . . ? C26 P1 Os2 115.51(15) . . ? C2 Os1 C3 102.3(2) . . ? C2 Os1 C4 92.0(2) . . ? C3 Os1 C4 95.1(2) . . ? C2 Os1 C1 94.5(2) . . ? C3 Os1 C1 93.2(2) . . ? C4 Os1 C1 168.1(2) . . ? C2 Os1 Os3 102.64(16) . . ? C3 Os1 Os3 154.82(17) . . ? C4 Os1 Os3 87.31(14) . . ? C1 Os1 Os3 81.58(15) . . ? C2 Os1 Os2 159.45(16) . . ? C3 Os1 Os2 98.10(18) . . ? C4 Os1 Os2 83.86(14) . . ? C1 Os1 Os2 86.55(15) . . ? Os3 Os1 Os2 57.162(7) . . ? C12 Os2 C10 87.7(2) . . ? C12 Os2 P1 95.92(15) . . ? C10 Os2 P1 95.80(15) . . ? C12 Os2 Os3 129.39(14) . . ? C10 Os2 Os3 132.46(16) . . ? P1 Os2 Os3 106.59(3) . . ? C12 Os2 Os1 92.57(15) . . ? C10 Os2 Os1 92.99(15) . . ? P1 Os2 Os1 168.00(3) . . ? Os3 Os2 Os1 61.412(7) . . ? C12 Os2 H01 172.5 . . ? C10 Os2 H01 97.7 . . ? P1 Os2 H01 88.8 . . ? Os3 Os2 H01 43.3 . . ? Os1 Os2 H01 82.0 . . ? C12 Os2 H02 93.7 . . ? C10 Os2 H02 174.1 . . ? P1 Os2 H02 89.7 . . ? Os3 Os2 H02 43.3 . . ? Os1 Os2 H02 81.2 . . ? H01 Os2 H02 80.4 . . ? C7 Os3 C5 88.4(2) . . ? C7 Os3 C6 98.2(2) . . ? C5 Os3 C6 94.1(2) . . ? C7 Os3 Os2 128.44(15) . . ? C5 Os3 Os2 130.64(14) . . ? C6 Os3 Os2 108.83(14) . . ? C7 Os3 Os1 86.80(15) . . ? C5 Os3 Os1 94.94(15) . . ? C6 Os3 Os1 169.78(15) . . ? Os2 Os3 Os1 61.426(7) . . ? C7 Os3 H01 168.6 . . ? C5 Os3 H01 94.4 . . ? C6 Os3 H01 92.6 . . ? Os2 Os3 H01 43.3 . . ? Os1 Os3 H01 82.0 . . ? C7 Os3 H02 96.1 . . ? C5 Os3 H02 173.9 . . ? C6 Os3 H02 89.3 . . ? Os2 Os3 H02 43.3 . . ? Os1 Os3 H02 81.2 . . ? H01 Os3 H02 80.4 . . ? 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 C25 C20 C21 C22 -0.9(8) . . . . ? P1 C20 C21 C22 -178.3(4) . . . . ? C20 C21 C22 C23 1.4(8) . . . . ? C21 C22 C23 C24 -1.1(8) . . . . ? C21 C22 C23 C27 179.3(5) . . . . ? C22 C23 C24 C25 0.2(9) . . . . ? C27 C23 C24 C25 179.8(5) . . . . ? C21 C20 C25 C24 0.0(8) . . . . ? P1 C20 C25 C24 177.3(5) . . . . ? C23 C24 C25 C20 0.3(9) . . . . ? C24 C23 C27 F3 9.0(8) . . . . ? C22 C23 C27 F3 -171.4(5) . . . . ? C24 C23 C27 F2 -112.1(6) . . . . ? C22 C23 C27 F2 67.5(6) . . . . ? C24 C23 C27 F1 129.8(6) . . . . ? C22 C23 C27 F1 -50.5(7) . . . . ? C32 C26 C28 C29 -1.3(7) . . . . ? P1 C26 C28 C29 -178.0(4) . . . . ? C26 C28 C29 C30 1.2(8) . . . . ? C28 C29 C30 C31 0.3(8) . . . . ? C28 C29 C30 C34 179.6(5) . . . . ? C29 C30 C31 C32 -1.7(8) . . . . ? C34 C30 C31 C32 179.0(5) . . . . ? C30 C31 C32 C26 1.6(8) . . . . ? C28 C26 C32 C31 0.0(7) . . . . ? P1 C26 C32 C31 176.7(4) . . . . ? C29 C30 C34 F6 121.2(7) . . . . ? C31 C30 C34 F6 -59.5(9) . . . . ? C29 C30 C34 F4 -2.4(8) . . . . ? C31 C30 C34 F4 176.9(5) . . . . ? C29 C30 C34 F5 -118.7(6) . . . . ? C31 C30 C34 F5 60.6(7) . . . . ? C39 C33 C35 C36 -0.9(7) . . . . ? P1 C33 C35 C36 178.0(4) . . . . ? C33 C35 C36 C37 1.6(7) . . . . ? C35 C36 C37 C38 -0.6(8) . . . . ? C35 C36 C37 C40 -179.2(5) . . . . ? C36 C37 C38 C39 -1.2(7) . . . . ? C40 C37 C38 C39 177.5(5) . . . . ? C37 C38 C39 C33 1.9(8) . . . . ? C35 C33 C39 C38 -0.9(7) . . . . ? P1 C33 C39 C38 -179.8(4) . . . . ? C36 C37 C40 F8 -112.8(6) . . . . ? C38 C37 C40 F8 68.5(7) . . . . ? C36 C37 C40 F7 7.3(8) . . . . ? C38 C37 C40 F7 -171.4(5) . . . . ? C36 C37 C40 F9 127.9(5) . . . . ? C38 C37 C40 F9 -50.7(6) . . . . ? C25 C20 P1 C33 6.6(5) . . . . ? C21 C20 P1 C33 -176.1(4) . . . . ? C25 C20 P1 C26 114.0(5) . . . . ? C21 C20 P1 C26 -68.8(4) . . . . ? C25 C20 P1 Os2 -120.5(4) . . . . ? C21 C20 P1 Os2 56.8(4) . . . . ? C35 C33 P1 C20 103.6(4) . . . . ? C39 C33 P1 C20 -77.5(4) . . . . ? C35 C33 P1 C26 -4.2(4) . . . . ? C39 C33 P1 C26 174.7(4) . . . . ? C35 C33 P1 Os2 -131.8(4) . . . . ? C39 C33 P1 Os2 47.1(4) . . . . ? C28 C26 P1 C20 -8.8(5) . . . . ? C32 C26 P1 C20 174.5(4) . . . . ? C28 C26 P1 C33 99.2(4) . . . . ? C32 C26 P1 C33 -77.5(4) . . . . ? C28 C26 P1 Os2 -132.5(4) . . . . ? C32 C26 P1 Os2 50.8(4) . . . . ? O2 C2 Os1 C3 -115(12) . . . . ? O2 C2 Os1 C4 -19(12) . . . . ? O2 C2 Os1 C1 151(12) . . . . ? O2 C2 Os1 Os3 68(12) . . . . ? O2 C2 Os1 Os2 58(12) . . . . ? O3 C3 Os1 C2 -121(18) . . . . ? O3 C3 Os1 C4 146(18) . . . . ? O3 C3 Os1 C1 -26(18) . . . . ? O3 C3 Os1 Os3 51(18) . . . . ? O3 C3 Os1 Os2 61(18) . . . . ? O4 C4 Os1 C2 12(18) . . . . ? O4 C4 Os1 C3 114(18) . . . . ? O4 C4 Os1 C1 -112(18) . . . . ? O4 C4 Os1 Os3 -91(18) . . . . ? O4 C4 Os1 Os2 -148(18) . . . . ? O1 C1 Os1 C2 -14(20) . . . . ? O1 C1 Os1 C3 -117(20) . . . . ? O1 C1 Os1 C4 109(20) . . . . ? O1 C1 Os1 Os3 88(20) . . . . ? O1 C1 Os1 Os2 145(20) . . . . ? O12 C12 Os2 C10 130(10) . . . . ? O12 C12 Os2 P1 -134(10) . . . . ? O12 C12 Os2 Os3 -17(10) . . . . ? O12 C12 Os2 Os1 37(10) . . . . ? O10 C10 Os2 C12 -75(15) . . . . ? O10 C10 Os2 P1 -171(15) . . . . ? O10 C10 Os2 Os3 70(15) . . . . ? O10 C10 Os2 Os1 17(15) . . . . ? C20 P1 Os2 C12 -73.8(2) . . . . ? C33 P1 Os2 C12 166.1(2) . . . . ? C26 P1 Os2 C12 45.0(2) . . . . ? C20 P1 Os2 C10 14.4(2) . . . . ? C33 P1 Os2 C10 -105.6(2) . . . . ? C26 P1 Os2 C10 133.2(2) . . . . ? C20 P1 Os2 Os3 152.04(18) . . . . ? C33 P1 Os2 Os3 31.99(17) . . . . ? C26 P1 Os2 Os3 -89.16(17) . . . . ? C20 P1 Os2 Os1 151.4(2) . . . . ? C33 P1 Os2 Os1 31.3(2) . . . . ? C26 P1 Os2 Os1 -89.8(2) . . . . ? C2 Os1 Os2 C12 -122.9(5) . . . . ? C3 Os1 Os2 C12 50.7(2) . . . . ? C4 Os1 Os2 C12 -43.6(2) . . . . ? C1 Os1 Os2 C12 143.5(2) . . . . ? Os3 Os1 Os2 C12 -134.35(15) . . . . ? C2 Os1 Os2 C10 149.3(5) . . . . ? C3 Os1 Os2 C10 -37.1(2) . . . . ? C4 Os1 Os2 C10 -131.4(2) . . . . ? C1 Os1 Os2 C10 55.7(2) . . . . ? Os3 Os1 Os2 C10 137.85(16) . . . . ? C2 Os1 Os2 P1 12.1(5) . . . . ? C3 Os1 Os2 P1 -174.2(2) . . . . ? C4 Os1 Os2 P1 91.5(2) . . . . ? C1 Os1 Os2 P1 -81.5(2) . . . . ? Os3 Os1 Os2 P1 0.71(14) . . . . ? C2 Os1 Os2 Os3 11.4(4) . . . . ? C3 Os1 Os2 Os3 -174.94(17) . . . . ? C4 Os1 Os2 Os3 90.76(15) . . . . ? C1 Os1 Os2 Os3 -82.20(15) . . . . ? O7 C7 Os3 C5 -97(9) . . . . ? O7 C7 Os3 C6 169(9) . . . . ? O7 C7 Os3 Os2 47(9) . . . . ? O7 C7 Os3 Os1 -2(9) . . . . ? O5 C5 Os3 C7 126(17) . . . . ? O5 C5 Os3 C6 -136(17) . . . . ? O5 C5 Os3 Os2 -17(17) . . . . ? O5 C5 Os3 Os1 39(17) . . . . ? O6 C6 Os3 C7 21(10) . . . . ? O6 C6 Os3 C5 -68(10) . . . . ? O6 C6 Os3 Os2 156(10) . . . . ? O6 C6 Os3 Os1 140(9) . . . . ? C12 Os2 Os3 C7 8.5(3) . . . . ? C10 Os2 Os3 C7 -124.4(3) . . . . ? P1 Os2 Os3 C7 121.05(19) . . . . ? Os1 Os2 Os3 C7 -59.10(19) . . . . ? C12 Os2 Os3 C5 137.8(3) . . . . ? C10 Os2 Os3 C5 4.9(3) . . . . ? P1 Os2 Os3 C5 -109.62(19) . . . . ? Os1 Os2 Os3 C5 70.23(19) . . . . ? C12 Os2 Os3 C6 -109.1(3) . . . . ? C10 Os2 Os3 C6 118.1(3) . . . . ? P1 Os2 Os3 C6 3.52(16) . . . . ? Os1 Os2 Os3 C6 -176.63(16) . . . . ? C12 Os2 Os3 Os1 67.6(2) . . . . ? C10 Os2 Os3 Os1 -65.3(2) . . . . ? P1 Os2 Os3 Os1 -179.85(3) . . . . ? C2 Os1 Os3 C7 -38.2(2) . . . . ? C3 Os1 Os3 C7 149.5(4) . . . . ? C4 Os1 Os3 C7 53.3(2) . . . . ? C1 Os1 Os3 C7 -131.0(2) . . . . ? Os2 Os1 Os3 C7 137.69(15) . . . . ? C2 Os1 Os3 C5 49.9(2) . . . . ? C3 Os1 Os3 C5 -122.4(4) . . . . ? C4 Os1 Os3 C5 141.36(19) . . . . ? C1 Os1 Os3 C5 -42.9(2) . . . . ? Os2 Os1 Os3 C5 -134.22(13) . . . . ? C2 Os1 Os3 C6 -157.6(8) . . . . ? C3 Os1 Os3 C6 30.1(9) . . . . ? C4 Os1 Os3 C6 -66.2(8) . . . . ? C1 Os1 Os3 C6 109.6(8) . . . . ? Os2 Os1 Os3 C6 18.3(8) . . . . ? C2 Os1 Os3 Os2 -175.91(16) . . . . ? C3 Os1 Os3 Os2 11.8(4) . . . . ? C4 Os1 Os3 Os2 -84.42(14) . . . . ? C1 Os1 Os3 Os2 91.33(15) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.511 _refine_diff_density_min -1.926 _refine_diff_density_rms 0.180 #===END======================================================================== data_V _database_code_depnum_ccdc_archive 'CCDC 228036' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HOs3(CO)8(C6H5O)PPh3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H21 O9 Os3 P' _chemical_formula_weight 1151.06 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4672(2) _cell_length_b 12.4349(2) _cell_length_c 13.9381(3) _cell_angle_alpha 74.3733(7) _cell_angle_beta 83.8221(7) _cell_angle_gamma 84.5688(8) _cell_volume 1567.32(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 12.235 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.14453 _exptl_absorpt_correction_T_max 0.67685 _exptl_absorpt_process_details 'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12617 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 25.07 _reflns_number_total 5510 _reflns_number_gt 5123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material SHELXL-97 _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. The idealized position of the hydride hydrogen H(1) was estimated with XHYDEX program. Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0810P)^2^+23.0155P] 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 0.0018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5510 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1379 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4388(13) 0.8032(11) 0.9453(10) 0.035(3) Uani 1 1 d . . . C2 C 0.4930(13) 0.6498(10) 0.8371(10) 0.034(3) Uani 1 1 d . . . C3 C 0.4536(12) 0.8849(10) 0.7432(9) 0.026(2) Uani 1 1 d . . . C4 C 0.9785(13) 0.9351(9) 0.6414(8) 0.026(2) Uani 1 1 d . . . C6 C 0.7144(12) 0.9337(10) 0.6023(8) 0.027(2) Uani 1 1 d . . . C7 C 0.9588(15) 0.9692(12) 0.8875(9) 0.037(3) Uani 1 1 d . . . C8 C 0.7016(14) 1.0281(10) 0.7925(9) 0.033(3) Uani 1 1 d . . . C9 C 0.6921(14) 0.9236(11) 1.0013(11) 0.040(3) Uani 1 1 d . . . C14 C 0.9426(12) 0.7666(10) 0.8254(10) 0.030(3) Uani 1 1 d . . . C13 C 0.8711(13) 0.7148(9) 0.9186(8) 0.027(2) Uani 1 1 d . . . C12 C 0.7200(12) 0.7105(9) 0.9400(7) 0.024(2) Uani 1 1 d . . . C11 C 0.7109(15) 0.6557(11) 1.0512(9) 0.036(3) Uani 1 1 d . . . H11 H 0.6257 0.6465 1.0944 0.044 Uiso 1 1 calc R . . C10 C 0.8384(17) 0.6232(13) 1.0778(9) 0.047(4) Uani 1 1 d . . . H10 H 0.8571 0.5810 1.1435 0.056 Uiso 1 1 calc R . . C15 C 1.1032(13) 0.7590(12) 0.8268(10) 0.039(3) Uani 1 1 d . . . H15A H 1.1438 0.8161 0.7701 0.058 Uiso 1 1 calc R . . H15B H 1.1420 0.6846 0.8218 0.058 Uiso 1 1 calc R . . H15C H 1.1276 0.7713 0.8894 0.058 Uiso 1 1 calc R . . C20 C 0.8563(11) 0.7328(9) 0.4850(8) 0.022(2) Uani 1 1 d . . . C21 C 0.7164(12) 0.7673(10) 0.4669(9) 0.027(2) Uani 1 1 d . . . H20 H 0.6492 0.7764 0.5203 0.033 Uiso 1 1 calc R . . C22 C 0.6737(13) 0.7888(10) 0.3711(9) 0.033(3) Uani 1 1 d . . . H21 H 0.5770 0.8107 0.3591 0.040 Uiso 1 1 calc R . . C23 C 0.7731(16) 0.7782(11) 0.2926(9) 0.041(3) Uani 1 1 d . . . H22 H 0.7445 0.7928 0.2268 0.049 Uiso 1 1 calc R . . C24 C 0.9128(16) 0.7464(11) 0.3105(9) 0.038(3) Uani 1 1 d . . . H23 H 0.9802 0.7392 0.2566 0.045 Uiso 1 1 calc R . . C25 C 0.9568(12) 0.7249(9) 0.4045(8) 0.025(2) Uani 1 1 d . . . H25 H 1.0542 0.7048 0.4155 0.031 Uiso 1 1 calc R . . C26 C 1.0950(11) 0.6646(10) 0.6049(7) 0.022(2) Uani 1 1 d . . . C27 C 1.1869(11) 0.7514(9) 0.5613(9) 0.027(2) Uani 1 1 d . . . H27 H 1.1485 0.8258 0.5356 0.032 Uiso 1 1 calc R . . C28 C 1.3330(12) 0.7277(10) 0.5560(10) 0.032(3) Uani 1 1 d . . . H28 H 1.3943 0.7869 0.5298 0.038 Uiso 1 1 calc R . . C29 C 1.3903(12) 0.6203(11) 0.5881(11) 0.037(3) Uani 1 1 d . . . H29 H 1.4904 0.6046 0.5801 0.045 Uiso 1 1 calc R . . C30 C 1.3010(13) 0.5334(10) 0.6328(10) 0.034(3) Uani 1 1 d . . . H30 H 1.3399 0.4593 0.6592 0.040 Uiso 1 1 calc R . . C31 C 1.1527(12) 0.5581(9) 0.6377(8) 0.025(2) Uani 1 1 d . . . H31 H 1.0914 0.4990 0.6646 0.030 Uiso 1 1 calc R . . C32 C 0.8293(10) 0.5686(9) 0.6729(8) 0.020(2) Uani 1 1 d . . . C33 C 0.8328(13) 0.5236(9) 0.7776(9) 0.029(2) Uani 1 1 d . . . H33 H 0.8737 0.5629 0.8162 0.034 Uiso 1 1 calc R . . C34 C 0.7753(14) 0.4208(11) 0.8234(9) 0.035(3) Uani 1 1 d . . . H34 H 0.7782 0.3905 0.8934 0.042 Uiso 1 1 calc R . . C35 C 0.7147(14) 0.3627(10) 0.7691(11) 0.039(3) Uani 1 1 d . . . H35 H 0.6772 0.2926 0.8016 0.046 Uiso 1 1 calc R . . C36 C 0.7085(12) 0.4063(9) 0.6673(9) 0.029(2) Uani 1 1 d . . . H36 H 0.6642 0.3674 0.6299 0.035 Uiso 1 1 calc R . . C37 C 0.7676(12) 0.5074(9) 0.6197(9) 0.026(2) Uani 1 1 d . . . H37 H 0.7658 0.5355 0.5493 0.031 Uiso 1 1 calc R . . O1 O 0.3575(10) 0.8149(9) 1.0136(7) 0.045(2) Uani 1 1 d . . . O2 O 0.4445(12) 0.5684(9) 0.8355(9) 0.056(3) Uani 1 1 d . . . O3 O 0.3826(10) 0.9416(9) 0.6915(8) 0.049(3) Uani 1 1 d . . . O4 O 1.0629(9) 0.9977(8) 0.6087(7) 0.039(2) Uani 1 1 d . . . O6 O 0.6449(9) 0.9949(7) 0.5460(6) 0.035(2) Uani 1 1 d . . . O7 O 1.0530(13) 1.0120(11) 0.8893(8) 0.063(3) Uani 1 1 d . . . O8 O 0.6462(12) 1.1065(8) 0.7427(8) 0.047(2) Uani 1 1 d . . . O9 O 0.6301(11) 0.9343(8) 1.0748(7) 0.045(2) Uani 1 1 d . . . O10 O 0.9451(10) 0.6557(8) 1.0016(7) 0.040(2) Uani 1 1 d . . . P1 P 0.9039(3) 0.7028(2) 0.61396(19) 0.0171(5) Uani 1 1 d . . . Os1 Os 0.57133(4) 0.78119(3) 0.84224(3) 0.02099(17) Uani 1 1 d . . . Os2 Os 0.83162(4) 0.83840(3) 0.69990(3) 0.01681(16) Uani 1 1 d . . . Os3 Os 0.78803(5) 0.90003(3) 0.88011(3) 0.02298(17) Uani 1 1 d . . . H1 H 0.6825 0.7461 0.7358 0.050 Uiso 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 C1 0.035(6) 0.032(7) 0.041(7) -0.012(6) -0.010(6) -0.004(5) C2 0.032(6) 0.028(6) 0.037(7) -0.003(5) 0.001(5) -0.003(5) C3 0.025(5) 0.028(6) 0.024(6) -0.007(5) 0.004(5) -0.008(5) C4 0.039(6) 0.025(6) 0.013(5) -0.004(4) -0.003(4) 0.003(5) C6 0.033(6) 0.036(6) 0.013(5) -0.012(5) 0.010(5) -0.014(5) C7 0.052(8) 0.045(7) 0.022(6) -0.016(5) -0.003(5) -0.020(6) C8 0.045(7) 0.030(6) 0.021(6) 0.002(5) -0.007(5) -0.007(5) C9 0.036(7) 0.033(7) 0.049(9) -0.007(6) -0.011(6) 0.002(5) C14 0.023(6) 0.029(6) 0.038(7) -0.004(5) -0.006(5) -0.004(5) C13 0.040(6) 0.021(5) 0.017(5) 0.003(4) -0.013(5) -0.003(5) C12 0.032(6) 0.021(5) 0.008(5) 0.008(4) 0.010(4) -0.003(4) C11 0.055(8) 0.034(7) 0.016(6) 0.000(5) -0.001(5) -0.005(6) C10 0.073(10) 0.052(8) 0.010(6) 0.008(5) -0.009(6) -0.013(7) C15 0.028(6) 0.047(8) 0.035(7) 0.003(6) -0.011(5) -0.003(5) C20 0.025(5) 0.020(5) 0.020(5) -0.005(4) -0.004(4) 0.001(4) C21 0.031(6) 0.029(6) 0.023(6) -0.011(5) 0.000(5) 0.005(5) C22 0.037(6) 0.032(6) 0.029(6) -0.004(5) -0.021(5) 0.009(5) C23 0.068(9) 0.040(7) 0.013(6) -0.002(5) -0.012(6) 0.000(6) C24 0.062(9) 0.032(6) 0.013(5) -0.002(5) 0.002(5) 0.008(6) C25 0.026(5) 0.031(6) 0.019(5) -0.009(4) 0.002(4) 0.005(5) C26 0.022(5) 0.034(6) 0.012(5) -0.007(4) -0.001(4) 0.000(4) C27 0.021(5) 0.021(5) 0.037(7) -0.003(5) 0.001(5) -0.006(4) C28 0.018(5) 0.034(6) 0.039(7) -0.004(5) -0.001(5) -0.006(5) C29 0.017(5) 0.041(7) 0.052(8) -0.009(6) -0.004(5) -0.004(5) C30 0.030(6) 0.027(6) 0.040(7) -0.002(5) -0.013(5) 0.007(5) C31 0.024(5) 0.024(6) 0.026(6) -0.003(4) -0.008(4) -0.004(4) C32 0.013(4) 0.020(5) 0.024(5) 0.000(4) 0.005(4) -0.005(4) C33 0.036(6) 0.020(5) 0.029(6) -0.004(5) 0.000(5) -0.006(5) C34 0.051(7) 0.032(6) 0.022(6) -0.006(5) -0.004(5) -0.002(6) C35 0.039(7) 0.022(6) 0.049(8) -0.004(6) 0.017(6) -0.010(5) C36 0.033(6) 0.019(5) 0.038(7) -0.014(5) 0.002(5) -0.002(4) C37 0.028(6) 0.023(6) 0.024(6) -0.006(4) 0.005(4) -0.003(4) O1 0.043(5) 0.059(6) 0.028(5) -0.009(4) 0.012(4) -0.001(4) O2 0.060(7) 0.039(6) 0.074(8) -0.015(5) -0.003(6) -0.025(5) O3 0.035(5) 0.059(6) 0.043(6) 0.005(5) -0.010(4) 0.005(5) O4 0.033(4) 0.039(5) 0.042(5) -0.006(4) 0.011(4) -0.022(4) O6 0.040(5) 0.027(4) 0.027(4) 0.009(4) -0.012(4) 0.009(4) O7 0.070(7) 0.089(9) 0.040(6) -0.013(6) -0.009(5) -0.058(7) O8 0.070(7) 0.028(5) 0.041(5) -0.003(4) -0.022(5) 0.002(5) O9 0.061(6) 0.050(6) 0.022(5) -0.011(4) 0.001(4) 0.003(5) O10 0.045(5) 0.040(5) 0.031(5) 0.003(4) -0.014(4) -0.005(4) P1 0.0155(11) 0.0186(12) 0.0147(12) -0.0005(10) -0.0003(9) -0.0014(9) Os1 0.0221(2) 0.0208(3) 0.0185(3) -0.00191(17) 0.00117(16) -0.00642(17) Os2 0.0165(2) 0.0191(2) 0.0138(2) -0.00192(16) -0.00072(15) -0.00380(15) Os3 0.0302(3) 0.0226(3) 0.0173(3) -0.00399(17) -0.00524(17) -0.00770(18) _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 C1 O1 1.189(16) . ? C1 Os1 1.863(13) . ? C2 O2 1.157(16) . ? C2 Os1 1.878(13) . ? C3 O3 1.099(15) . ? C3 Os1 1.978(12) . ? C4 O4 1.139(14) . ? C4 Os2 1.895(12) . ? C6 O6 1.150(15) . ? C6 Os2 1.922(13) . ? C7 O7 1.088(17) . ? C7 Os3 1.926(13) . ? C8 O8 1.151(15) . ? C8 Os3 1.902(12) . ? C9 O9 1.158(17) . ? C9 Os3 1.911(15) . ? C14 C13 1.416(17) . ? C14 C15 1.516(16) . ? C14 Os2 2.083(12) . ? C14 Os3 2.336(12) . ? C13 O10 1.409(13) . ? C13 C12 1.433(16) . ? C13 Os3 2.301(11) . ? C12 C11 1.512(15) . ? C12 Os1 2.036(11) . ? C12 Os3 2.404(11) . ? C11 C10 1.30(2) . ? C11 H11 0.9500 . ? C10 O10 1.388(17) . ? C10 H10 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C20 C21 1.381(16) . ? C20 C25 1.409(15) . ? C20 P1 1.832(11) . ? C21 C22 1.386(16) . ? C21 H20 0.9500 . ? C22 C23 1.390(19) . ? C22 H21 0.9500 . ? C23 C24 1.37(2) . ? C23 H22 0.9500 . ? C24 C25 1.367(17) . ? C24 H23 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.361(16) . ? C26 C27 1.415(15) . ? C26 P1 1.826(10) . ? C27 C28 1.385(16) . ? C27 H27 0.9500 . ? C28 C29 1.368(18) . ? C28 H28 0.9500 . ? C29 C30 1.402(18) . ? C29 H29 0.9500 . ? C30 C31 1.407(16) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.397(16) . ? C32 C33 1.418(16) . ? C32 P1 1.822(10) . ? C33 C34 1.397(17) . ? C33 H33 0.9500 . ? C34 C35 1.375(19) . ? C34 H34 0.9500 . ? C35 C36 1.382(19) . ? C35 H35 0.9500 . ? C36 C37 1.391(16) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? P1 Os2 2.332(3) . ? Os1 Os3 2.8104(6) . ? Os1 Os2 3.0057(5) . ? Os1 H1 1.8501 . ? Os2 Os3 2.7966(6) . ? Os2 H1 1.8457 . ? 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 O1 C1 Os1 177.6(11) . . ? O2 C2 Os1 179.0(12) . . ? O3 C3 Os1 176.6(10) . . ? O4 C4 Os2 176.1(10) . . ? O6 C6 Os2 176.6(10) . . ? O7 C7 Os3 177.2(14) . . ? O8 C8 Os3 177.3(12) . . ? O9 C9 Os3 177.0(13) . . ? C13 C14 C15 113.5(11) . . ? C13 C14 Os2 121.4(8) . . ? C15 C14 Os2 125.1(9) . . ? C13 C14 Os3 70.9(7) . . ? C15 C14 Os3 124.5(9) . . ? Os2 C14 Os3 78.3(4) . . ? O10 C13 C14 122.2(11) . . ? O10 C13 C12 111.9(9) . . ? C14 C13 C12 125.9(10) . . ? O10 C13 Os3 127.5(8) . . ? C14 C13 Os3 73.6(6) . . ? C12 C13 Os3 76.2(6) . . ? C13 C12 C11 100.5(10) . . ? C13 C12 Os1 125.7(7) . . ? C11 C12 Os1 133.3(8) . . ? C13 C12 Os3 68.4(6) . . ? C11 C12 Os3 119.1(8) . . ? Os1 C12 Os3 78.1(3) . . ? C10 C11 C12 108.8(11) . . ? C10 C11 H11 125.6 . . ? C12 C11 H11 125.6 . . ? C11 C10 O10 113.9(11) . . ? C11 C10 H10 123.1 . . ? O10 C10 H10 123.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C20 C25 119.4(10) . . ? C21 C20 P1 117.8(8) . . ? C25 C20 P1 122.7(8) . . ? C20 C21 C22 120.3(10) . . ? C20 C21 H20 119.9 . . ? C22 C21 H20 119.9 . . ? C21 C22 C23 119.7(11) . . ? C21 C22 H21 120.1 . . ? C23 C22 H21 120.1 . . ? C24 C23 C22 119.8(11) . . ? C24 C23 H22 120.1 . . ? C22 C23 H22 120.1 . . ? C25 C24 C23 121.3(11) . . ? C25 C24 H23 119.4 . . ? C23 C24 H23 119.4 . . ? C24 C25 C20 119.4(11) . . ? C24 C25 H25 120.3 . . ? C20 C25 H25 120.3 . . ? C31 C26 C27 118.8(10) . . ? C31 C26 P1 123.6(9) . . ? C27 C26 P1 117.6(8) . . ? C28 C27 C26 119.9(10) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 120.9(11) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C30 119.9(11) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C29 C30 C31 118.8(11) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C26 C31 C30 121.6(11) . . ? C26 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C37 C32 C33 118.0(10) . . ? C37 C32 P1 123.0(8) . . ? C33 C32 P1 119.0(9) . . ? C34 C33 C32 119.3(11) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 121.4(12) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C34 C35 C36 119.9(11) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C37 119.7(12) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C36 C37 C32 121.6(11) . . ? C36 C37 H37 119.2 . . ? C32 C37 H37 119.2 . . ? C10 O10 C13 104.2(10) . . ? C32 P1 C26 102.5(5) . . ? C32 P1 C20 102.9(5) . . ? C26 P1 C20 104.0(5) . . ? C32 P1 Os2 113.1(3) . . ? C26 P1 Os2 115.6(4) . . ? C20 P1 Os2 116.9(3) . . ? C1 Os1 C2 93.1(5) . . ? C1 Os1 C3 90.0(5) . . ? C2 Os1 C3 96.2(5) . . ? C1 Os1 C12 91.7(5) . . ? C2 Os1 C12 98.5(5) . . ? C3 Os1 C12 165.1(5) . . ? C1 Os1 Os3 97.4(4) . . ? C2 Os1 Os3 153.2(4) . . ? C3 Os1 Os3 108.3(3) . . ? C12 Os1 Os3 56.8(3) . . ? C1 Os1 Os2 153.0(4) . . ? C2 Os1 Os2 113.8(4) . . ? C3 Os1 Os2 89.5(3) . . ? C12 Os1 Os2 82.3(3) . . ? Os3 Os1 Os2 57.361(14) . . ? C1 Os1 H1 171.2 . . ? C2 Os1 H1 78.8 . . ? C3 Os1 H1 87.6 . . ? C12 Os1 H1 92.8 . . ? Os3 Os1 H1 91.4 . . ? Os2 Os1 H1 35.5 . . ? C4 Os2 C6 86.6(5) . . ? C4 Os2 C14 91.5(5) . . ? C6 Os2 C14 165.2(5) . . ? C4 Os2 P1 96.5(3) . . ? C6 Os2 P1 97.6(3) . . ? C14 Os2 P1 97.2(3) . . ? C4 Os2 Os3 96.4(3) . . ? C6 Os2 Os3 110.7(3) . . ? C14 Os2 Os3 54.9(3) . . ? P1 Os2 Os3 149.46(6) . . ? C4 Os2 Os1 150.6(3) . . ? C6 Os2 Os1 89.9(3) . . ? C14 Os2 Os1 84.5(3) . . ? P1 Os2 Os1 112.86(6) . . ? Os3 Os2 Os1 57.808(14) . . ? C4 Os2 H1 170.7 . . ? C6 Os2 H1 86.5 . . ? C14 Os2 H1 96.7 . . ? P1 Os2 H1 78.2 . . ? Os3 Os2 H1 91.9 . . ? Os1 Os2 H1 35.6 . . ? C8 Os3 C9 96.5(5) . . ? C8 Os3 C7 95.7(6) . . ? C9 Os3 C7 96.1(6) . . ? C8 Os3 C13 151.1(5) . . ? C9 Os3 C13 105.5(5) . . ? C7 Os3 C13 100.1(5) . . ? C8 Os3 C14 123.7(5) . . ? C9 Os3 C14 139.5(5) . . ? C7 Os3 C14 85.1(5) . . ? C13 Os3 C14 35.5(4) . . ? C8 Os3 C12 131.3(5) . . ? C9 Os3 C12 86.4(5) . . ? C7 Os3 C12 132.5(5) . . ? C13 Os3 C12 35.4(4) . . ? C14 Os3 C12 64.7(4) . . ? C8 Os3 Os2 79.5(4) . . ? C9 Os3 Os2 159.1(4) . . ? C7 Os3 Os2 104.7(4) . . ? C13 Os3 Os2 73.3(3) . . ? C14 Os3 Os2 46.8(3) . . ? C12 Os3 Os2 81.2(3) . . ? C8 Os3 Os1 86.2(4) . . ? C9 Os3 Os1 94.6(4) . . ? C7 Os3 Os1 168.9(4) . . ? C13 Os3 Os1 73.9(3) . . ? C14 Os3 Os1 84.8(3) . . ? C12 Os3 Os1 45.1(3) . . ? Os2 Os3 Os1 64.831(15) . . ? 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 C15 C14 C13 O10 -4.2(17) . . . . ? Os2 C14 C13 O10 173.2(8) . . . . ? Os3 C14 C13 O10 -124.3(11) . . . . ? C15 C14 C13 C12 178.9(12) . . . . ? Os2 C14 C13 C12 -3.7(17) . . . . ? Os3 C14 C13 C12 58.7(11) . . . . ? C15 C14 C13 Os3 120.2(11) . . . . ? Os2 C14 C13 Os3 -62.4(7) . . . . ? O10 C13 C12 C11 8.0(13) . . . . ? C14 C13 C12 C11 -174.8(12) . . . . ? Os3 C13 C12 C11 -117.2(8) . . . . ? O10 C13 C12 Os1 -178.8(8) . . . . ? C14 C13 C12 Os1 -1.6(18) . . . . ? Os3 C13 C12 Os1 56.0(8) . . . . ? O10 C13 C12 Os3 125.2(9) . . . . ? C14 C13 C12 Os3 -57.6(11) . . . . ? C13 C12 C11 C10 -8.0(14) . . . . ? Os1 C12 C11 C10 179.6(11) . . . . ? Os3 C12 C11 C10 -79.0(13) . . . . ? C12 C11 C10 O10 5.4(17) . . . . ? C25 C20 C21 C22 3.1(17) . . . . ? P1 C20 C21 C22 -178.6(9) . . . . ? C20 C21 C22 C23 -1.6(19) . . . . ? C21 C22 C23 C24 0(2) . . . . ? C22 C23 C24 C25 0(2) . . . . ? C23 C24 C25 C20 2(2) . . . . ? C21 C20 C25 C24 -3.1(17) . . . . ? P1 C20 C25 C24 178.7(9) . . . . ? C31 C26 C27 C28 -2.4(17) . . . . ? P1 C26 C27 C28 177.5(10) . . . . ? C26 C27 C28 C29 3.2(19) . . . . ? C27 C28 C29 C30 -4(2) . . . . ? C28 C29 C30 C31 4(2) . . . . ? C27 C26 C31 C30 2.5(17) . . . . ? P1 C26 C31 C30 -177.4(9) . . . . ? C29 C30 C31 C26 -3.4(19) . . . . ? C37 C32 C33 C34 0.1(16) . . . . ? P1 C32 C33 C34 179.8(9) . . . . ? C32 C33 C34 C35 -0.4(18) . . . . ? C33 C34 C35 C36 -0.6(19) . . . . ? C34 C35 C36 C37 1.9(18) . . . . ? C35 C36 C37 C32 -2.2(17) . . . . ? C33 C32 C37 C36 1.2(16) . . . . ? P1 C32 C37 C36 -178.5(8) . . . . ? C11 C10 O10 C13 -0.3(16) . . . . ? C14 C13 O10 C10 177.3(12) . . . . ? C12 C13 O10 C10 -5.4(14) . . . . ? Os3 C13 O10 C10 83.8(12) . . . . ? C37 C32 P1 C26 -101.6(9) . . . . ? C33 C32 P1 C26 78.7(9) . . . . ? C37 C32 P1 C20 6.1(10) . . . . ? C33 C32 P1 C20 -173.5(8) . . . . ? C37 C32 P1 Os2 133.2(8) . . . . ? C33 C32 P1 Os2 -46.4(9) . . . . ? C31 C26 P1 C32 -0.2(11) . . . . ? C27 C26 P1 C32 179.9(9) . . . . ? C31 C26 P1 C20 -107.1(10) . . . . ? C27 C26 P1 C20 72.9(10) . . . . ? C31 C26 P1 Os2 123.3(9) . . . . ? C27 C26 P1 Os2 -56.6(9) . . . . ? C21 C20 P1 C32 74.9(9) . . . . ? C25 C20 P1 C32 -106.9(10) . . . . ? C21 C20 P1 C26 -178.5(9) . . . . ? C25 C20 P1 C26 -0.2(11) . . . . ? C21 C20 P1 Os2 -49.7(10) . . . . ? C25 C20 P1 Os2 128.5(9) . . . . ? O1 C1 Os1 C2 89(28) . . . . ? O1 C1 Os1 C3 -174(28) . . . . ? O1 C1 Os1 C12 -9(28) . . . . ? O1 C1 Os1 Os3 -66(28) . . . . ? O1 C1 Os1 Os2 -86(28) . . . . ? O2 C2 Os1 C1 -42(64) . . . . ? O2 C2 Os1 C3 -132(64) . . . . ? O2 C2 Os1 C12 51(64) . . . . ? O2 C2 Os1 Os3 72(64) . . . . ? O2 C2 Os1 Os2 136(63) . . . . ? O3 C3 Os1 C1 -22(19) . . . . ? O3 C3 Os1 C2 71(19) . . . . ? O3 C3 Os1 C12 -119(19) . . . . ? O3 C3 Os1 Os3 -120(19) . . . . ? O3 C3 Os1 Os2 -175(19) . . . . ? C13 C12 Os1 C1 -149.7(11) . . . . ? C11 C12 Os1 C1 21.1(12) . . . . ? Os3 C12 Os1 C1 -97.8(4) . . . . ? C13 C12 Os1 C2 116.9(10) . . . . ? C11 C12 Os1 C2 -72.2(12) . . . . ? Os3 C12 Os1 C2 168.9(4) . . . . ? C13 C12 Os1 C3 -53(2) . . . . ? C11 C12 Os1 C3 117.7(17) . . . . ? Os3 C12 Os1 C3 -1.2(17) . . . . ? C13 C12 Os1 Os3 -52.0(9) . . . . ? C11 C12 Os1 Os3 118.9(12) . . . . ? C13 C12 Os1 Os2 3.8(10) . . . . ? C11 C12 Os1 Os2 174.7(12) . . . . ? Os3 C12 Os1 Os2 55.81(16) . . . . ? O4 C4 Os2 C6 73(15) . . . . ? O4 C4 Os2 C14 -92(15) . . . . ? O4 C4 Os2 P1 170(15) . . . . ? O4 C4 Os2 Os3 -37(15) . . . . ? O4 C4 Os2 Os1 -11(16) . . . . ? O6 C6 Os2 C4 -64(16) . . . . ? O6 C6 Os2 C14 20(17) . . . . ? O6 C6 Os2 P1 -160(16) . . . . ? O6 C6 Os2 Os3 32(17) . . . . ? O6 C6 Os2 Os1 87(16) . . . . ? C13 C14 Os2 C4 155.5(10) . . . . ? C15 C14 Os2 C4 -27.4(11) . . . . ? Os3 C14 Os2 C4 96.7(4) . . . . ? C13 C14 Os2 C6 73(2) . . . . ? C15 C14 Os2 C6 -110.0(19) . . . . ? Os3 C14 Os2 C6 14.1(19) . . . . ? C13 C14 Os2 P1 -107.7(10) . . . . ? C15 C14 Os2 P1 69.4(11) . . . . ? Os3 C14 Os2 P1 -166.5(2) . . . . ? C13 C14 Os2 Os3 58.8(9) . . . . ? C15 C14 Os2 Os3 -124.1(12) . . . . ? C13 C14 Os2 Os1 4.7(9) . . . . ? C15 C14 Os2 Os1 -178.2(11) . . . . ? Os3 C14 Os2 Os1 -54.1(2) . . . . ? C32 P1 Os2 C4 161.4(5) . . . . ? C26 P1 Os2 C4 43.6(5) . . . . ? C20 P1 Os2 C4 -79.3(5) . . . . ? C32 P1 Os2 C6 -111.2(5) . . . . ? C26 P1 Os2 C6 131.0(5) . . . . ? C20 P1 Os2 C6 8.1(5) . . . . ? C32 P1 Os2 C14 69.0(5) . . . . ? C26 P1 Os2 C14 -48.8(5) . . . . ? C20 P1 Os2 C14 -171.7(5) . . . . ? C32 P1 Os2 Os3 46.9(4) . . . . ? C26 P1 Os2 Os3 -70.8(4) . . . . ? C20 P1 Os2 Os3 166.2(4) . . . . ? C32 P1 Os2 Os1 -18.0(4) . . . . ? C26 P1 Os2 Os1 -135.8(4) . . . . ? C20 P1 Os2 Os1 101.3(4) . . . . ? C1 Os1 Os2 C4 -8.5(11) . . . . ? C2 Os1 Os2 C4 177.1(8) . . . . ? C3 Os1 Os2 C4 80.6(7) . . . . ? C12 Os1 Os2 C4 -87.0(7) . . . . ? Os3 Os1 Os2 C4 -31.7(7) . . . . ? C1 Os1 Os2 C6 -91.5(9) . . . . ? C2 Os1 Os2 C6 94.1(5) . . . . ? C3 Os1 Os2 C6 -2.4(5) . . . . ? C12 Os1 Os2 C6 -170.0(5) . . . . ? Os3 Os1 Os2 C6 -114.7(3) . . . . ? C1 Os1 Os2 C14 74.8(9) . . . . ? C2 Os1 Os2 C14 -99.7(5) . . . . ? C3 Os1 Os2 C14 163.8(5) . . . . ? C12 Os1 Os2 C14 -3.8(5) . . . . ? Os3 Os1 Os2 C14 51.5(3) . . . . ? C1 Os1 Os2 P1 170.3(9) . . . . ? C2 Os1 Os2 P1 -4.1(4) . . . . ? C3 Os1 Os2 P1 -100.7(3) . . . . ? C12 Os1 Os2 P1 91.8(3) . . . . ? Os3 Os1 Os2 P1 147.04(7) . . . . ? C1 Os1 Os2 Os3 23.2(9) . . . . ? C2 Os1 Os2 Os3 -151.2(4) . . . . ? C3 Os1 Os2 Os3 112.3(3) . . . . ? C12 Os1 Os2 Os3 -55.3(3) . . . . ? O8 C8 Os3 C9 -1(25) . . . . ? O8 C8 Os3 C7 -98(25) . . . . ? O8 C8 Os3 C13 139(25) . . . . ? O8 C8 Os3 C14 174(25) . . . . ? O8 C8 Os3 C12 90(25) . . . . ? O8 C8 Os3 Os2 158(25) . . . . ? O8 C8 Os3 Os1 93(25) . . . . ? O9 C9 Os3 C8 102(23) . . . . ? O9 C9 Os3 C7 -161(23) . . . . ? O9 C9 Os3 C13 -59(23) . . . . ? O9 C9 Os3 C14 -72(23) . . . . ? O9 C9 Os3 C12 -29(23) . . . . ? O9 C9 Os3 Os2 25(23) . . . . ? O9 C9 Os3 Os1 16(23) . . . . ? O7 C7 Os3 C8 3(26) . . . . ? O7 C7 Os3 C9 -94(26) . . . . ? O7 C7 Os3 C13 159(26) . . . . ? O7 C7 Os3 C14 126(26) . . . . ? O7 C7 Os3 C12 175(26) . . . . ? O7 C7 Os3 Os2 83(26) . . . . ? O7 C7 Os3 Os1 102(26) . . . . ? O10 C13 Os3 C8 174.1(10) . . . . ? C14 C13 Os3 C8 55.8(13) . . . . ? C12 C13 Os3 C8 -78.7(12) . . . . ? O10 C13 Os3 C9 -47.4(11) . . . . ? C14 C13 Os3 C9 -165.7(7) . . . . ? C12 C13 Os3 C9 59.8(8) . . . . ? O10 C13 Os3 C7 51.9(11) . . . . ? C14 C13 Os3 C7 -66.4(8) . . . . ? C12 C13 Os3 C7 159.1(7) . . . . ? O10 C13 Os3 C14 118.3(13) . . . . ? C12 C13 Os3 C14 -134.5(10) . . . . ? O10 C13 Os3 C12 -107.2(12) . . . . ? C14 C13 Os3 C12 134.5(10) . . . . ? O10 C13 Os3 Os2 154.3(11) . . . . ? C14 C13 Os3 Os2 36.1(6) . . . . ? C12 C13 Os3 Os2 -98.4(6) . . . . ? O10 C13 Os3 Os1 -137.7(10) . . . . ? C14 C13 Os3 Os1 104.0(7) . . . . ? C12 C13 Os3 Os1 -30.5(6) . . . . ? C13 C14 Os3 C8 -151.3(7) . . . . ? C15 C14 Os3 C8 102.8(11) . . . . ? Os2 C14 Os3 C8 -22.0(7) . . . . ? C13 C14 Os3 C9 21.6(11) . . . . ? C15 C14 Os3 C9 -84.3(12) . . . . ? Os2 C14 Os3 C9 150.9(7) . . . . ? C13 C14 Os3 C7 115.1(8) . . . . ? C15 C14 Os3 C7 9.3(10) . . . . ? Os2 C14 Os3 C7 -115.5(5) . . . . ? C15 C14 Os3 C13 -105.8(13) . . . . ? Os2 C14 Os3 C13 129.4(8) . . . . ? C13 C14 Os3 C12 -27.2(7) . . . . ? C15 C14 Os3 C12 -133.0(11) . . . . ? Os2 C14 Os3 C12 102.2(4) . . . . ? C13 C14 Os3 Os2 -129.4(8) . . . . ? C15 C14 Os3 Os2 124.8(11) . . . . ? C13 C14 Os3 Os1 -69.4(6) . . . . ? C15 C14 Os3 Os1 -175.2(10) . . . . ? Os2 C14 Os3 Os1 60.0(3) . . . . ? C13 C12 Os3 C8 141.0(7) . . . . ? C11 C12 Os3 C8 -128.7(10) . . . . ? Os1 C12 Os3 C8 4.4(7) . . . . ? C13 C12 Os3 C9 -123.4(7) . . . . ? C11 C12 Os3 C9 -33.2(10) . . . . ? Os1 C12 Os3 C9 100.0(5) . . . . ? C13 C12 Os3 C7 -28.5(9) . . . . ? C11 C12 Os3 C7 61.8(11) . . . . ? Os1 C12 Os3 C7 -165.0(5) . . . . ? C11 C12 Os3 C13 90.3(11) . . . . ? Os1 C12 Os3 C13 -136.5(7) . . . . ? C13 C12 Os3 C14 27.3(6) . . . . ? C11 C12 Os3 C14 117.6(10) . . . . ? Os1 C12 Os3 C14 -109.2(5) . . . . ? C13 C12 Os3 Os2 73.5(6) . . . . ? C11 C12 Os3 Os2 163.7(9) . . . . ? Os1 C12 Os3 Os2 -63.1(2) . . . . ? C13 C12 Os3 Os1 136.5(7) . . . . ? C11 C12 Os3 Os1 -133.2(10) . . . . ? C4 Os2 Os3 C8 74.2(5) . . . . ? C6 Os2 Os3 C8 -14.6(5) . . . . ? C14 Os2 Os3 C8 161.5(6) . . . . ? P1 Os2 Os3 C8 -171.4(4) . . . . ? Os1 Os2 Os3 C8 -90.8(4) . . . . ? C4 Os2 Os3 C9 154.8(11) . . . . ? C6 Os2 Os3 C9 66.0(11) . . . . ? C14 Os2 Os3 C9 -117.8(12) . . . . ? P1 Os2 Os3 C9 -90.7(11) . . . . ? Os1 Os2 Os3 C9 -10.1(11) . . . . ? C4 Os2 Os3 C7 -19.0(5) . . . . ? C6 Os2 Os3 C7 -107.8(6) . . . . ? C14 Os2 Os3 C7 68.4(6) . . . . ? P1 Os2 Os3 C7 95.5(5) . . . . ? Os1 Os2 Os3 C7 176.1(4) . . . . ? C4 Os2 Os3 C13 -115.3(5) . . . . ? C6 Os2 Os3 C13 155.8(5) . . . . ? C14 Os2 Os3 C13 -28.0(5) . . . . ? P1 Os2 Os3 C13 -0.9(3) . . . . ? Os1 Os2 Os3 C13 79.7(3) . . . . ? C4 Os2 Os3 C14 -87.4(5) . . . . ? C6 Os2 Os3 C14 -176.2(5) . . . . ? P1 Os2 Os3 C14 27.1(4) . . . . ? Os1 Os2 Os3 C14 107.7(4) . . . . ? C4 Os2 Os3 C12 -150.8(4) . . . . ? C6 Os2 Os3 C12 120.4(4) . . . . ? C14 Os2 Os3 C12 -63.4(5) . . . . ? P1 Os2 Os3 C12 -36.3(3) . . . . ? Os1 Os2 Os3 C12 44.3(3) . . . . ? C4 Os2 Os3 Os1 165.0(3) . . . . ? C6 Os2 Os3 Os1 76.2(4) . . . . ? C14 Os2 Os3 Os1 -107.7(4) . . . . ? P1 Os2 Os3 Os1 -80.59(13) . . . . ? C1 Os1 Os3 C8 -89.5(6) . . . . ? C2 Os1 Os3 C8 158.3(9) . . . . ? C3 Os1 Os3 C8 3.0(5) . . . . ? C12 Os1 Os3 C8 -176.7(5) . . . . ? Os2 Os1 Os3 C8 80.1(4) . . . . ? C1 Os1 Os3 C9 6.8(5) . . . . ? C2 Os1 Os3 C9 -105.4(9) . . . . ? C3 Os1 Os3 C9 99.3(5) . . . . ? C12 Os1 Os3 C9 -80.4(5) . . . . ? Os2 Os1 Os3 C9 176.4(4) . . . . ? C1 Os1 Os3 C7 170(2) . . . . ? C2 Os1 Os3 C7 58(2) . . . . ? C3 Os1 Os3 C7 -97(2) . . . . ? C12 Os1 Os3 C7 83(2) . . . . ? Os2 Os1 Os3 C7 -20(2) . . . . ? C1 Os1 Os3 C13 111.7(5) . . . . ? C2 Os1 Os3 C13 -0.5(9) . . . . ? C3 Os1 Os3 C13 -155.8(4) . . . . ? C12 Os1 Os3 C13 24.5(4) . . . . ? Os2 Os1 Os3 C13 -78.7(3) . . . . ? C1 Os1 Os3 C14 146.2(5) . . . . ? C2 Os1 Os3 C14 34.0(9) . . . . ? C3 Os1 Os3 C14 -121.3(4) . . . . ? C12 Os1 Os3 C14 59.0(5) . . . . ? Os2 Os1 Os3 C14 -44.2(3) . . . . ? C1 Os1 Os3 C12 87.2(5) . . . . ? C2 Os1 Os3 C12 -25.0(9) . . . . ? C3 Os1 Os3 C12 179.7(5) . . . . ? Os2 Os1 Os3 C12 -103.2(3) . . . . ? C1 Os1 Os3 Os2 -169.6(4) . . . . ? C2 Os1 Os3 Os2 78.2(9) . . . . ? C3 Os1 Os3 Os2 -77.1(3) . . . . ? C12 Os1 Os3 Os2 103.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.896 _refine_diff_density_min -2.819 _refine_diff_density_rms 0.330 #===END======================================================================== data_Va _database_code_depnum_ccdc_archive 'CCDC 228037' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HOs3(CO)8(C6H5O)PPh3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H21 O9 Os3 P' _chemical_formula_weight 1151.06 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3420(3) _cell_length_b 10.8940(2) _cell_length_c 15.4198(5) _cell_angle_alpha 97.2840(10) _cell_angle_beta 92.1850(10) _cell_angle_gamma 101.063(2) _cell_volume 1524.56(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 12.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.15745 _exptl_absorpt_correction_T_max 0.24790 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.12 (Bruker AXS, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14150 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 26.07 _reflns_number_total 5566 _reflns_number_gt 5334 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The idealized position of the hydride hydrogen H(1) was estimated with XHYDEX program. Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0047P)^2^+9.9358P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 5566 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C4 C 0.4071(8) -0.2342(6) 0.1086(5) 0.0324(16) Uani 1 1 d . . . C5 C 0.4529(8) 0.0222(6) 0.1265(5) 0.0302(16) Uani 1 1 d . . . C6 C 0.4637(8) -0.1162(7) 0.2757(5) 0.0318(16) Uani 1 1 d . . . C1 C -0.0263(7) -0.0590(6) 0.3803(4) 0.0237(14) Uani 1 1 d . . . C3 C 0.2632(7) -0.0196(6) 0.4029(4) 0.0241(14) Uani 1 1 d . . . C9 C -0.1440(9) -0.3207(6) 0.2130(5) 0.0370(18) Uani 1 1 d . . . C8 C 0.1350(9) -0.2939(6) 0.3051(5) 0.0344(17) Uani 1 1 d . . . C7 C 0.0773(8) -0.4014(6) 0.1271(5) 0.0301(15) Uani 1 1 d . . . C14 C 0.1512(8) -0.1421(6) 0.0901(4) 0.0266(15) Uani 1 1 d . . . C13 C 0.0210(7) -0.1047(6) 0.1114(4) 0.0237(13) Uani 1 1 d . . . C12 C -0.0196(7) -0.0590(6) 0.1971(4) 0.0210(13) Uani 1 1 d . . . C11 C -0.1718(7) -0.0470(6) 0.1860(4) 0.0263(14) Uani 1 1 d . . . H11 H -0.2315 -0.0229 0.2311 0.032 Uiso 1 1 calc R . . C10 C -0.2120(9) -0.0769(7) 0.0993(6) 0.0424(19) Uani 1 1 d . . . H10 H -0.3051 -0.0724 0.0743 0.051 Uiso 1 1 calc R . . C15 C 0.1410(9) -0.2025(7) -0.0065(5) 0.0355(17) Uani 1 1 d . . . H15A H 0.0385 -0.2232 -0.0290 0.053 Uiso 1 1 calc R . . H15B H 0.1810 -0.2797 -0.0108 0.053 Uiso 1 1 calc R . . H15C H 0.1970 -0.1429 -0.0412 0.053 Uiso 1 1 calc R . . C20 C -0.0578(7) 0.2309(6) 0.3162(4) 0.0220(13) Uani 1 1 d . . . C21 C -0.1618(8) 0.1877(6) 0.3740(5) 0.0271(14) Uani 1 1 d . . . H21 H -0.1341 0.1478 0.4216 0.033 Uiso 1 1 calc R . . C22 C -0.3063(8) 0.2029(6) 0.3623(5) 0.0318(16) Uani 1 1 d . . . H22 H -0.3763 0.1738 0.4019 0.038 Uiso 1 1 calc R . . C23 C -0.3474(8) 0.2607(7) 0.2922(5) 0.0353(17) Uani 1 1 d . . . H23 H -0.4459 0.2697 0.2833 0.042 Uiso 1 1 calc R . . C24 C -0.2451(9) 0.3044(7) 0.2364(5) 0.0347(17) Uani 1 1 d . . . H24 H -0.2731 0.3449 0.1893 0.042 Uiso 1 1 calc R . . C25 C -0.1006(8) 0.2908(6) 0.2475(4) 0.0262(14) Uani 1 1 d . . . H25 H -0.0311 0.3222 0.2082 0.031 Uiso 1 1 calc R . . C26 C 0.2295(7) 0.2907(6) 0.2526(4) 0.0214(13) Uani 1 1 d . . . C27 C 0.2334(8) 0.2391(6) 0.1652(4) 0.0299(15) Uani 1 1 d . . . H27 H 0.1782 0.1571 0.1446 0.036 Uiso 1 1 calc R . . C28 C 0.3174(9) 0.3068(7) 0.1083(5) 0.0332(16) Uani 1 1 d . . . H28 H 0.3194 0.2712 0.0489 0.040 Uiso 1 1 calc R . . C29 C 0.3980(8) 0.4258(7) 0.1377(5) 0.0317(16) Uani 1 1 d . . . H29 H 0.4601 0.4701 0.0997 0.038 Uiso 1 1 calc R . . C30 C 0.3880(8) 0.4805(6) 0.2227(5) 0.0314(16) Uani 1 1 d . . . H30 H 0.4387 0.5644 0.2418 0.038 Uiso 1 1 calc R . . C31 C 0.3051(7) 0.4140(6) 0.2799(4) 0.0252(14) Uani 1 1 d . . . H31 H 0.2994 0.4523 0.3383 0.030 Uiso 1 1 calc R . . C32 C 0.1997(7) 0.2867(6) 0.4347(4) 0.0208(13) Uani 1 1 d . . . C33 C 0.3415(8) 0.2798(6) 0.4622(4) 0.0275(14) Uani 1 1 d . . . H33 H 0.3915 0.2241 0.4285 0.033 Uiso 1 1 calc R . . C34 C 0.4100(8) 0.3520(7) 0.5371(5) 0.0322(16) Uani 1 1 d . . . H34 H 0.5076 0.3480 0.5543 0.039 Uiso 1 1 calc R . . C35 C 0.3359(9) 0.4308(7) 0.5874(5) 0.0345(17) Uani 1 1 d . . . H35 H 0.3828 0.4810 0.6393 0.041 Uiso 1 1 calc R . . C36 C 0.1935(9) 0.4367(7) 0.5624(5) 0.0354(17) Uani 1 1 d . . . H36 H 0.1424 0.4895 0.5978 0.042 Uiso 1 1 calc R . . C37 C 0.1254(8) 0.3653(6) 0.4854(5) 0.0279(14) Uani 1 1 d . . . H37 H 0.0284 0.3704 0.4676 0.034 Uiso 1 1 calc R . . O4 O 0.4582(6) -0.3067(5) 0.0664(4) 0.0412(13) Uani 1 1 d . . . O5 O 0.5211(6) 0.0959(5) 0.0900(4) 0.0409(13) Uani 1 1 d . . . O6 O 0.5419(7) -0.1265(6) 0.3317(4) 0.0492(15) Uani 1 1 d . . . O1 O -0.1210(6) -0.0910(5) 0.4229(3) 0.0366(12) Uani 1 1 d . . . O3 O 0.3397(6) -0.0280(5) 0.4611(3) 0.0382(12) Uani 1 1 d . . . O9 O -0.2663(7) -0.3611(6) 0.2169(5) 0.0571(17) Uani 1 1 d . . . O8 O 0.1828(7) -0.3245(5) 0.3663(3) 0.0432(14) Uani 1 1 d . . . O7 O 0.0914(7) -0.4920(5) 0.0838(4) 0.0478(15) Uani 1 1 d . . . O10 O -0.0975(6) -0.1164(5) 0.0491(3) 0.0409(13) Uani 1 1 d . . . P1 P 0.12503(17) 0.19772(14) 0.32871(10) 0.0183(3) Uani 1 1 d . . . Os2 Os 0.33166(3) -0.10746(2) 0.177153(17) 0.02322(8) Uani 1 1 d . . . Os1 Os 0.12668(3) -0.01768(2) 0.306693(15) 0.01763(7) Uani 1 1 d . . . Os3 Os 0.05629(3) -0.25275(2) 0.199766(16) 0.02115(8) Uani 1 1 d . . . H1 H 0.2858 0.0325 0.2429 0.050 Uiso 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 C4 0.037(5) 0.026(3) 0.033(4) 0.007(3) 0.012(3) 0.001(3) C5 0.032(4) 0.028(3) 0.031(4) -0.006(3) 0.015(3) 0.009(3) C6 0.024(4) 0.035(4) 0.042(4) 0.009(3) 0.018(3) 0.013(3) C1 0.024(4) 0.024(3) 0.026(3) 0.004(3) 0.003(3) 0.011(3) C3 0.020(4) 0.029(3) 0.025(3) 0.001(3) 0.011(3) 0.011(3) C9 0.046(6) 0.024(3) 0.038(4) 0.007(3) 0.004(3) -0.003(3) C8 0.040(5) 0.023(3) 0.039(4) 0.000(3) 0.005(3) 0.006(3) C7 0.033(4) 0.028(4) 0.028(4) 0.008(3) -0.001(3) 0.002(3) C14 0.047(5) 0.017(3) 0.024(3) 0.012(2) 0.023(3) 0.014(3) C13 0.027(4) 0.022(3) 0.020(3) 0.001(2) -0.005(3) 0.000(2) C12 0.019(4) 0.021(3) 0.023(3) 0.007(2) 0.005(2) 0.002(2) C11 0.020(4) 0.034(4) 0.023(3) -0.002(3) 0.001(3) 0.005(3) C10 0.033(5) 0.044(4) 0.053(5) 0.006(4) 0.006(4) 0.015(3) C15 0.045(5) 0.040(4) 0.024(4) 0.006(3) 0.010(3) 0.011(3) C20 0.015(4) 0.024(3) 0.025(3) -0.004(2) 0.001(2) 0.004(2) C21 0.027(4) 0.024(3) 0.031(4) 0.003(3) 0.004(3) 0.006(3) C22 0.022(4) 0.032(4) 0.042(4) 0.000(3) 0.007(3) 0.008(3) C23 0.024(4) 0.040(4) 0.040(4) -0.007(3) -0.003(3) 0.012(3) C24 0.037(5) 0.040(4) 0.029(4) 0.000(3) -0.009(3) 0.019(3) C25 0.031(4) 0.024(3) 0.023(3) -0.001(3) 0.002(3) 0.004(3) C26 0.022(4) 0.019(3) 0.024(3) 0.004(2) 0.002(2) 0.004(2) C27 0.038(4) 0.021(3) 0.028(4) 0.002(3) 0.008(3) 0.000(3) C28 0.043(5) 0.032(4) 0.027(4) 0.008(3) 0.015(3) 0.009(3) C29 0.030(4) 0.033(4) 0.036(4) 0.015(3) 0.014(3) 0.006(3) C30 0.032(4) 0.023(3) 0.039(4) 0.012(3) 0.000(3) -0.002(3) C31 0.023(4) 0.025(3) 0.026(3) 0.004(3) -0.001(3) 0.001(3) C32 0.023(4) 0.020(3) 0.019(3) 0.002(2) 0.002(2) 0.003(2) C33 0.032(4) 0.025(3) 0.025(3) 0.000(3) 0.004(3) 0.006(3) C34 0.023(4) 0.040(4) 0.029(4) 0.003(3) -0.005(3) -0.004(3) C35 0.041(5) 0.036(4) 0.021(3) -0.006(3) -0.005(3) 0.001(3) C36 0.044(5) 0.035(4) 0.025(4) -0.009(3) 0.001(3) 0.013(3) C37 0.022(4) 0.028(3) 0.033(4) -0.002(3) 0.002(3) 0.008(3) O4 0.051(4) 0.027(3) 0.050(3) 0.003(2) 0.026(3) 0.016(2) O5 0.046(4) 0.028(3) 0.049(3) 0.008(2) 0.025(3) 0.002(2) O6 0.036(4) 0.070(4) 0.049(4) 0.016(3) 0.006(3) 0.022(3) O1 0.036(3) 0.038(3) 0.038(3) 0.011(2) 0.021(2) 0.005(2) O3 0.039(3) 0.056(3) 0.022(3) 0.003(2) -0.002(2) 0.018(2) O9 0.028(4) 0.063(4) 0.076(5) 0.027(3) 0.006(3) -0.012(3) O8 0.065(4) 0.036(3) 0.031(3) 0.013(2) -0.005(3) 0.015(3) O7 0.068(4) 0.029(3) 0.043(3) -0.011(2) -0.013(3) 0.015(3) O10 0.050(4) 0.041(3) 0.027(3) 0.007(2) -0.010(2) -0.002(2) P1 0.0167(9) 0.0192(7) 0.0181(8) 0.0005(6) 0.0044(6) 0.0021(6) Os2 0.02331(16) 0.01925(13) 0.02750(15) 0.00251(10) 0.01106(10) 0.00381(10) Os1 0.01781(15) 0.01781(12) 0.01680(13) 0.00119(9) 0.00419(9) 0.00256(9) Os3 0.02399(16) 0.01684(12) 0.02124(14) 0.00227(9) 0.00452(10) 0.00021(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C4 O4 1.146(9) . ? C4 Os2 1.892(7) . ? C5 O5 1.146(8) . ? C5 Os2 1.903(7) . ? C6 O6 1.140(9) . ? C6 Os2 1.944(8) . ? C1 O1 1.150(8) . ? C1 Os1 1.881(7) . ? C3 O3 1.150(8) . ? C3 Os1 1.924(7) . ? C9 O9 1.150(10) . ? C9 Os3 1.904(8) . ? C8 O8 1.142(9) . ? C8 Os3 1.898(8) . ? C7 O7 1.152(9) . ? C7 Os3 1.896(7) . ? C14 C13 1.393(10) . ? C14 C15 1.542(9) . ? C14 Os2 2.059(8) . ? C14 Os3 2.306(6) . ? C13 O10 1.414(8) . ? C13 C12 1.442(9) . ? C13 Os3 2.300(6) . ? C12 C11 1.458(9) . ? C12 Os1 2.079(6) . ? C12 Os3 2.357(6) . ? C11 C10 1.357(11) . ? C11 H11 0.9500 . ? C10 O10 1.443(10) . ? C10 H10 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C20 C25 1.397(9) . ? C20 C21 1.399(9) . ? C20 P1 1.820(6) . ? C21 C22 1.399(10) . ? C21 H21 0.9500 . ? C22 C23 1.395(11) . ? C22 H22 0.9500 . ? C23 C24 1.368(11) . ? C23 H23 0.9500 . ? C24 C25 1.392(10) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.396(9) . ? C26 C27 1.398(9) . ? C26 P1 1.835(6) . ? C27 C28 1.387(9) . ? C27 H27 0.9500 . ? C28 C29 1.379(10) . ? C28 H28 0.9500 . ? C29 C30 1.384(10) . ? C29 H29 0.9500 . ? C30 C31 1.379(9) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.388(9) . ? C32 C33 1.395(9) . ? C32 P1 1.829(6) . ? C33 C34 1.373(10) . ? C33 H33 0.9500 . ? C34 C35 1.385(11) . ? C34 H34 0.9500 . ? C35 C36 1.387(11) . ? C35 H35 0.9500 . ? C36 C37 1.392(10) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? P1 Os1 2.3311(15) . ? Os2 Os3 2.8090(4) . ? Os2 Os1 3.0214(3) . ? Os2 H1 1.8513 . ? Os1 Os3 2.8123(3) . ? Os1 H1 1.8470 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 C4 Os2 176.8(6) . . ? O5 C5 Os2 174.9(7) . . ? O6 C6 Os2 176.9(6) . . ? O1 C1 Os1 176.2(6) . . ? O3 C3 Os1 175.7(6) . . ? O9 C9 Os3 176.7(7) . . ? O8 C8 Os3 176.5(6) . . ? O7 C7 Os3 179.0(7) . . ? C13 C14 C15 110.5(6) . . ? C13 C14 Os2 122.5(5) . . ? C15 C14 Os2 126.9(5) . . ? C13 C14 Os3 72.1(4) . . ? C15 C14 Os3 122.4(5) . . ? Os2 C14 Os3 79.9(2) . . ? C14 C13 O10 122.5(6) . . ? C14 C13 C12 127.5(6) . . ? O10 C13 C12 109.8(6) . . ? C14 C13 Os3 72.7(4) . . ? O10 C13 Os3 125.9(4) . . ? C12 C13 Os3 74.1(3) . . ? C13 C12 C11 106.1(6) . . ? C13 C12 Os1 122.5(5) . . ? C11 C12 Os1 131.3(5) . . ? C13 C12 Os3 69.8(3) . . ? C11 C12 Os3 124.0(4) . . ? Os1 C12 Os3 78.4(2) . . ? C10 C11 C12 107.0(6) . . ? C10 C11 H11 126.5 . . ? C12 C11 H11 126.5 . . ? C11 C10 O10 112.4(7) . . ? C11 C10 H10 123.8 . . ? O10 C10 H10 123.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C25 C20 C21 118.7(6) . . ? C25 C20 P1 122.3(5) . . ? C21 C20 P1 118.9(5) . . ? C22 C21 C20 120.4(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 119.9(7) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 119.6(7) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 121.2(7) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C24 C25 C20 120.1(6) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? C31 C26 C27 118.7(6) . . ? C31 C26 P1 121.2(5) . . ? C27 C26 P1 120.1(5) . . ? C28 C27 C26 120.4(6) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C29 C28 C27 120.2(7) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 119.7(6) . . ? C28 C29 H29 120.1 . . ? C30 C29 H29 120.1 . . ? C31 C30 C29 120.5(6) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C26 120.3(6) . . ? C30 C31 H31 119.8 . . ? C26 C31 H31 119.8 . . ? C37 C32 C33 119.3(6) . . ? C37 C32 P1 123.1(5) . . ? C33 C32 P1 117.5(5) . . ? C34 C33 C32 121.1(6) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 119.5(7) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 120.3(6) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 120.0(7) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C32 C37 C36 119.8(7) . . ? C32 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C13 O10 C10 104.5(6) . . ? C20 P1 C32 104.3(3) . . ? C20 P1 C26 103.9(3) . . ? C32 P1 C26 101.5(3) . . ? C20 P1 Os1 112.8(2) . . ? C32 P1 Os1 117.5(2) . . ? C26 P1 Os1 115.2(2) . . ? C4 Os2 C5 91.5(3) . . ? C4 Os2 C6 90.1(3) . . ? C5 Os2 C6 98.5(3) . . ? C4 Os2 C14 89.4(3) . . ? C5 Os2 C14 99.5(3) . . ? C6 Os2 C14 162.0(3) . . ? C4 Os2 Os3 97.9(2) . . ? C5 Os2 Os3 151.4(2) . . ? C6 Os2 Os3 108.4(2) . . ? C14 Os2 Os3 53.93(16) . . ? C4 Os2 Os1 153.2(2) . . ? C5 Os2 Os1 115.18(19) . . ? C6 Os2 Os1 88.4(2) . . ? C14 Os2 Os1 84.02(16) . . ? Os3 Os2 Os1 57.541(8) . . ? C4 Os2 H1 171.1 . . ? C5 Os2 H1 80.6 . . ? C6 Os2 H1 86.9 . . ? C14 Os2 H1 96.0 . . ? Os3 Os2 H1 91.0 . . ? Os1 Os2 H1 35.2 . . ? C1 Os1 C3 88.6(3) . . ? C1 Os1 C12 91.0(3) . . ? C3 Os1 C12 167.0(2) . . ? C1 Os1 P1 93.99(19) . . ? C3 Os1 P1 97.62(19) . . ? C12 Os1 P1 95.40(17) . . ? C1 Os1 Os3 93.52(19) . . ? C3 Os1 Os3 111.84(19) . . ? C12 Os1 Os3 55.18(17) . . ? P1 Os1 Os3 149.73(4) . . ? C1 Os1 Os2 148.21(19) . . ? C3 Os1 Os2 90.85(18) . . ? C12 Os1 Os2 82.64(17) . . ? P1 Os1 Os2 117.55(4) . . ? Os3 Os1 Os2 57.434(8) . . ? C1 Os1 H1 174.9 . . ? C3 Os1 H1 87.5 . . ? C12 Os1 H1 93.5 . . ? P1 Os1 H1 83.2 . . ? Os3 Os1 H1 91.0 . . ? Os2 Os1 H1 35.3 . . ? C7 Os3 C8 96.7(3) . . ? C7 Os3 C9 91.5(3) . . ? C8 Os3 C9 97.9(3) . . ? C7 Os3 C13 108.3(3) . . ? C8 Os3 C13 150.1(3) . . ? C9 Os3 C13 97.7(3) . . ? C7 Os3 C14 87.1(3) . . ? C8 Os3 C14 134.7(3) . . ? C9 Os3 C14 127.2(3) . . ? C13 Os3 C14 35.2(2) . . ? C7 Os3 C12 142.6(3) . . ? C8 Os3 C12 120.7(3) . . ? C9 Os3 C12 85.4(3) . . ? C13 Os3 C12 36.1(2) . . ? C14 Os3 C12 66.1(2) . . ? C7 Os3 Os2 97.1(2) . . ? C8 Os3 Os2 88.7(2) . . ? C9 Os3 Os2 168.5(2) . . ? C13 Os3 Os2 72.36(17) . . ? C14 Os3 Os2 46.2(2) . . ? C12 Os3 Os2 83.05(15) . . ? C7 Os3 Os1 160.9(2) . . ? C8 Os3 Os1 77.1(2) . . ? C9 Os3 Os1 107.1(2) . . ? C13 Os3 Os1 73.98(15) . . ? C14 Os3 Os1 84.89(16) . . ? C12 Os3 Os1 46.40(15) . . ? Os2 Os3 Os1 65.025(9) . . ? 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 C15 C14 C13 O10 -3.2(8) . . . . ? Os2 C14 C13 O10 173.1(4) . . . . ? Os3 C14 C13 O10 -122.0(6) . . . . ? C15 C14 C13 C12 171.8(6) . . . . ? Os2 C14 C13 C12 -11.8(9) . . . . ? Os3 C14 C13 C12 53.1(6) . . . . ? C15 C14 C13 Os3 118.7(5) . . . . ? Os2 C14 C13 Os3 -64.9(4) . . . . ? C14 C13 C12 C11 -173.5(6) . . . . ? O10 C13 C12 C11 2.1(7) . . . . ? Os3 C13 C12 C11 -121.0(5) . . . . ? C14 C13 C12 Os1 8.3(9) . . . . ? O10 C13 C12 Os1 -176.2(4) . . . . ? Os3 C13 C12 Os1 60.8(4) . . . . ? C14 C13 C12 Os3 -52.5(6) . . . . ? O10 C13 C12 Os3 123.1(5) . . . . ? C13 C12 C11 C10 -3.2(7) . . . . ? Os1 C12 C11 C10 174.8(5) . . . . ? Os3 C12 C11 C10 -79.5(7) . . . . ? C12 C11 C10 O10 3.3(8) . . . . ? C25 C20 C21 C22 0.8(9) . . . . ? P1 C20 C21 C22 -175.0(5) . . . . ? C20 C21 C22 C23 0.4(10) . . . . ? C21 C22 C23 C24 -1.3(10) . . . . ? C22 C23 C24 C25 0.9(11) . . . . ? C23 C24 C25 C20 0.3(10) . . . . ? C21 C20 C25 C24 -1.2(9) . . . . ? P1 C20 C25 C24 174.5(5) . . . . ? C31 C26 C27 C28 3.5(10) . . . . ? P1 C26 C27 C28 -177.1(6) . . . . ? C26 C27 C28 C29 0.1(12) . . . . ? C27 C28 C29 C30 -3.8(12) . . . . ? C28 C29 C30 C31 3.9(11) . . . . ? C29 C30 C31 C26 -0.3(11) . . . . ? C27 C26 C31 C30 -3.4(10) . . . . ? P1 C26 C31 C30 177.2(5) . . . . ? C37 C32 C33 C34 -1.9(10) . . . . ? P1 C32 C33 C34 174.4(5) . . . . ? C32 C33 C34 C35 1.6(11) . . . . ? C33 C34 C35 C36 0.0(11) . . . . ? C34 C35 C36 C37 -1.4(12) . . . . ? C33 C32 C37 C36 0.5(10) . . . . ? P1 C32 C37 C36 -175.5(5) . . . . ? C35 C36 C37 C32 1.1(11) . . . . ? C14 C13 O10 C10 175.6(6) . . . . ? C12 C13 O10 C10 -0.2(7) . . . . ? Os3 C13 O10 C10 84.2(6) . . . . ? C11 C10 O10 C13 -2.0(8) . . . . ? C25 C20 P1 C32 118.7(5) . . . . ? C21 C20 P1 C32 -65.6(5) . . . . ? C25 C20 P1 C26 12.8(6) . . . . ? C21 C20 P1 C26 -171.6(5) . . . . ? C25 C20 P1 Os1 -112.6(5) . . . . ? C21 C20 P1 Os1 63.1(5) . . . . ? C37 C32 P1 C20 -3.6(6) . . . . ? C33 C32 P1 C20 -179.7(5) . . . . ? C37 C32 P1 C26 104.1(6) . . . . ? C33 C32 P1 C26 -72.0(5) . . . . ? C37 C32 P1 Os1 -129.3(5) . . . . ? C33 C32 P1 Os1 54.5(5) . . . . ? C31 C26 P1 C20 91.3(6) . . . . ? C27 C26 P1 C20 -88.1(6) . . . . ? C31 C26 P1 C32 -16.8(6) . . . . ? C27 C26 P1 C32 163.9(6) . . . . ? C31 C26 P1 Os1 -144.8(5) . . . . ? C27 C26 P1 Os1 35.8(6) . . . . ? O4 C4 Os2 C5 18(13) . . . . ? O4 C4 Os2 C6 -81(13) . . . . ? O4 C4 Os2 C14 117(13) . . . . ? O4 C4 Os2 Os3 171(13) . . . . ? O4 C4 Os2 Os1 -167(12) . . . . ? O5 C5 Os2 C4 58(7) . . . . ? O5 C5 Os2 C6 148(7) . . . . ? O5 C5 Os2 C14 -32(7) . . . . ? O5 C5 Os2 Os3 -52(7) . . . . ? O5 C5 Os2 Os1 -119(7) . . . . ? O6 C6 Os2 C4 -18(13) . . . . ? O6 C6 Os2 C5 -109(13) . . . . ? O6 C6 Os2 C14 71(13) . . . . ? O6 C6 Os2 Os3 81(13) . . . . ? O6 C6 Os2 Os1 136(13) . . . . ? C13 C14 Os2 C4 161.3(5) . . . . ? C15 C14 Os2 C4 -23.0(6) . . . . ? Os3 C14 Os2 C4 100.2(2) . . . . ? C13 C14 Os2 C5 -107.2(5) . . . . ? C15 C14 Os2 C5 68.5(6) . . . . ? Os3 C14 Os2 C5 -168.3(2) . . . . ? C13 C14 Os2 C6 72.9(10) . . . . ? C15 C14 Os2 C6 -111.4(9) . . . . ? Os3 C14 Os2 C6 11.8(9) . . . . ? C13 C14 Os2 Os3 61.1(5) . . . . ? C15 C14 Os2 Os3 -123.1(6) . . . . ? C13 C14 Os2 Os1 7.4(5) . . . . ? C15 C14 Os2 Os1 -176.9(5) . . . . ? Os3 C14 Os2 Os1 -53.75(11) . . . . ? O1 C1 Os1 C3 -102(9) . . . . ? O1 C1 Os1 C12 65(9) . . . . ? O1 C1 Os1 P1 160(9) . . . . ? O1 C1 Os1 Os3 9(9) . . . . ? O1 C1 Os1 Os2 -13(9) . . . . ? O3 C3 Os1 C1 50(7) . . . . ? O3 C3 Os1 C12 -38(8) . . . . ? O3 C3 Os1 P1 144(7) . . . . ? O3 C3 Os1 Os3 -43(8) . . . . ? O3 C3 Os1 Os2 -98(7) . . . . ? C13 C12 Os1 C1 -150.3(5) . . . . ? C11 C12 Os1 C1 31.9(6) . . . . ? Os3 C12 Os1 C1 -93.6(2) . . . . ? C13 C12 Os1 C3 -62.2(13) . . . . ? C11 C12 Os1 C3 120.1(11) . . . . ? Os3 C12 Os1 C3 -5.4(12) . . . . ? C13 C12 Os1 P1 115.6(5) . . . . ? C11 C12 Os1 P1 -62.2(6) . . . . ? Os3 C12 Os1 P1 172.30(11) . . . . ? C13 C12 Os1 Os3 -56.7(4) . . . . ? C11 C12 Os1 Os3 125.5(6) . . . . ? C13 C12 Os1 Os2 -1.6(5) . . . . ? C11 C12 Os1 Os2 -179.4(6) . . . . ? Os3 C12 Os1 Os2 55.16(11) . . . . ? C20 P1 Os1 C1 -48.1(3) . . . . ? C32 P1 Os1 C1 73.4(3) . . . . ? C26 P1 Os1 C1 -167.1(3) . . . . ? C20 P1 Os1 C3 -137.2(3) . . . . ? C32 P1 Os1 C3 -15.7(3) . . . . ? C26 P1 Os1 C3 103.8(3) . . . . ? C20 P1 Os1 C12 43.3(3) . . . . ? C32 P1 Os1 C12 164.8(3) . . . . ? C26 P1 Os1 C12 -75.7(3) . . . . ? C20 P1 Os1 Os3 55.9(2) . . . . ? C32 P1 Os1 Os3 177.4(2) . . . . ? C26 P1 Os1 Os3 -63.1(3) . . . . ? C20 P1 Os1 Os2 127.8(2) . . . . ? C32 P1 Os1 Os2 -110.7(2) . . . . ? C26 P1 Os1 Os2 8.8(2) . . . . ? C4 Os2 Os1 C1 0.7(6) . . . . ? C5 Os2 Os1 C1 175.1(5) . . . . ? C6 Os2 Os1 C1 -86.2(4) . . . . ? C14 Os2 Os1 C1 77.4(4) . . . . ? Os3 Os2 Os1 C1 26.8(4) . . . . ? C4 Os2 Os1 C3 89.5(6) . . . . ? C5 Os2 Os1 C3 -96.2(3) . . . . ? C6 Os2 Os1 C3 2.5(3) . . . . ? C14 Os2 Os1 C3 166.2(3) . . . . ? Os3 Os2 Os1 C3 115.6(2) . . . . ? C4 Os2 Os1 C12 -79.2(6) . . . . ? C5 Os2 Os1 C12 95.2(3) . . . . ? C6 Os2 Os1 C12 -166.2(3) . . . . ? C14 Os2 Os1 C12 -2.5(2) . . . . ? Os3 Os2 Os1 C12 -53.08(16) . . . . ? C4 Os2 Os1 P1 -171.5(5) . . . . ? C5 Os2 Os1 P1 2.9(3) . . . . ? C6 Os2 Os1 P1 101.6(2) . . . . ? C14 Os2 Os1 P1 -94.77(17) . . . . ? Os3 Os2 Os1 P1 -145.35(5) . . . . ? C4 Os2 Os1 Os3 -26.1(5) . . . . ? C5 Os2 Os1 Os3 148.2(3) . . . . ? C6 Os2 Os1 Os3 -113.1(2) . . . . ? C14 Os2 Os1 Os3 50.58(16) . . . . ? O7 C7 Os3 C8 -16(44) . . . . ? O7 C7 Os3 C9 -114(44) . . . . ? O7 C7 Os3 C13 147(44) . . . . ? O7 C7 Os3 C14 119(44) . . . . ? O7 C7 Os3 C12 162(44) . . . . ? O7 C7 Os3 Os2 74(44) . . . . ? O7 C7 Os3 Os1 54(45) . . . . ? O8 C8 Os3 C7 -5(12) . . . . ? O8 C8 Os3 C9 88(12) . . . . ? O8 C8 Os3 C13 -152(11) . . . . ? O8 C8 Os3 C14 -97(12) . . . . ? O8 C8 Os3 C12 177(12) . . . . ? O8 C8 Os3 Os2 -102(12) . . . . ? O8 C8 Os3 Os1 -167(12) . . . . ? O9 C9 Os3 C7 -70(12) . . . . ? O9 C9 Os3 C8 -167(12) . . . . ? O9 C9 Os3 C13 38(12) . . . . ? O9 C9 Os3 C14 17(12) . . . . ? O9 C9 Os3 C12 72(12) . . . . ? O9 C9 Os3 Os2 68(13) . . . . ? O9 C9 Os3 Os1 114(12) . . . . ? C14 C13 Os3 C7 -55.9(5) . . . . ? O10 C13 Os3 C7 62.1(6) . . . . ? C12 C13 Os3 C7 165.4(4) . . . . ? C14 C13 Os3 C8 89.1(7) . . . . ? O10 C13 Os3 C8 -152.9(6) . . . . ? C12 C13 Os3 C8 -49.6(7) . . . . ? C14 C13 Os3 C9 -150.1(4) . . . . ? O10 C13 Os3 C9 -32.0(6) . . . . ? C12 C13 Os3 C9 71.2(4) . . . . ? O10 C13 Os3 C14 118.0(7) . . . . ? C12 C13 Os3 C14 -138.7(6) . . . . ? C14 C13 Os3 C12 138.7(6) . . . . ? O10 C13 Os3 C12 -103.3(7) . . . . ? C14 C13 Os3 Os2 36.0(4) . . . . ? O10 C13 Os3 Os2 154.0(6) . . . . ? C12 C13 Os3 Os2 -102.8(4) . . . . ? C14 C13 Os3 Os1 104.3(4) . . . . ? O10 C13 Os3 Os1 -137.7(6) . . . . ? C12 C13 Os3 Os1 -34.5(3) . . . . ? C13 C14 Os3 C7 128.1(4) . . . . ? C15 C14 Os3 C7 24.7(6) . . . . ? Os2 C14 Os3 C7 -102.8(3) . . . . ? C13 C14 Os3 C8 -135.5(4) . . . . ? C15 C14 Os3 C8 121.2(6) . . . . ? Os2 C14 Os3 C8 -6.3(4) . . . . ? C13 C14 Os3 C9 38.4(5) . . . . ? C15 C14 Os3 C9 -65.0(7) . . . . ? Os2 C14 Os3 C9 167.5(3) . . . . ? C15 C14 Os3 C13 -103.4(7) . . . . ? Os2 C14 Os3 C13 129.2(4) . . . . ? C13 C14 Os3 C12 -25.1(4) . . . . ? C15 C14 Os3 C12 -128.5(6) . . . . ? Os2 C14 Os3 C12 104.0(2) . . . . ? C13 C14 Os3 Os2 -129.2(4) . . . . ? C15 C14 Os3 Os2 127.5(6) . . . . ? C13 C14 Os3 Os1 -69.3(4) . . . . ? C15 C14 Os3 Os1 -172.6(6) . . . . ? Os2 C14 Os3 Os1 59.89(13) . . . . ? C13 C12 Os3 C7 -23.2(6) . . . . ? C11 C12 Os3 C7 73.0(7) . . . . ? Os1 C12 Os3 C7 -154.6(4) . . . . ? C13 C12 Os3 C8 153.8(4) . . . . ? C11 C12 Os3 C8 -110.0(6) . . . . ? Os1 C12 Os3 C8 22.5(4) . . . . ? C13 C12 Os3 C9 -109.8(4) . . . . ? C11 C12 Os3 C9 -13.5(6) . . . . ? Os1 C12 Os3 C9 118.9(3) . . . . ? C11 C12 Os3 C13 96.2(6) . . . . ? Os1 C12 Os3 C13 -131.3(4) . . . . ? C13 C12 Os3 C14 24.6(4) . . . . ? C11 C12 Os3 C14 120.8(6) . . . . ? Os1 C12 Os3 C14 -106.7(3) . . . . ? C13 C12 Os3 Os2 69.4(4) . . . . ? C11 C12 Os3 Os2 165.7(5) . . . . ? Os1 C12 Os3 Os2 -61.89(14) . . . . ? C13 C12 Os3 Os1 131.3(4) . . . . ? C11 C12 Os3 Os1 -132.4(6) . . . . ? C4 Os2 Os3 C7 -4.5(3) . . . . ? C5 Os2 Os3 C7 103.5(4) . . . . ? C6 Os2 Os3 C7 -97.2(3) . . . . ? C14 Os2 Os3 C7 79.0(3) . . . . ? Os1 Os2 Os3 C7 -172.9(2) . . . . ? C4 Os2 Os3 C8 92.0(3) . . . . ? C5 Os2 Os3 C8 -159.9(4) . . . . ? C6 Os2 Os3 C8 -0.7(3) . . . . ? C14 Os2 Os3 C8 175.5(3) . . . . ? Os1 Os2 Os3 C8 -76.4(2) . . . . ? C4 Os2 Os3 C9 -142.8(12) . . . . ? C5 Os2 Os3 C9 -34.7(12) . . . . ? C6 Os2 Os3 C9 124.5(12) . . . . ? C14 Os2 Os3 C9 -59.3(12) . . . . ? Os1 Os2 Os3 C9 48.8(12) . . . . ? C4 Os2 Os3 C13 -111.5(3) . . . . ? C5 Os2 Os3 C13 -3.4(4) . . . . ? C6 Os2 Os3 C13 155.8(3) . . . . ? C14 Os2 Os3 C13 -28.0(3) . . . . ? Os1 Os2 Os3 C13 80.13(17) . . . . ? C4 Os2 Os3 C14 -83.5(3) . . . . ? C5 Os2 Os3 C14 24.6(4) . . . . ? C6 Os2 Os3 C14 -176.2(3) . . . . ? Os1 Os2 Os3 C14 108.1(2) . . . . ? C4 Os2 Os3 C12 -146.8(3) . . . . ? C5 Os2 Os3 C12 -38.7(4) . . . . ? C6 Os2 Os3 C12 120.5(3) . . . . ? C14 Os2 Os3 C12 -63.3(3) . . . . ? Os1 Os2 Os3 C12 44.80(15) . . . . ? C4 Os2 Os3 Os1 168.4(2) . . . . ? C5 Os2 Os3 Os1 -83.5(4) . . . . ? C6 Os2 Os3 Os1 75.7(2) . . . . ? C14 Os2 Os3 Os1 -108.1(2) . . . . ? C1 Os1 Os3 C7 -144.2(7) . . . . ? C3 Os1 Os3 C7 -54.3(7) . . . . ? C12 Os1 Os3 C7 127.0(7) . . . . ? P1 Os1 Os3 C7 111.7(6) . . . . ? Os2 Os1 Os3 C7 22.0(6) . . . . ? C1 Os1 Os3 C8 -71.5(3) . . . . ? C3 Os1 Os3 C8 18.4(3) . . . . ? C12 Os1 Os3 C8 -160.3(3) . . . . ? P1 Os1 Os3 C8 -175.7(3) . . . . ? Os2 Os1 Os3 C8 94.7(2) . . . . ? C1 Os1 Os3 C9 22.9(3) . . . . ? C3 Os1 Os3 C9 112.8(3) . . . . ? C12 Os1 Os3 C9 -65.9(3) . . . . ? P1 Os1 Os3 C9 -81.3(3) . . . . ? Os2 Os1 Os3 C9 -170.9(2) . . . . ? C1 Os1 Os3 C13 116.1(3) . . . . ? C3 Os1 Os3 C13 -153.9(3) . . . . ? C12 Os1 Os3 C13 27.4(3) . . . . ? P1 Os1 Os3 C13 12.0(2) . . . . ? Os2 Os1 Os3 C13 -77.64(18) . . . . ? C1 Os1 Os3 C14 150.3(3) . . . . ? C3 Os1 Os3 C14 -119.8(3) . . . . ? C12 Os1 Os3 C14 61.5(3) . . . . ? P1 Os1 Os3 C14 46.1(2) . . . . ? Os2 Os1 Os3 C14 -43.53(18) . . . . ? C1 Os1 Os3 C12 88.8(3) . . . . ? C3 Os1 Os3 C12 178.7(3) . . . . ? P1 Os1 Os3 C12 -15.3(2) . . . . ? Os2 Os1 Os3 C12 -105.0(2) . . . . ? C1 Os1 Os3 Os2 -166.21(19) . . . . ? C3 Os1 Os3 Os2 -76.3(2) . . . . ? C12 Os1 Os3 Os2 105.0(2) . . . . ? P1 Os1 Os3 Os2 89.68(8) . . . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 1.617 _refine_diff_density_min -1.807 _refine_diff_density_rms 0.163 #===END======================================================================== data_VI _database_code_depnum_ccdc_archive 'CCDC 228038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common HOs3(CO)8(C6H5O)(P(C6H4CF3)3) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H18 F9 O9 Os3 P' _chemical_formula_weight 1355.06 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' F F 0.0171 0.0103 '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 'P 21/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 8.62560(10) _cell_length_b 11.4157(2) _cell_length_c 37.6229(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.1791(9) _cell_angle_gamma 90.00 _cell_volume 3701.95(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 10.414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.06948 _exptl_absorpt_correction_T_max 0.10975 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.12 (Bruker AXS, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17381 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.25 _reflns_number_total 6119 _reflns_number_gt 5026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The idealized position of the hydride hydrogen H(1) was estimated with XHYDEX program. Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0268P)^2^+30.5427P] 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 6119 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7177(14) 0.9018(10) 0.4717(3) 0.046(3) Uani 1 1 d . . . C2 C 0.8459(15) 0.7129(11) 0.4369(3) 0.053(3) Uani 1 1 d . . . C3 C 0.5741(13) 0.6889(10) 0.4795(3) 0.040(3) Uani 1 1 d . . . C4 C 0.2090(13) 0.6409(10) 0.3705(3) 0.041(3) Uani 1 1 d . . . C6 C 0.3345(13) 0.5729(9) 0.4305(3) 0.038(3) Uani 1 1 d . . . C9 C 0.4220(15) 1.0505(11) 0.4351(4) 0.054(3) Uani 1 1 d . . . C8 C 0.2863(14) 0.8325(9) 0.4520(3) 0.039(3) Uani 1 1 d . . . C7 C 0.1903(14) 0.9498(12) 0.3895(4) 0.058(4) Uani 1 1 d . . . C12 C 0.6450(12) 0.9064(8) 0.3996(3) 0.034(2) Uani 1 1 d . . . C13 C 0.5481(14) 0.8987(8) 0.3672(3) 0.038(3) Uani 1 1 d . . . C14 C 0.4339(12) 0.8135(10) 0.3595(3) 0.040(3) Uani 1 1 d . . . C11 C 0.7286(13) 1.0189(10) 0.3941(4) 0.048(3) Uani 1 1 d . . . H11 H 0.7976 1.0566 0.4107 0.058 Uiso 1 1 calc R . . C10 C 0.6894(14) 1.0562(10) 0.3620(4) 0.051(3) Uani 1 1 d . . . H10 H 0.7344 1.1239 0.3520 0.061 Uiso 1 1 calc R . . C15 C 0.3492(14) 0.8326(11) 0.3241(3) 0.049(3) Uani 1 1 d . . . H15A H 0.3543 0.9157 0.3177 0.073 Uiso 1 1 calc R . . H15B H 0.2405 0.8091 0.3259 0.073 Uiso 1 1 calc R . . H15C H 0.3978 0.7855 0.3058 0.073 Uiso 1 1 calc R . . C20 C 0.6433(11) 0.5737(8) 0.3242(3) 0.029(2) Uani 1 1 d . . . C21 C 0.7349(12) 0.6740(9) 0.3290(3) 0.036(3) Uani 1 1 d . . . H21 H 0.7271 0.7185 0.3502 0.043 Uiso 1 1 calc R . . C22 C 0.8356(12) 0.7095(9) 0.3038(3) 0.037(3) Uani 1 1 d . . . H22 H 0.8958 0.7785 0.3072 0.045 Uiso 1 1 calc R . . C23 C 0.8480(12) 0.6432(10) 0.2735(3) 0.037(3) Uani 1 1 d . . . C24 C 0.7590(13) 0.5444(10) 0.2677(3) 0.044(3) Uani 1 1 d . . . H24 H 0.7675 0.5012 0.2462 0.053 Uiso 1 1 calc R . . C25 C 0.6581(13) 0.5083(9) 0.2927(3) 0.036(3) Uani 1 1 d . . . H25 H 0.5983 0.4393 0.2889 0.043 Uiso 1 1 calc R . . C26 C 0.3979(11) 0.4157(8) 0.3403(3) 0.029(2) Uani 1 1 d . . . C27 C 0.9634(14) 0.6774(11) 0.2462(3) 0.048(3) Uani 1 1 d . . . C28 C 0.3908(12) 0.2986(9) 0.3516(3) 0.033(2) Uani 1 1 d . . . H28 H 0.4592 0.2714 0.3702 0.040 Uiso 1 1 calc R . . C29 C 0.2842(12) 0.2231(9) 0.3356(3) 0.037(3) Uani 1 1 d . . . H29 H 0.2786 0.1441 0.3434 0.044 Uiso 1 1 calc R . . C30 C 0.1858(12) 0.2622(9) 0.3083(3) 0.037(3) Uani 1 1 d . . . C31 C 0.1914(12) 0.3761(10) 0.2970(3) 0.037(3) Uani 1 1 d . . . H31 H 0.1217 0.4026 0.2785 0.045 Uiso 1 1 calc R . . C32 C 0.2989(12) 0.4524(9) 0.3125(3) 0.034(2) Uani 1 1 d . . . H32 H 0.3051 0.5307 0.3040 0.041 Uiso 1 1 calc R . . C33 C 0.0670(15) 0.1802(12) 0.2916(4) 0.051(3) Uani 1 1 d . . . C34 C 0.6780(11) 0.4365(8) 0.3864(3) 0.025(2) Uani 1 1 d . . . C35 C 0.8132(14) 0.4058(11) 0.3712(3) 0.056(4) Uani 1 1 d . . . H35 H 0.8275 0.4247 0.3470 0.067 Uiso 1 1 calc R . . C36 C 0.9324(15) 0.3467(12) 0.3907(3) 0.059(4) Uani 1 1 d . . . H36 H 1.0261 0.3254 0.3799 0.070 Uiso 1 1 calc R . . C37 C 0.9084(12) 0.3205(9) 0.4261(3) 0.031(2) Uani 1 1 d . . . C38 C 0.7732(15) 0.3516(11) 0.4409(3) 0.058(4) Uani 1 1 d . . . H38 H 0.7592 0.3352 0.4653 0.070 Uiso 1 1 calc R . . C39 C 0.6544(14) 0.4071(11) 0.4212(3) 0.049(3) Uani 1 1 d . . . H39 H 0.5585 0.4243 0.4316 0.059 Uiso 1 1 calc R . . C40 C 1.0360(15) 0.2582(13) 0.4465(3) 0.054(3) Uani 1 1 d . . . O1 O 0.7668(11) 0.9730(8) 0.4914(2) 0.067(3) Uani 1 1 d . . . O2 O 0.9625(11) 0.6697(9) 0.4339(3) 0.072(3) Uani 1 1 d . . . O3 O 0.5344(10) 0.6369(7) 0.5023(2) 0.052(2) Uani 1 1 d . . . O4 O 0.0873(9) 0.6236(8) 0.3575(2) 0.063(3) Uani 1 1 d . . . O6 O 0.2810(10) 0.5227(7) 0.4533(2) 0.050(2) Uani 1 1 d . . . O9 O 0.4555(10) 1.1355(8) 0.4489(3) 0.070(3) Uani 1 1 d . . . O8 O 0.2262(10) 0.7913(7) 0.4765(2) 0.051(2) Uani 1 1 d . . . O7 O 0.0791(12) 0.9760(11) 0.3753(3) 0.097(4) Uani 1 1 d . . . O10 O 0.5781(10) 0.9903(7) 0.3439(2) 0.053(2) Uani 1 1 d . . . F1 F 1.0661(12) 0.5973(9) 0.2403(3) 0.132(5) Uani 1 1 d . . . F2 F 1.0410(10) 0.7762(9) 0.2549(2) 0.099(3) Uani 1 1 d . . . F3 F 0.9016(9) 0.7031(7) 0.21496(18) 0.070(2) Uani 1 1 d . . . F4 F 0.0521(13) 0.1956(10) 0.2579(2) 0.131(5) Uani 1 1 d . . . F5 F 0.1001(12) 0.0715(8) 0.2947(3) 0.129(5) Uani 1 1 d . . . F6 F -0.0652(11) 0.1931(11) 0.3039(3) 0.139(5) Uani 1 1 d . . . F7 F 1.0002(10) 0.1487(7) 0.4529(3) 0.105(4) Uani 1 1 d . . . F8 F 1.0618(10) 0.3045(7) 0.4786(2) 0.081(3) Uani 1 1 d . . . F9 F 1.1697(10) 0.2628(9) 0.4319(2) 0.098(3) Uani 1 1 d . . . P1 P 0.5293(3) 0.5228(2) 0.36107(7) 0.0261(6) Uani 1 1 d . . . Os1 Os 0.64654(5) 0.78552(4) 0.439803(11) 0.03174(12) Uani 1 1 d . . . Os2 Os 0.40567(5) 0.66826(3) 0.391818(10) 0.02766(11) Uani 1 1 d . . . Os3 Os 0.37961(5) 0.90251(4) 0.412984(12) 0.03289(12) Uani 1 1 d . . . H1 H 0.6031 0.6555 0.4120 0.050 Uiso 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 C1 0.054(8) 0.055(8) 0.028(6) -0.003(6) 0.004(5) -0.003(6) C2 0.044(8) 0.065(9) 0.050(8) 0.002(6) -0.009(7) 0.001(7) C3 0.042(7) 0.041(7) 0.035(6) -0.007(5) -0.011(6) 0.009(5) C4 0.030(6) 0.044(7) 0.050(7) -0.004(5) 0.006(6) 0.005(5) C6 0.029(6) 0.041(7) 0.044(7) 0.005(5) 0.008(5) 0.010(5) C9 0.055(9) 0.047(8) 0.064(8) -0.006(7) 0.034(7) 0.015(6) C8 0.047(7) 0.025(6) 0.045(7) -0.009(5) 0.011(6) 0.001(5) C7 0.029(7) 0.086(10) 0.059(8) 0.017(7) 0.015(6) 0.020(7) C12 0.034(6) 0.030(6) 0.039(6) 0.001(5) 0.017(5) 0.001(5) C13 0.063(8) 0.023(5) 0.026(6) 0.003(4) -0.015(6) -0.001(5) C14 0.029(6) 0.061(8) 0.029(6) 0.004(5) 0.005(5) 0.015(5) C11 0.032(7) 0.049(7) 0.065(9) 0.001(6) 0.014(6) -0.013(5) C10 0.044(8) 0.043(7) 0.067(9) 0.016(6) 0.017(6) -0.007(6) C15 0.053(8) 0.058(8) 0.034(6) 0.002(6) -0.005(6) 0.000(6) C20 0.017(5) 0.035(6) 0.034(6) 0.002(4) -0.002(4) 0.011(4) C21 0.034(7) 0.042(6) 0.032(6) -0.007(5) 0.002(5) 0.003(5) C22 0.027(6) 0.040(6) 0.045(7) 0.012(5) 0.010(5) -0.001(5) C23 0.021(6) 0.053(7) 0.036(6) 0.022(5) 0.005(5) 0.006(5) C24 0.044(8) 0.053(7) 0.035(6) 0.000(6) -0.001(5) 0.006(6) C25 0.046(7) 0.036(6) 0.026(6) 0.005(4) 0.001(5) -0.009(5) C26 0.021(5) 0.032(6) 0.036(6) 0.000(4) 0.006(4) -0.001(4) C27 0.026(7) 0.067(9) 0.053(8) 0.015(6) 0.014(6) 0.009(6) C28 0.026(6) 0.043(6) 0.031(6) 0.011(5) 0.000(5) -0.003(5) C29 0.039(6) 0.037(6) 0.035(6) -0.003(5) 0.008(5) -0.012(5) C30 0.023(6) 0.042(7) 0.046(7) -0.006(5) 0.005(5) -0.006(5) C31 0.029(6) 0.051(7) 0.031(6) -0.004(5) -0.004(5) 0.003(5) C32 0.037(6) 0.041(6) 0.025(5) -0.001(5) 0.001(5) 0.005(5) C33 0.039(8) 0.052(8) 0.061(9) -0.012(6) -0.012(7) -0.004(6) C34 0.025(5) 0.023(5) 0.027(5) 0.001(4) 0.005(4) 0.002(4) C35 0.041(8) 0.094(10) 0.032(6) 0.019(6) 0.010(5) 0.023(7) C36 0.042(8) 0.088(10) 0.047(8) 0.014(7) 0.005(6) 0.033(7) C37 0.025(6) 0.035(6) 0.035(6) 0.003(5) 0.000(5) 0.004(4) C38 0.070(10) 0.070(9) 0.035(7) 0.017(6) 0.010(6) 0.037(7) C39 0.040(7) 0.077(9) 0.032(6) 0.016(6) 0.018(5) 0.019(6) C40 0.036(7) 0.078(10) 0.046(8) 0.012(7) -0.007(6) 0.012(7) O1 0.083(7) 0.067(6) 0.051(6) -0.021(5) 0.004(5) -0.012(5) O2 0.043(6) 0.108(8) 0.065(6) -0.010(6) -0.003(5) 0.024(5) O3 0.063(6) 0.058(5) 0.034(5) 0.017(4) 0.004(4) -0.003(4) O4 0.035(5) 0.079(6) 0.074(7) -0.007(5) -0.021(5) 0.001(4) O6 0.045(5) 0.058(5) 0.047(5) 0.013(4) 0.013(4) -0.001(4) O9 0.056(6) 0.049(5) 0.108(8) -0.028(6) 0.039(6) -0.006(5) O8 0.060(6) 0.053(5) 0.043(5) -0.002(4) 0.031(4) -0.001(4) O7 0.054(7) 0.168(11) 0.069(7) 0.022(7) 0.009(6) 0.043(7) O10 0.054(6) 0.055(5) 0.050(5) 0.018(4) 0.012(4) -0.002(4) F1 0.098(8) 0.136(9) 0.169(10) 0.099(8) 0.108(7) 0.079(7) F2 0.080(7) 0.162(9) 0.056(5) 0.003(6) 0.024(5) -0.066(6) F3 0.066(5) 0.105(6) 0.040(4) 0.024(4) 0.012(4) -0.017(4) F4 0.163(11) 0.181(10) 0.045(5) -0.002(6) -0.024(6) -0.127(9) F5 0.120(9) 0.069(7) 0.192(12) -0.027(7) -0.067(9) -0.022(6) F6 0.048(6) 0.206(12) 0.167(11) -0.124(9) 0.051(6) -0.068(7) F7 0.098(7) 0.052(5) 0.159(9) 0.031(5) -0.078(7) -0.006(5) F8 0.078(6) 0.096(6) 0.067(6) 0.002(5) -0.038(5) 0.013(5) F9 0.045(5) 0.169(9) 0.081(6) 0.041(6) 0.002(5) 0.046(6) P1 0.0252(14) 0.0285(14) 0.0246(13) 0.0010(10) 0.0017(11) -0.0007(10) Os1 0.0290(2) 0.0377(2) 0.0285(2) -0.00335(18) 0.00128(17) 0.00030(18) Os2 0.0234(2) 0.0307(2) 0.0289(2) -0.00094(17) 0.00094(16) 0.00202(16) Os3 0.0296(2) 0.0320(2) 0.0377(2) 0.00157(18) 0.00966(18) 0.00466(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.169(12) . ? C1 Os1 1.877(12) . ? C2 O2 1.129(14) . ? C2 Os1 1.916(14) . ? C3 O3 1.107(14) . ? C3 Os1 1.977(13) . ? C4 O4 1.159(12) . ? C4 Os2 1.875(11) . ? C6 O6 1.144(13) . ? C6 Os2 1.936(12) . ? C9 O9 1.134(14) . ? C9 Os3 1.913(14) . ? C8 O8 1.173(13) . ? C8 Os3 1.881(12) . ? C7 O7 1.121(13) . ? C7 Os3 1.905(12) . ? C12 C13 1.456(13) . ? C12 C11 1.491(14) . ? C12 Os1 2.047(10) . ? C12 Os3 2.363(11) . ? C13 O10 1.395(12) . ? C13 C14 1.407(15) . ? C13 Os3 2.296(12) . ? C14 C15 1.508(13) . ? C14 Os2 2.076(11) . ? C14 Os3 2.319(11) . ? C11 C10 1.311(16) . ? C11 H11 0.9500 . ? C10 O10 1.379(14) . ? C10 H10 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C20 C21 1.399(14) . ? C20 C25 1.410(14) . ? C20 P1 1.826(11) . ? C21 C22 1.370(14) . ? C21 H21 0.9500 . ? C22 C23 1.378(16) . ? C22 H22 0.9500 . ? C23 C24 1.376(15) . ? C23 C27 1.506(15) . ? C24 C25 1.370(15) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C32 1.389(13) . ? C26 C28 1.405(13) . ? C26 P1 1.824(9) . ? C27 F1 1.299(14) . ? C27 F3 1.307(13) . ? C27 F2 1.345(14) . ? C28 C29 1.381(13) . ? C28 H28 0.9500 . ? C29 C30 1.380(14) . ? C29 H29 0.9500 . ? C30 C31 1.370(15) . ? C30 C33 1.507(15) . ? C31 C32 1.386(14) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 F6 1.255(15) . ? C33 F5 1.278(14) . ? C33 F4 1.283(15) . ? C34 C35 1.363(15) . ? C34 C39 1.373(14) . ? C34 P1 1.852(9) . ? C35 C36 1.411(15) . ? C35 H35 0.9500 . ? C36 C37 1.390(16) . ? C36 H36 0.9500 . ? C37 C38 1.357(15) . ? C37 C40 1.498(14) . ? C38 C39 1.394(15) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 F9 1.298(15) . ? C40 F7 1.311(15) . ? C40 F8 1.327(15) . ? P1 Os2 2.308(3) . ? Os1 Os3 2.8153(6) . ? Os1 Os2 3.0137(5) . ? Os1 H1 1.8455 . ? Os2 Os3 2.8016(6) . ? Os2 H1 1.8444 . ? 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 O1 C1 Os1 177.9(11) . . ? O2 C2 Os1 177.7(12) . . ? O3 C3 Os1 178.4(10) . . ? O4 C4 Os2 179.6(13) . . ? O6 C6 Os2 174.0(10) . . ? O9 C9 Os3 175.9(12) . . ? O8 C8 Os3 178.4(10) . . ? O7 C7 Os3 178.8(14) . . ? C13 C12 C11 101.6(9) . . ? C13 C12 Os1 124.4(7) . . ? C11 C12 Os1 133.9(8) . . ? C13 C12 Os3 69.3(6) . . ? C11 C12 Os3 121.6(7) . . ? Os1 C12 Os3 79.0(4) . . ? O10 C13 C14 122.3(8) . . ? O10 C13 C12 111.4(9) . . ? C14 C13 C12 126.2(9) . . ? O10 C13 Os3 126.5(8) . . ? C14 C13 Os3 73.1(7) . . ? C12 C13 Os3 74.3(6) . . ? C13 C14 C15 113.2(10) . . ? C13 C14 Os2 121.9(7) . . ? C15 C14 Os2 124.7(8) . . ? C13 C14 Os3 71.4(7) . . ? C15 C14 Os3 126.5(8) . . ? Os2 C14 Os3 79.0(4) . . ? C10 C11 C12 107.3(10) . . ? C10 C11 H11 126.3 . . ? C12 C11 H11 126.3 . . ? C11 C10 O10 115.4(10) . . ? C11 C10 H10 122.3 . . ? O10 C10 H10 122.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C20 C25 118.2(10) . . ? C21 C20 P1 118.7(8) . . ? C25 C20 P1 122.6(8) . . ? C22 C21 C20 121.5(10) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 118.8(10) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 121.4(11) . . ? C24 C23 C27 119.0(11) . . ? C22 C23 C27 119.6(11) . . ? C25 C24 C23 120.2(11) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C20 119.9(10) . . ? C24 C25 H25 120.0 . . ? C20 C25 H25 120.0 . . ? C32 C26 C28 118.9(9) . . ? C32 C26 P1 118.3(7) . . ? C28 C26 P1 122.8(7) . . ? F1 C27 F3 105.1(12) . . ? F1 C27 F2 107.2(11) . . ? F3 C27 F2 102.3(10) . . ? F1 C27 C23 114.0(11) . . ? F3 C27 C23 114.4(9) . . ? F2 C27 C23 112.9(11) . . ? C29 C28 C26 119.8(9) . . ? C29 C28 H28 120.1 . . ? C26 C28 H28 120.1 . . ? C30 C29 C28 120.2(10) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 120.7(9) . . ? C31 C30 C33 119.3(10) . . ? C29 C30 C33 119.9(10) . . ? C30 C31 C32 119.8(9) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C31 C32 C26 120.6(10) . . ? C31 C32 H32 119.7 . . ? C26 C32 H32 119.7 . . ? F6 C33 F5 106.4(14) . . ? F6 C33 F4 106.8(12) . . ? F5 C33 F4 103.6(12) . . ? F6 C33 C30 112.8(11) . . ? F5 C33 C30 114.8(10) . . ? F4 C33 C30 111.7(12) . . ? C35 C34 C39 119.7(10) . . ? C35 C34 P1 120.6(8) . . ? C39 C34 P1 119.7(8) . . ? C34 C35 C36 121.6(11) . . ? C34 C35 H35 119.2 . . ? C36 C35 H35 119.2 . . ? C37 C36 C35 117.9(12) . . ? C37 C36 H36 121.0 . . ? C35 C36 H36 121.0 . . ? C38 C37 C36 119.8(10) . . ? C38 C37 C40 122.8(11) . . ? C36 C37 C40 117.4(11) . . ? C37 C38 C39 121.8(11) . . ? C37 C38 H38 119.1 . . ? C39 C38 H38 119.1 . . ? C34 C39 C38 119.0(11) . . ? C34 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? F9 C40 F7 109.6(12) . . ? F9 C40 F8 104.4(11) . . ? F7 C40 F8 104.2(11) . . ? F9 C40 C37 114.3(11) . . ? F7 C40 C37 111.9(10) . . ? F8 C40 C37 111.7(11) . . ? C10 O10 C13 104.0(8) . . ? C26 P1 C20 103.4(5) . . ? C26 P1 C34 105.7(4) . . ? C20 P1 C34 100.2(4) . . ? C26 P1 Os2 114.0(3) . . ? C20 P1 Os2 115.1(3) . . ? C34 P1 Os2 116.7(3) . . ? C1 Os1 C2 94.0(5) . . ? C1 Os1 C3 91.0(5) . . ? C2 Os1 C3 96.4(5) . . ? C1 Os1 C12 89.3(4) . . ? C2 Os1 C12 103.3(5) . . ? C3 Os1 C12 160.2(4) . . ? C1 Os1 Os3 97.9(4) . . ? C2 Os1 Os3 155.3(4) . . ? C3 Os1 Os3 104.9(3) . . ? C12 Os1 Os3 55.5(3) . . ? C1 Os1 Os2 154.0(4) . . ? C2 Os1 Os2 111.9(4) . . ? C3 Os1 Os2 88.5(3) . . ? C12 Os1 Os2 82.7(3) . . ? Os3 Os1 Os2 57.332(13) . . ? C1 Os1 H1 170.1 . . ? C2 Os1 H1 77.4 . . ? C3 Os1 H1 85.2 . . ? C12 Os1 H1 97.4 . . ? Os3 Os1 H1 91.9 . . ? Os2 Os1 H1 35.2 . . ? C4 Os2 C6 85.4(5) . . ? C4 Os2 C14 90.4(5) . . ? C6 Os2 C14 159.6(4) . . ? C4 Os2 P1 95.4(3) . . ? C6 Os2 P1 97.9(3) . . ? C14 Os2 P1 102.3(3) . . ? C4 Os2 Os3 101.5(3) . . ? C6 Os2 Os3 107.0(3) . . ? C14 Os2 Os3 54.3(3) . . ? P1 Os2 Os3 150.79(7) . . ? C4 Os2 Os1 157.2(3) . . ? C6 Os2 Os1 91.7(3) . . ? C14 Os2 Os1 84.4(3) . . ? P1 Os2 Os1 107.39(6) . . ? Os3 Os2 Os1 57.771(13) . . ? C4 Os2 H1 165.8 . . ? C6 Os2 H1 87.7 . . ? C14 Os2 H1 100.3 . . ? P1 Os2 H1 73.3 . . ? Os3 Os2 H1 92.4 . . ? Os1 Os2 H1 35.3 . . ? C8 Os3 C7 95.6(5) . . ? C8 Os3 C9 96.6(5) . . ? C7 Os3 C9 95.6(6) . . ? C8 Os3 C13 151.7(4) . . ? C7 Os3 C13 102.3(5) . . ? C9 Os3 C13 103.2(5) . . ? C8 Os3 C14 126.8(4) . . ? C7 Os3 C14 85.4(5) . . ? C9 Os3 C14 136.4(5) . . ? C13 Os3 C14 35.5(4) . . ? C8 Os3 C12 128.4(4) . . ? C7 Os3 C12 135.7(5) . . ? C9 Os3 C12 84.6(4) . . ? C13 Os3 C12 36.4(3) . . ? C14 Os3 C12 66.1(4) . . ? C8 Os3 Os2 81.8(3) . . ? C7 Os3 Os2 102.4(4) . . ? C9 Os3 Os2 161.9(4) . . ? C13 Os3 Os2 73.1(2) . . ? C14 Os3 Os2 46.7(3) . . ? C12 Os3 Os2 82.5(2) . . ? C8 Os3 Os1 83.5(3) . . ? C7 Os3 Os1 167.3(4) . . ? C9 Os3 Os1 97.0(4) . . ? C13 Os3 Os1 74.2(2) . . ? C14 Os3 Os1 85.1(2) . . ? C12 Os3 Os1 45.5(2) . . ? Os2 Os3 Os1 64.897(14) . . ? 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 C11 C12 C13 O10 4.0(12) . . . . ? Os1 C12 C13 O10 -176.9(7) . . . . ? Os3 C12 C13 O10 123.6(9) . . . . ? C11 C12 C13 C14 -174.2(11) . . . . ? Os1 C12 C13 C14 4.9(17) . . . . ? Os3 C12 C13 C14 -54.6(11) . . . . ? C11 C12 C13 Os3 -119.6(8) . . . . ? Os1 C12 C13 Os3 59.6(7) . . . . ? O10 C13 C14 C15 -0.3(16) . . . . ? C12 C13 C14 C15 177.7(11) . . . . ? Os3 C13 C14 C15 122.6(9) . . . . ? O10 C13 C14 Os2 173.6(8) . . . . ? C12 C13 C14 Os2 -8.3(17) . . . . ? Os3 C13 C14 Os2 -63.5(7) . . . . ? O10 C13 C14 Os3 -122.9(11) . . . . ? C12 C13 C14 Os3 55.1(11) . . . . ? C13 C12 C11 C10 -5.0(13) . . . . ? Os1 C12 C11 C10 176.0(9) . . . . ? Os3 C12 C11 C10 -77.7(12) . . . . ? C12 C11 C10 O10 4.6(15) . . . . ? C25 C20 C21 C22 0.7(14) . . . . ? P1 C20 C21 C22 172.9(7) . . . . ? C20 C21 C22 C23 -1.1(15) . . . . ? C21 C22 C23 C24 1.6(15) . . . . ? C21 C22 C23 C27 -177.1(9) . . . . ? C22 C23 C24 C25 -1.7(15) . . . . ? C27 C23 C24 C25 177.1(9) . . . . ? C23 C24 C25 C20 1.2(15) . . . . ? C21 C20 C25 C24 -0.7(14) . . . . ? P1 C20 C25 C24 -172.7(8) . . . . ? C24 C23 C27 F1 -58.2(15) . . . . ? C22 C23 C27 F1 120.5(13) . . . . ? C24 C23 C27 F3 62.8(14) . . . . ? C22 C23 C27 F3 -118.5(12) . . . . ? C24 C23 C27 F2 179.2(10) . . . . ? C22 C23 C27 F2 -2.1(14) . . . . ? C32 C26 C28 C29 -1.4(16) . . . . ? P1 C26 C28 C29 177.4(9) . . . . ? C26 C28 C29 C30 0.6(17) . . . . ? C28 C29 C30 C31 -0.5(17) . . . . ? C28 C29 C30 C33 -178.5(11) . . . . ? C29 C30 C31 C32 1.3(17) . . . . ? C33 C30 C31 C32 179.3(11) . . . . ? C30 C31 C32 C26 -2.1(17) . . . . ? C28 C26 C32 C31 2.2(16) . . . . ? P1 C26 C32 C31 -176.6(8) . . . . ? C31 C30 C33 F6 -79.8(17) . . . . ? C29 C30 C33 F6 98.2(15) . . . . ? C31 C30 C33 F5 158.0(13) . . . . ? C29 C30 C33 F5 -24.0(19) . . . . ? C31 C30 C33 F4 40.5(17) . . . . ? C29 C30 C33 F4 -141.5(13) . . . . ? C39 C34 C35 C36 -1.6(19) . . . . ? P1 C34 C35 C36 175.9(10) . . . . ? C34 C35 C36 C37 0(2) . . . . ? C35 C36 C37 C38 0.2(19) . . . . ? C35 C36 C37 C40 -179.7(12) . . . . ? C36 C37 C38 C39 2(2) . . . . ? C40 C37 C38 C39 -178.4(12) . . . . ? C35 C34 C39 C38 3.4(18) . . . . ? P1 C34 C39 C38 -174.1(9) . . . . ? C37 C38 C39 C34 -3(2) . . . . ? C38 C37 C40 F9 -162.5(12) . . . . ? C36 C37 C40 F9 17.4(17) . . . . ? C38 C37 C40 F7 72.1(16) . . . . ? C36 C37 C40 F7 -108.0(14) . . . . ? C38 C37 C40 F8 -44.3(17) . . . . ? C36 C37 C40 F8 135.6(12) . . . . ? C11 C10 O10 C13 -2.0(15) . . . . ? C14 C13 O10 C10 176.7(11) . . . . ? C12 C13 O10 C10 -1.6(13) . . . . ? Os3 C13 O10 C10 84.3(10) . . . . ? C32 C26 P1 C20 -58.8(9) . . . . ? C28 C26 P1 C20 122.5(9) . . . . ? C32 C26 P1 C34 -163.6(8) . . . . ? C28 C26 P1 C34 17.6(10) . . . . ? C32 C26 P1 Os2 66.9(9) . . . . ? C28 C26 P1 Os2 -111.9(9) . . . . ? C21 C20 P1 C26 167.2(7) . . . . ? C25 C20 P1 C26 -20.9(9) . . . . ? C21 C20 P1 C34 -83.8(8) . . . . ? C25 C20 P1 C34 88.1(8) . . . . ? C21 C20 P1 Os2 42.2(8) . . . . ? C25 C20 P1 Os2 -145.9(7) . . . . ? C35 C34 P1 C26 92.6(10) . . . . ? C39 C34 P1 C26 -89.9(9) . . . . ? C35 C34 P1 C20 -14.5(10) . . . . ? C39 C34 P1 C20 162.9(9) . . . . ? C35 C34 P1 Os2 -139.5(8) . . . . ? C39 C34 P1 Os2 38.0(10) . . . . ? O1 C1 Os1 C2 6(29) . . . . ? O1 C1 Os1 C3 102(29) . . . . ? O1 C1 Os1 C12 -98(29) . . . . ? O1 C1 Os1 Os3 -153(29) . . . . ? O1 C1 Os1 Os2 -169(100) . . . . ? O2 C2 Os1 C1 -137(31) . . . . ? O2 C2 Os1 C3 131(31) . . . . ? O2 C2 Os1 C12 -47(31) . . . . ? O2 C2 Os1 Os3 -18(31) . . . . ? O2 C2 Os1 Os2 40(31) . . . . ? O3 C3 Os1 C1 4(39) . . . . ? O3 C3 Os1 C2 98(39) . . . . ? O3 C3 Os1 C12 -86(39) . . . . ? O3 C3 Os1 Os3 -94(39) . . . . ? O3 C3 Os1 Os2 -150(39) . . . . ? C13 C12 Os1 C1 -155.3(10) . . . . ? C11 C12 Os1 C1 23.5(12) . . . . ? Os3 C12 Os1 C1 -100.0(4) . . . . ? C13 C12 Os1 C2 110.7(10) . . . . ? C11 C12 Os1 C2 -70.5(12) . . . . ? Os3 C12 Os1 C2 166.0(4) . . . . ? C13 C12 Os1 C3 -64.4(16) . . . . ? C11 C12 Os1 C3 114.4(14) . . . . ? Os3 C12 Os1 C3 -9.1(13) . . . . ? C13 C12 Os1 Os3 -55.3(8) . . . . ? C11 C12 Os1 Os3 123.6(12) . . . . ? C13 C12 Os1 Os2 -0.1(9) . . . . ? C11 C12 Os1 Os2 178.7(11) . . . . ? Os3 C12 Os1 Os2 55.12(18) . . . . ? O4 C4 Os2 C6 -5(100) . . . . ? O4 C4 Os2 C14 -165(100) . . . . ? O4 C4 Os2 P1 93(100) . . . . ? O4 C4 Os2 Os3 -111(100) . . . . ? O4 C4 Os2 Os1 -88(100) . . . . ? O6 C6 Os2 C4 -50(10) . . . . ? O6 C6 Os2 C14 29(10) . . . . ? O6 C6 Os2 P1 -145(10) . . . . ? O6 C6 Os2 Os3 51(10) . . . . ? O6 C6 Os2 Os1 107(10) . . . . ? C13 C14 Os2 C4 163.7(10) . . . . ? C15 C14 Os2 C4 -23.1(10) . . . . ? Os3 C14 Os2 C4 103.9(4) . . . . ? C13 C14 Os2 C6 85.8(15) . . . . ? C15 C14 Os2 C6 -100.9(15) . . . . ? Os3 C14 Os2 C6 26.1(13) . . . . ? C13 C14 Os2 P1 -100.8(9) . . . . ? C15 C14 Os2 P1 72.5(9) . . . . ? Os3 C14 Os2 P1 -160.49(16) . . . . ? C13 C14 Os2 Os3 59.7(9) . . . . ? C15 C14 Os2 Os3 -127.0(10) . . . . ? C13 C14 Os2 Os1 5.9(9) . . . . ? C15 C14 Os2 Os1 179.1(10) . . . . ? Os3 C14 Os2 Os1 -53.87(19) . . . . ? C26 P1 Os2 C4 -16.8(5) . . . . ? C20 P1 Os2 C4 102.4(5) . . . . ? C34 P1 Os2 C4 -140.6(5) . . . . ? C26 P1 Os2 C6 69.3(5) . . . . ? C20 P1 Os2 C6 -171.5(4) . . . . ? C34 P1 Os2 C6 -54.5(5) . . . . ? C26 P1 Os2 C14 -108.4(5) . . . . ? C20 P1 Os2 C14 10.8(4) . . . . ? C34 P1 Os2 C14 127.9(5) . . . . ? C26 P1 Os2 Os3 -142.2(3) . . . . ? C20 P1 Os2 Os3 -23.0(4) . . . . ? C34 P1 Os2 Os3 94.1(4) . . . . ? C26 P1 Os2 Os1 163.6(4) . . . . ? C20 P1 Os2 Os1 -77.1(3) . . . . ? C34 P1 Os2 Os1 39.9(4) . . . . ? C1 Os1 Os2 C4 -7.0(13) . . . . ? C2 Os1 Os2 C4 178.5(10) . . . . ? C3 Os1 Os2 C4 82.1(10) . . . . ? C12 Os1 Os2 C4 -80.1(10) . . . . ? Os3 Os1 Os2 C4 -26.7(9) . . . . ? C1 Os1 Os2 C6 -89.4(9) . . . . ? C2 Os1 Os2 C6 96.2(5) . . . . ? C3 Os1 Os2 C6 -0.2(5) . . . . ? C12 Os1 Os2 C6 -162.4(4) . . . . ? Os3 Os1 Os2 C6 -109.0(3) . . . . ? C1 Os1 Os2 C14 70.5(9) . . . . ? C2 Os1 Os2 C14 -103.9(5) . . . . ? C3 Os1 Os2 C14 159.7(4) . . . . ? C12 Os1 Os2 C14 -2.5(4) . . . . ? Os3 Os1 Os2 C14 50.9(3) . . . . ? C1 Os1 Os2 P1 171.8(8) . . . . ? C2 Os1 Os2 P1 -2.7(4) . . . . ? C3 Os1 Os2 P1 -99.1(3) . . . . ? C12 Os1 Os2 P1 98.7(3) . . . . ? Os3 Os1 Os2 P1 152.11(7) . . . . ? C1 Os1 Os2 Os3 19.7(8) . . . . ? C2 Os1 Os2 Os3 -154.8(4) . . . . ? C3 Os1 Os2 Os3 108.8(3) . . . . ? C12 Os1 Os2 Os3 -53.4(3) . . . . ? O8 C8 Os3 C7 -54(37) . . . . ? O8 C8 Os3 C9 42(37) . . . . ? O8 C8 Os3 C13 176(100) . . . . ? O8 C8 Os3 C14 -143(37) . . . . ? O8 C8 Os3 C12 130(37) . . . . ? O8 C8 Os3 Os2 -156(37) . . . . ? O8 C8 Os3 Os1 139(37) . . . . ? O7 C7 Os3 C8 -99(73) . . . . ? O7 C7 Os3 C9 163(100) . . . . ? O7 C7 Os3 C13 59(73) . . . . ? O7 C7 Os3 C14 27(73) . . . . ? O7 C7 Os3 C12 75(73) . . . . ? O7 C7 Os3 Os2 -17(73) . . . . ? O7 C7 Os3 Os1 -14(74) . . . . ? O9 C9 Os3 C8 91(17) . . . . ? O9 C9 Os3 C7 -173(100) . . . . ? O9 C9 Os3 C13 -69(17) . . . . ? O9 C9 Os3 C14 -84(17) . . . . ? O9 C9 Os3 C12 -37(17) . . . . ? O9 C9 Os3 Os2 7(18) . . . . ? O9 C9 Os3 Os1 6(17) . . . . ? O10 C13 Os3 C8 -177.3(9) . . . . ? C14 C13 Os3 C8 64.6(10) . . . . ? C12 C13 Os3 C8 -71.9(10) . . . . ? O10 C13 Os3 C7 54.7(9) . . . . ? C14 C13 Os3 C7 -63.4(7) . . . . ? C12 C13 Os3 C7 160.1(7) . . . . ? O10 C13 Os3 C9 -44.1(9) . . . . ? C14 C13 Os3 C9 -162.2(6) . . . . ? C12 C13 Os3 C9 61.2(7) . . . . ? O10 C13 Os3 C14 118.1(11) . . . . ? C12 C13 Os3 C14 -136.6(8) . . . . ? O10 C13 Os3 C12 -105.3(10) . . . . ? C14 C13 Os3 C12 136.6(8) . . . . ? O10 C13 Os3 Os2 154.2(8) . . . . ? C14 C13 Os3 Os2 36.1(5) . . . . ? C12 C13 Os3 Os2 -100.5(5) . . . . ? O10 C13 Os3 Os1 -137.8(8) . . . . ? C14 C13 Os3 Os1 104.1(6) . . . . ? C12 C13 Os3 Os1 -32.5(5) . . . . ? C13 C14 Os3 C8 -147.6(6) . . . . ? C15 C14 Os3 C8 106.9(11) . . . . ? Os2 C14 Os3 C8 -18.4(6) . . . . ? C13 C14 Os3 C7 118.8(7) . . . . ? C15 C14 Os3 C7 13.3(11) . . . . ? Os2 C14 Os3 C7 -111.9(5) . . . . ? C13 C14 Os3 C9 25.5(9) . . . . ? C15 C14 Os3 C9 -80.0(12) . . . . ? Os2 C14 Os3 C9 154.8(6) . . . . ? C15 C14 Os3 C13 -105.5(12) . . . . ? Os2 C14 Os3 C13 129.3(7) . . . . ? C13 C14 Os3 C12 -26.5(5) . . . . ? C15 C14 Os3 C12 -132.0(11) . . . . ? Os2 C14 Os3 C12 102.8(4) . . . . ? C13 C14 Os3 Os2 -129.3(7) . . . . ? C15 C14 Os3 Os2 125.2(11) . . . . ? C13 C14 Os3 Os1 -69.5(5) . . . . ? C15 C14 Os3 Os1 -175.0(10) . . . . ? Os2 C14 Os3 Os1 59.7(2) . . . . ? C13 C12 Os3 C8 144.8(6) . . . . ? C11 C12 Os3 C8 -124.0(9) . . . . ? Os1 C12 Os3 C8 11.3(6) . . . . ? C13 C12 Os3 C7 -28.5(9) . . . . ? C11 C12 Os3 C7 62.7(12) . . . . ? Os1 C12 Os3 C7 -162.1(6) . . . . ? C13 C12 Os3 C9 -121.0(7) . . . . ? C11 C12 Os3 C9 -29.8(10) . . . . ? Os1 C12 Os3 C9 105.4(5) . . . . ? C11 C12 Os3 C13 91.2(10) . . . . ? Os1 C12 Os3 C13 -133.6(7) . . . . ? C13 C12 Os3 C14 25.9(5) . . . . ? C11 C12 Os3 C14 117.1(10) . . . . ? Os1 C12 Os3 C14 -107.7(4) . . . . ? C13 C12 Os3 Os2 71.6(5) . . . . ? C11 C12 Os3 Os2 162.8(9) . . . . ? Os1 C12 Os3 Os2 -62.0(2) . . . . ? C13 C12 Os3 Os1 133.6(7) . . . . ? C11 C12 Os3 Os1 -135.2(10) . . . . ? C4 Os2 Os3 C8 83.2(5) . . . . ? C6 Os2 Os3 C8 -5.5(5) . . . . ? C14 Os2 Os3 C8 165.2(5) . . . . ? P1 Os2 Os3 C8 -152.8(4) . . . . ? Os1 Os2 Os3 C8 -86.6(3) . . . . ? C4 Os2 Os3 C7 -10.9(6) . . . . ? C6 Os2 Os3 C7 -99.5(5) . . . . ? C14 Os2 Os3 C7 71.2(5) . . . . ? P1 Os2 Os3 C7 113.2(4) . . . . ? Os1 Os2 Os3 C7 179.4(4) . . . . ? C4 Os2 Os3 C9 169.4(13) . . . . ? C6 Os2 Os3 C9 80.7(13) . . . . ? C14 Os2 Os3 C9 -108.5(13) . . . . ? P1 Os2 Os3 C9 -66.5(13) . . . . ? Os1 Os2 Os3 C9 -0.4(13) . . . . ? C4 Os2 Os3 C13 -110.1(5) . . . . ? C6 Os2 Os3 C13 161.2(4) . . . . ? C14 Os2 Os3 C13 -28.0(4) . . . . ? P1 Os2 Os3 C13 13.9(3) . . . . ? Os1 Os2 Os3 C13 80.1(2) . . . . ? C4 Os2 Os3 C14 -82.1(5) . . . . ? C6 Os2 Os3 C14 -170.8(5) . . . . ? P1 Os2 Os3 C14 42.0(4) . . . . ? Os1 Os2 Os3 C14 108.1(4) . . . . ? C4 Os2 Os3 C12 -146.1(5) . . . . ? C6 Os2 Os3 C12 125.2(4) . . . . ? C14 Os2 Os3 C12 -64.0(4) . . . . ? P1 Os2 Os3 C12 -22.1(3) . . . . ? Os1 Os2 Os3 C12 44.1(3) . . . . ? C4 Os2 Os3 Os1 169.8(4) . . . . ? C6 Os2 Os3 Os1 81.1(3) . . . . ? C14 Os2 Os3 Os1 -108.1(3) . . . . ? P1 Os2 Os3 Os1 -66.18(12) . . . . ? C1 Os1 Os3 C8 -87.4(5) . . . . ? C2 Os1 Os3 C8 154.6(9) . . . . ? C3 Os1 Os3 C8 5.7(4) . . . . ? C12 Os1 Os3 C8 -171.1(5) . . . . ? Os2 Os1 Os3 C8 84.0(3) . . . . ? C1 Os1 Os3 C7 -174.3(19) . . . . ? C2 Os1 Os3 C7 68(2) . . . . ? C3 Os1 Os3 C7 -81.2(19) . . . . ? C12 Os1 Os3 C7 102.0(19) . . . . ? Os2 Os1 Os3 C7 -2.9(18) . . . . ? C1 Os1 Os3 C9 8.5(5) . . . . ? C2 Os1 Os3 C9 -109.5(10) . . . . ? C3 Os1 Os3 C9 101.6(5) . . . . ? C12 Os1 Os3 C9 -75.2(5) . . . . ? Os2 Os1 Os3 C9 179.9(4) . . . . ? C1 Os1 Os3 C13 110.2(5) . . . . ? C2 Os1 Os3 C13 -7.8(9) . . . . ? C3 Os1 Os3 C13 -156.7(4) . . . . ? C12 Os1 Os3 C13 26.5(4) . . . . ? Os2 Os1 Os3 C13 -78.4(3) . . . . ? C1 Os1 Os3 C14 144.6(5) . . . . ? C2 Os1 Os3 C14 26.6(9) . . . . ? C3 Os1 Os3 C14 -122.3(4) . . . . ? C12 Os1 Os3 C14 60.9(5) . . . . ? Os2 Os1 Os3 C14 -43.9(3) . . . . ? C1 Os1 Os3 C12 83.7(5) . . . . ? C2 Os1 Os3 C12 -34.3(10) . . . . ? C3 Os1 Os3 C12 176.8(5) . . . . ? Os2 Os1 Os3 C12 -104.9(3) . . . . ? C1 Os1 Os3 Os2 -171.4(4) . . . . ? C2 Os1 Os3 Os2 70.6(9) . . . . ? C3 Os1 Os3 Os2 -78.3(3) . . . . ? C12 Os1 Os3 Os2 104.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 2.184 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.181 #===END======================================================================== data_VIIa _database_code_depnum_ccdc_archive 'CCDC 228039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Os3(CO)8(C6H5O)(PEt3) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H21 O9 Os3 P' _chemical_formula_weight 1006.94 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.66840(10) _cell_length_b 10.68670(10) _cell_length_c 12.1747(2) _cell_angle_alpha 85.1412(6) _cell_angle_beta 79.5292(6) _cell_angle_gamma 88.8925(7) _cell_volume 1232.53(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 15.536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.06686 _exptl_absorpt_correction_T_max 0.17701 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.12 (Bruker AXS, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16126 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 25.49 _reflns_number_total 4562 _reflns_number_gt 4363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The idealized position of the hydride hydrogen H(1) was estimated with XHYDEX program. Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0165P)^2^+5.4290P] 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 4562 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0579 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4807(6) 0.2801(5) 0.4058(5) 0.0250(12) Uani 1 1 d . . . C3 C 0.3239(6) 0.4867(5) 0.3530(5) 0.0220(12) Uani 1 1 d . . . C4 C 0.1456(6) 0.3688(6) 0.0025(5) 0.0268(13) Uani 1 1 d . . . C5 C -0.0490(7) 0.3424(6) 0.2005(5) 0.0274(13) Uani 1 1 d . . . C6 C 0.1753(7) 0.5267(6) 0.1581(6) 0.0336(15) Uani 1 1 d . . . C9 C 0.5849(7) 0.1381(6) 0.1410(5) 0.0317(14) Uani 1 1 d . . . C8 C 0.4943(6) 0.3892(6) 0.1253(5) 0.0259(13) Uani 1 1 d . . . C7 C 0.4332(6) 0.2140(5) -0.0267(5) 0.0263(13) Uani 1 1 d . . . C14 C 0.1867(6) 0.1531(5) 0.1447(5) 0.0226(12) Uani 1 1 d . . . C13 C 0.2501(6) 0.0804(5) 0.2233(5) 0.0220(12) Uani 1 1 d . . . C12 C 0.3220(6) 0.1222(5) 0.3050(5) 0.0231(12) Uani 1 1 d . . . C11 C 0.3866(8) 0.0110(5) 0.3521(5) 0.0315(14) Uani 1 1 d . . . H11 H 0.4476 0.0070 0.4052 0.038 Uiso 1 1 calc R . . C10 C 0.3403(9) -0.0861(7) 0.3032(7) 0.055(2) Uani 1 1 d . . . H10 H 0.3591 -0.1714 0.3244 0.066 Uiso 1 1 calc R . . C15 C 0.1357(7) 0.0773(6) 0.0626(6) 0.0367(16) Uani 1 1 d . . . H15A H 0.1758 -0.0075 0.0671 0.055 Uiso 1 1 calc R . . H15B H 0.1649 0.1174 -0.0133 0.055 Uiso 1 1 calc R . . H15C H 0.0328 0.0723 0.0802 0.055 Uiso 1 1 calc R . . C20 C -0.0127(6) 0.2845(6) 0.5233(5) 0.0279(13) Uani 1 1 d . . . H20A H -0.0635 0.2884 0.6013 0.033 Uiso 1 1 calc R . . H20B H -0.0356 0.3620 0.4795 0.033 Uiso 1 1 calc R . . C21 C -0.0658(7) 0.1711(6) 0.4742(6) 0.0361(15) Uani 1 1 d . . . H21A H -0.0066 0.1588 0.4015 0.054 Uiso 1 1 calc R . . H21B H -0.1632 0.1860 0.4643 0.054 Uiso 1 1 calc R . . H21C H -0.0614 0.0959 0.5255 0.054 Uiso 1 1 calc R . . C22 C 0.2072(6) 0.1331(5) 0.6014(5) 0.0243(12) Uani 1 1 d . . . H22A H 0.1934 0.0636 0.5556 0.029 Uiso 1 1 calc R . . H22B H 0.3067 0.1305 0.6111 0.029 Uiso 1 1 calc R . . C23 C 0.1136(8) 0.1086(7) 0.7176(6) 0.0432(18) Uani 1 1 d . . . H23A H 0.1396 0.1664 0.7688 0.065 Uiso 1 1 calc R . . H23B H 0.1268 0.0218 0.7470 0.065 Uiso 1 1 calc R . . H23C H 0.0148 0.1221 0.7110 0.065 Uiso 1 1 calc R . . C24 C 0.1929(6) 0.4008(6) 0.6195(5) 0.0263(13) Uani 1 1 d . . . H24A H 0.1662 0.4833 0.5859 0.032 Uiso 1 1 calc R . . H24B H 0.1255 0.3815 0.6902 0.032 Uiso 1 1 calc R . . C25 C 0.3391(7) 0.4108(6) 0.6466(5) 0.0326(14) Uani 1 1 d . . . H25A H 0.3619 0.3333 0.6888 0.049 Uiso 1 1 calc R . . H25B H 0.3422 0.4820 0.6918 0.049 Uiso 1 1 calc R . . H25C H 0.4078 0.4236 0.5768 0.049 Uiso 1 1 calc R . . O1 O 0.5818(5) 0.2579(5) 0.4402(4) 0.0384(11) Uani 1 1 d . . . O3 O 0.3279(5) 0.5931(4) 0.3586(4) 0.0341(10) Uani 1 1 d . . . O4 O 0.1411(5) 0.3827(5) -0.0902(4) 0.0418(12) Uani 1 1 d . . . O5 O -0.1687(5) 0.3354(5) 0.2229(4) 0.0428(12) Uani 1 1 d . . . O6 O 0.1874(7) 0.6326(5) 0.1544(5) 0.0571(16) Uani 1 1 d . . . O9 O 0.6879(6) 0.0869(6) 0.1479(5) 0.0568(15) Uani 1 1 d . . . O8 O 0.5471(5) 0.4856(4) 0.1130(4) 0.0371(11) Uani 1 1 d . . . O7 O 0.4418(5) 0.2082(5) -0.1196(4) 0.0429(12) Uani 1 1 d . . . O10 O 0.2606(5) -0.0490(4) 0.2166(4) 0.0359(11) Uani 1 1 d . . . P1 P 0.17627(15) 0.28117(13) 0.52355(12) 0.0193(3) Uani 1 1 d . . . Os1 Os 0.31485(2) 0.308220(18) 0.347036(17) 0.01604(7) Uani 1 1 d . . . Os2 Os 0.15027(2) 0.346383(19) 0.158616(18) 0.01867(7) Uani 1 1 d . . . Os3 Os 0.41362(2) 0.227226(19) 0.131606(17) 0.01850(7) Uani 1 1 d . . . H1 H 0.1380 0.3135 0.3141 0.050 Uiso 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 C1 0.025(3) 0.026(3) 0.023(3) -0.004(2) -0.002(3) 0.001(2) C3 0.021(3) 0.026(3) 0.019(3) -0.001(2) -0.004(2) 0.000(2) C4 0.024(3) 0.031(3) 0.026(3) 0.000(2) -0.007(3) -0.002(2) C5 0.029(3) 0.029(3) 0.026(3) 0.000(2) -0.010(3) 0.001(2) C6 0.037(4) 0.033(4) 0.034(4) 0.003(3) -0.018(3) 0.002(3) C9 0.029(3) 0.034(3) 0.031(3) -0.005(3) -0.002(3) 0.007(3) C8 0.027(3) 0.032(3) 0.018(3) 0.001(2) -0.004(2) -0.002(3) C7 0.026(3) 0.027(3) 0.026(3) -0.007(2) -0.003(3) -0.001(2) C14 0.021(3) 0.027(3) 0.018(3) -0.004(2) 0.001(2) 0.000(2) C13 0.026(3) 0.018(3) 0.019(3) -0.002(2) 0.004(2) -0.005(2) C12 0.025(3) 0.024(3) 0.020(3) -0.002(2) -0.001(2) 0.000(2) C11 0.054(4) 0.017(3) 0.021(3) 0.000(2) -0.002(3) 0.004(3) C10 0.066(5) 0.037(4) 0.055(5) 0.000(4) 0.005(4) 0.010(4) C15 0.042(4) 0.036(4) 0.031(4) -0.014(3) 0.002(3) -0.017(3) C20 0.016(3) 0.043(3) 0.022(3) 0.002(3) 0.001(2) 0.005(2) C21 0.028(3) 0.042(4) 0.039(4) 0.009(3) -0.012(3) -0.010(3) C22 0.022(3) 0.028(3) 0.020(3) 0.007(2) -0.003(2) 0.000(2) C23 0.038(4) 0.058(4) 0.026(3) 0.020(3) 0.005(3) 0.004(3) C24 0.028(3) 0.033(3) 0.017(3) -0.007(2) -0.001(2) 0.005(3) C25 0.035(4) 0.039(4) 0.026(3) -0.012(3) -0.008(3) -0.002(3) O1 0.027(2) 0.050(3) 0.042(3) -0.006(2) -0.016(2) 0.008(2) O3 0.037(3) 0.021(2) 0.046(3) -0.0065(19) -0.010(2) -0.0012(18) O4 0.053(3) 0.057(3) 0.017(2) 0.001(2) -0.012(2) 0.003(2) O5 0.023(3) 0.052(3) 0.051(3) -0.004(2) -0.002(2) 0.002(2) O6 0.081(4) 0.024(3) 0.074(4) 0.005(2) -0.041(3) -0.001(3) O9 0.040(3) 0.065(4) 0.067(4) -0.008(3) -0.015(3) 0.024(3) O8 0.049(3) 0.037(3) 0.026(2) 0.0012(19) -0.007(2) -0.020(2) O7 0.051(3) 0.057(3) 0.020(3) -0.009(2) -0.003(2) 0.006(2) O10 0.035(2) 0.0154(19) 0.055(3) -0.0053(19) -0.001(2) -0.0006(17) P1 0.0180(7) 0.0239(7) 0.0159(7) -0.0003(5) -0.0036(6) 0.0025(5) Os1 0.01706(12) 0.01701(11) 0.01425(11) -0.00124(8) -0.00345(8) 0.00035(8) Os2 0.02003(12) 0.02029(12) 0.01646(12) -0.00036(8) -0.00593(9) 0.00048(8) Os3 0.02061(12) 0.01896(11) 0.01521(12) -0.00178(8) -0.00116(9) 0.00026(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.145(7) . ? C1 Os1 1.880(6) . ? C3 O3 1.147(7) . ? C3 Os1 1.919(6) . ? C4 O4 1.134(7) . ? C4 Os2 1.904(6) . ? C5 O5 1.142(8) . ? C5 Os2 1.902(6) . ? C6 O6 1.136(8) . ? C6 Os2 1.946(7) . ? C9 O9 1.140(8) . ? C9 Os3 1.912(6) . ? C8 O8 1.145(7) . ? C8 Os3 1.902(6) . ? C7 O7 1.126(7) . ? C7 Os3 1.919(6) . ? C14 C13 1.401(8) . ? C14 C15 1.493(8) . ? C14 Os2 2.105(6) . ? C14 Os3 2.320(6) . ? C13 O10 1.393(7) . ? C13 C12 1.419(8) . ? C13 Os3 2.316(5) . ? C12 C11 1.455(8) . ? C12 Os1 2.091(6) . ? C12 Os3 2.336(6) . ? C11 C10 1.360(11) . ? C11 H11 0.9500 . ? C10 O10 1.440(10) . ? C10 H10 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C20 C21 1.533(9) . ? C20 P1 1.828(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.539(8) . ? C22 P1 1.823(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.517(8) . ? C24 P1 1.831(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? P1 Os1 2.3153(14) . ? Os1 Os3 2.8253(3) . ? Os1 Os2 3.0173(3) . ? Os1 H1 1.8246 . ? Os2 Os3 2.8025(3) . ? Os2 H1 1.8784 . ? 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 O1 C1 Os1 177.1(5) . . ? O3 C3 Os1 178.7(5) . . ? O4 C4 Os2 179.1(6) . . ? O5 C5 Os2 176.9(6) . . ? O6 C6 Os2 177.4(6) . . ? O9 C9 Os3 178.5(6) . . ? O8 C8 Os3 174.7(5) . . ? O7 C7 Os3 178.3(6) . . ? C13 C14 C15 113.3(5) . . ? C13 C14 Os2 120.9(4) . . ? C15 C14 Os2 125.4(4) . . ? C13 C14 Os3 72.2(3) . . ? C15 C14 Os3 126.2(4) . . ? Os2 C14 Os3 78.43(19) . . ? O10 C13 C14 118.9(5) . . ? O10 C13 C12 112.5(5) . . ? C14 C13 C12 128.2(5) . . ? O10 C13 Os3 125.7(4) . . ? C14 C13 Os3 72.6(3) . . ? C12 C13 Os3 73.0(3) . . ? C13 C12 C11 106.0(5) . . ? C13 C12 Os1 123.0(4) . . ? C11 C12 Os1 130.9(4) . . ? C13 C12 Os3 71.5(3) . . ? C11 C12 Os3 123.5(4) . . ? Os1 C12 Os3 79.11(19) . . ? C10 C11 C12 104.8(6) . . ? C10 C11 H11 127.6 . . ? C12 C11 H11 127.6 . . ? C11 C10 O10 114.6(6) . . ? C11 C10 H10 122.7 . . ? O10 C10 H10 122.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C20 P1 113.9(4) . . ? C21 C20 H20A 108.8 . . ? P1 C20 H20A 108.8 . . ? C21 C20 H20B 108.8 . . ? P1 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 P1 115.8(4) . . ? C23 C22 H22A 108.3 . . ? P1 C22 H22A 108.3 . . ? C23 C22 H22B 108.3 . . ? P1 C22 H22B 108.3 . . ? H22A C22 H22B 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 P1 114.3(4) . . ? C25 C24 H24A 108.7 . . ? P1 C24 H24A 108.7 . . ? C25 C24 H24B 108.7 . . ? P1 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C13 O10 C10 101.7(5) . . ? C22 P1 C20 105.0(3) . . ? C22 P1 C24 104.4(3) . . ? C20 P1 C24 101.7(3) . . ? C22 P1 Os1 113.9(2) . . ? C20 P1 Os1 114.2(2) . . ? C24 P1 Os1 116.2(2) . . ? C1 Os1 C3 92.8(2) . . ? C1 Os1 C12 89.5(2) . . ? C3 Os1 C12 168.0(2) . . ? C1 Os1 P1 91.93(18) . . ? C3 Os1 P1 92.58(17) . . ? C12 Os1 P1 99.09(16) . . ? C1 Os1 Os3 98.03(18) . . ? C3 Os1 Os3 113.74(17) . . ? C12 Os1 Os3 54.29(16) . . ? P1 Os1 Os3 151.17(4) . . ? C1 Os1 Os2 153.68(18) . . ? C3 Os1 Os2 90.12(16) . . ? C12 Os1 Os2 82.70(16) . . ? P1 Os1 Os2 114.08(3) . . ? Os3 Os1 Os2 57.214(7) . . ? C1 Os1 H1 168.3 . . ? C3 Os1 H1 93.7 . . ? C12 Os1 H1 86.1 . . ? P1 Os1 H1 78.1 . . ? Os3 Os1 H1 88.2 . . ? Os2 Os1 H1 36.0 . . ? C5 Os2 C4 93.5(3) . . ? C5 Os2 C6 98.0(3) . . ? C4 Os2 C6 88.9(3) . . ? C5 Os2 C14 98.6(2) . . ? C4 Os2 C14 89.6(2) . . ? C6 Os2 C14 163.4(3) . . ? C5 Os2 Os3 151.35(18) . . ? C4 Os2 Os3 94.95(18) . . ? C6 Os2 Os3 109.5(2) . . ? C14 Os2 Os3 54.21(15) . . ? C5 Os2 Os1 116.34(18) . . ? C4 Os2 Os1 150.05(18) . . ? C6 Os2 Os1 88.88(18) . . ? C14 Os2 Os1 84.13(16) . . ? Os3 Os2 Os1 57.946(7) . . ? C5 Os2 H1 81.5 . . ? C4 Os2 H1 173.9 . . ? C6 Os2 H1 95.2 . . ? C14 Os2 H1 87.6 . . ? Os3 Os2 H1 87.9 . . ? Os1 Os2 H1 34.8 . . ? C8 Os3 C9 94.9(3) . . ? C8 Os3 C7 97.9(2) . . ? C9 Os3 C7 93.2(3) . . ? C8 Os3 C13 148.5(2) . . ? C9 Os3 C13 100.7(2) . . ? C7 Os3 C13 108.3(2) . . ? C8 Os3 C14 134.6(2) . . ? C9 Os3 C14 130.2(2) . . ? C7 Os3 C14 86.2(2) . . ? C13 Os3 C14 35.2(2) . . ? C8 Os3 C12 119.9(2) . . ? C9 Os3 C12 86.7(2) . . ? C7 Os3 C12 142.1(2) . . ? C13 Os3 C12 35.5(2) . . ? C14 Os3 C12 66.0(2) . . ? C8 Os3 Os2 87.33(18) . . ? C9 Os3 Os2 169.9(2) . . ? C7 Os3 Os2 96.32(18) . . ? C13 Os3 Os2 72.98(14) . . ? C14 Os3 Os2 47.36(14) . . ? C12 Os3 Os2 83.68(14) . . ? C8 Os3 Os1 76.04(18) . . ? C9 Os3 Os1 106.06(19) . . ? C7 Os3 Os1 160.16(18) . . ? C13 Os3 Os1 73.42(14) . . ? C14 Os3 Os1 85.05(14) . . ? C12 Os3 Os1 46.60(14) . . ? Os2 Os3 Os1 64.840(7) . . ? 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 C15 C14 C13 O10 0.9(8) . . . . ? Os2 C14 C13 O10 174.2(4) . . . . ? Os3 C14 C13 O10 -121.7(5) . . . . ? C15 C14 C13 C12 173.0(6) . . . . ? Os2 C14 C13 C12 -13.6(8) . . . . ? Os3 C14 C13 C12 50.5(6) . . . . ? C15 C14 C13 Os3 122.5(5) . . . . ? Os2 C14 C13 Os3 -64.1(3) . . . . ? O10 C13 C12 C11 1.6(7) . . . . ? C14 C13 C12 C11 -171.0(6) . . . . ? Os3 C13 C12 C11 -120.7(4) . . . . ? O10 C13 C12 Os1 -174.8(4) . . . . ? C14 C13 C12 Os1 12.6(9) . . . . ? Os3 C13 C12 Os1 62.9(4) . . . . ? O10 C13 C12 Os3 122.2(4) . . . . ? C14 C13 C12 Os3 -50.3(6) . . . . ? C13 C12 C11 C10 -4.7(7) . . . . ? Os1 C12 C11 C10 171.3(5) . . . . ? Os3 C12 C11 C10 -82.8(7) . . . . ? C12 C11 C10 O10 6.4(8) . . . . ? C14 C13 O10 C10 175.3(6) . . . . ? C12 C13 O10 C10 2.0(6) . . . . ? Os3 C13 O10 C10 86.7(6) . . . . ? C11 C10 O10 C13 -5.4(8) . . . . ? C23 C22 P1 C20 -52.2(6) . . . . ? C23 C22 P1 C24 54.4(6) . . . . ? C23 C22 P1 Os1 -177.8(4) . . . . ? C21 C20 P1 C22 -56.5(5) . . . . ? C21 C20 P1 C24 -165.0(5) . . . . ? C21 C20 P1 Os1 69.0(5) . . . . ? C25 C24 P1 C22 65.0(5) . . . . ? C25 C24 P1 C20 174.0(5) . . . . ? C25 C24 P1 Os1 -61.3(5) . . . . ? O1 C1 Os1 C3 -167(11) . . . . ? O1 C1 Os1 C12 1(11) . . . . ? O1 C1 Os1 P1 100(11) . . . . ? O1 C1 Os1 Os3 -53(11) . . . . ? O1 C1 Os1 Os2 -71(11) . . . . ? O3 C3 Os1 C1 -88(23) . . . . ? O3 C3 Os1 C12 171(23) . . . . ? O3 C3 Os1 P1 4(23) . . . . ? O3 C3 Os1 Os3 172(100) . . . . ? O3 C3 Os1 Os2 118(23) . . . . ? C13 C12 Os1 C1 -159.6(5) . . . . ? C11 C12 Os1 C1 25.0(6) . . . . ? Os3 C12 Os1 C1 -100.3(2) . . . . ? C13 C12 Os1 C3 -58.3(13) . . . . ? C11 C12 Os1 C3 126.3(10) . . . . ? Os3 C12 Os1 C3 1.0(12) . . . . ? C13 C12 Os1 P1 108.6(5) . . . . ? C11 C12 Os1 P1 -66.9(6) . . . . ? Os3 C12 Os1 P1 167.86(10) . . . . ? C13 C12 Os1 Os3 -59.3(4) . . . . ? C11 C12 Os1 Os3 125.3(6) . . . . ? C13 C12 Os1 Os2 -4.8(4) . . . . ? C11 C12 Os1 Os2 179.8(6) . . . . ? Os3 C12 Os1 Os2 54.53(10) . . . . ? C22 P1 Os1 C1 -54.4(3) . . . . ? C20 P1 Os1 C1 -175.0(3) . . . . ? C24 P1 Os1 C1 67.0(3) . . . . ? C22 P1 Os1 C3 -147.3(3) . . . . ? C20 P1 Os1 C3 92.1(3) . . . . ? C24 P1 Os1 C3 -25.9(3) . . . . ? C22 P1 Os1 C12 35.4(3) . . . . ? C20 P1 Os1 C12 -85.2(3) . . . . ? C24 P1 Os1 C12 156.8(3) . . . . ? C22 P1 Os1 Os3 56.2(2) . . . . ? C20 P1 Os1 Os3 -64.4(2) . . . . ? C24 P1 Os1 Os3 177.5(2) . . . . ? C22 P1 Os1 Os2 121.4(2) . . . . ? C20 P1 Os1 Os2 0.8(2) . . . . ? C24 P1 Os1 Os2 -117.2(2) . . . . ? O5 C5 Os2 C4 60(10) . . . . ? O5 C5 Os2 C6 149(10) . . . . ? O5 C5 Os2 C14 -30(10) . . . . ? O5 C5 Os2 Os3 -47(11) . . . . ? O5 C5 Os2 Os1 -118(10) . . . . ? O4 C4 Os2 C5 21(37) . . . . ? O4 C4 Os2 C6 -77(37) . . . . ? O4 C4 Os2 C14 119(37) . . . . ? O4 C4 Os2 Os3 173(100) . . . . ? O4 C4 Os2 Os1 -163(37) . . . . ? O6 C6 Os2 C5 -68(16) . . . . ? O6 C6 Os2 C4 26(16) . . . . ? O6 C6 Os2 C14 111(16) . . . . ? O6 C6 Os2 Os3 121(16) . . . . ? O6 C6 Os2 Os1 176(16) . . . . ? C13 C14 Os2 C5 -109.1(5) . . . . ? C15 C14 Os2 C5 63.4(5) . . . . ? Os3 C14 Os2 C5 -170.1(2) . . . . ? C13 C14 Os2 C4 157.3(5) . . . . ? C15 C14 Os2 C4 -30.1(5) . . . . ? Os3 C14 Os2 C4 96.4(2) . . . . ? C13 C14 Os2 C6 72.2(10) . . . . ? C15 C14 Os2 C6 -115.2(9) . . . . ? Os3 C14 Os2 C6 11.3(9) . . . . ? C13 C14 Os2 Os3 61.0(4) . . . . ? C15 C14 Os2 Os3 -126.5(5) . . . . ? C13 C14 Os2 Os1 6.7(4) . . . . ? C15 C14 Os2 Os1 179.2(5) . . . . ? Os3 C14 Os2 Os1 -54.29(10) . . . . ? C1 Os1 Os2 C5 169.6(4) . . . . ? C3 Os1 Os2 C5 -93.8(3) . . . . ? C12 Os1 Os2 C5 95.8(3) . . . . ? P1 Os1 Os2 C5 -0.9(2) . . . . ? Os3 Os1 Os2 C5 147.7(2) . . . . ? C1 Os1 Os2 C4 -6.1(5) . . . . ? C3 Os1 Os2 C4 90.5(4) . . . . ? C12 Os1 Os2 C4 -79.9(4) . . . . ? P1 Os1 Os2 C4 -176.6(4) . . . . ? Os3 Os1 Os2 C4 -28.0(4) . . . . ? C1 Os1 Os2 C6 -92.0(4) . . . . ? C3 Os1 Os2 C6 4.6(3) . . . . ? C12 Os1 Os2 C6 -165.8(3) . . . . ? P1 Os1 Os2 C6 97.5(2) . . . . ? Os3 Os1 Os2 C6 -113.9(2) . . . . ? C1 Os1 Os2 C14 72.9(4) . . . . ? C3 Os1 Os2 C14 169.5(2) . . . . ? C12 Os1 Os2 C14 -0.9(2) . . . . ? P1 Os1 Os2 C14 -97.59(16) . . . . ? Os3 Os1 Os2 C14 51.00(15) . . . . ? C1 Os1 Os2 Os3 21.9(4) . . . . ? C3 Os1 Os2 Os3 118.53(17) . . . . ? C12 Os1 Os2 Os3 -51.87(16) . . . . ? P1 Os1 Os2 Os3 -148.60(4) . . . . ? O8 C8 Os3 C9 77(6) . . . . ? O8 C8 Os3 C7 -16(6) . . . . ? O8 C8 Os3 C13 -163(6) . . . . ? O8 C8 Os3 C14 -109(6) . . . . ? O8 C8 Os3 C12 166(6) . . . . ? O8 C8 Os3 Os2 -112(6) . . . . ? O8 C8 Os3 Os1 -177(6) . . . . ? O9 C9 Os3 C8 33(27) . . . . ? O9 C9 Os3 C7 131(27) . . . . ? O9 C9 Os3 C13 -120(27) . . . . ? O9 C9 Os3 C14 -141(27) . . . . ? O9 C9 Os3 C12 -87(27) . . . . ? O9 C9 Os3 Os2 -69(27) . . . . ? O9 C9 Os3 Os1 -44(27) . . . . ? O7 C7 Os3 C8 -77(20) . . . . ? O7 C7 Os3 C9 -173(20) . . . . ? O7 C7 Os3 C13 85(20) . . . . ? O7 C7 Os3 C14 57(20) . . . . ? O7 C7 Os3 C12 99(20) . . . . ? O7 C7 Os3 Os2 11(20) . . . . ? O7 C7 Os3 Os1 -7(20) . . . . ? O10 C13 Os3 C8 -155.6(5) . . . . ? C14 C13 Os3 C8 90.9(5) . . . . ? C12 C13 Os3 C8 -49.7(6) . . . . ? O10 C13 Os3 C9 -37.3(5) . . . . ? C14 C13 Os3 C9 -150.8(4) . . . . ? C12 C13 Os3 C9 68.5(4) . . . . ? O10 C13 Os3 C7 59.6(5) . . . . ? C14 C13 Os3 C7 -53.8(4) . . . . ? C12 C13 Os3 C7 165.5(3) . . . . ? O10 C13 Os3 C14 113.5(6) . . . . ? C12 C13 Os3 C14 -140.7(5) . . . . ? O10 C13 Os3 C12 -105.9(6) . . . . ? C14 C13 Os3 C12 140.7(5) . . . . ? O10 C13 Os3 Os2 150.8(5) . . . . ? C14 C13 Os3 Os2 37.3(3) . . . . ? C12 C13 Os3 Os2 -103.3(3) . . . . ? O10 C13 Os3 Os1 -141.1(5) . . . . ? C14 C13 Os3 Os1 105.4(3) . . . . ? C12 C13 Os3 Os1 -35.2(3) . . . . ? C13 C14 Os3 C8 -132.9(4) . . . . ? C15 C14 Os3 C8 120.8(5) . . . . ? Os2 C14 Os3 C8 -4.8(4) . . . . ? C13 C14 Os3 C9 38.8(5) . . . . ? C15 C14 Os3 C9 -67.5(6) . . . . ? Os2 C14 Os3 C9 166.9(3) . . . . ? C13 C14 Os3 C7 129.8(4) . . . . ? C15 C14 Os3 C7 23.5(5) . . . . ? Os2 C14 Os3 C7 -102.2(2) . . . . ? C15 C14 Os3 C13 -106.3(6) . . . . ? Os2 C14 Os3 C13 128.0(4) . . . . ? C13 C14 Os3 C12 -23.8(3) . . . . ? C15 C14 Os3 C12 -130.1(6) . . . . ? Os2 C14 Os3 C12 104.2(2) . . . . ? C13 C14 Os3 Os2 -128.0(4) . . . . ? C15 C14 Os3 Os2 125.7(6) . . . . ? C13 C14 Os3 Os1 -68.0(3) . . . . ? C15 C14 Os3 Os1 -174.3(5) . . . . ? Os2 C14 Os3 Os1 59.98(12) . . . . ? C13 C12 Os3 C8 152.6(3) . . . . ? C11 C12 Os3 C8 -110.1(5) . . . . ? Os1 C12 Os3 C8 22.2(3) . . . . ? C13 C12 Os3 C9 -113.7(4) . . . . ? C11 C12 Os3 C9 -16.4(5) . . . . ? Os1 C12 Os3 C9 115.9(2) . . . . ? C13 C12 Os3 C7 -22.8(5) . . . . ? C11 C12 Os3 C7 74.5(6) . . . . ? Os1 C12 Os3 C7 -153.2(3) . . . . ? C11 C12 Os3 C13 97.3(6) . . . . ? Os1 C12 Os3 C13 -130.5(4) . . . . ? C13 C12 Os3 C14 23.6(3) . . . . ? C11 C12 Os3 C14 120.9(5) . . . . ? Os1 C12 Os3 C14 -106.9(2) . . . . ? C13 C12 Os3 Os2 69.4(3) . . . . ? C11 C12 Os3 Os2 166.7(5) . . . . ? Os1 C12 Os3 Os2 -61.05(13) . . . . ? C13 C12 Os3 Os1 130.5(4) . . . . ? C11 C12 Os3 Os1 -132.3(6) . . . . ? C5 Os2 Os3 C8 -162.7(4) . . . . ? C4 Os2 Os3 C8 90.6(2) . . . . ? C6 Os2 Os3 C8 -0.1(3) . . . . ? C14 Os2 Os3 C8 176.5(3) . . . . ? Os1 Os2 Os3 C8 -75.83(17) . . . . ? C5 Os2 Os3 C9 -59.9(12) . . . . ? C4 Os2 Os3 C9 -166.6(11) . . . . ? C6 Os2 Os3 C9 102.8(11) . . . . ? C14 Os2 Os3 C9 -80.6(11) . . . . ? Os1 Os2 Os3 C9 27.0(11) . . . . ? C5 Os2 Os3 C7 99.6(4) . . . . ? C4 Os2 Os3 C7 -7.1(2) . . . . ? C6 Os2 Os3 C7 -97.7(3) . . . . ? C14 Os2 Os3 C7 78.9(3) . . . . ? Os1 Os2 Os3 C7 -173.49(18) . . . . ? C5 Os2 Os3 C13 -7.6(4) . . . . ? C4 Os2 Os3 C13 -114.3(2) . . . . ? C6 Os2 Os3 C13 155.1(3) . . . . ? C14 Os2 Os3 C13 -28.3(2) . . . . ? Os1 Os2 Os3 C13 79.28(15) . . . . ? C5 Os2 Os3 C14 20.7(4) . . . . ? C4 Os2 Os3 C14 -86.0(3) . . . . ? C6 Os2 Os3 C14 -176.6(3) . . . . ? Os1 Os2 Os3 C14 107.62(19) . . . . ? C5 Os2 Os3 C12 -42.3(4) . . . . ? C4 Os2 Os3 C12 -149.0(2) . . . . ? C6 Os2 Os3 C12 120.4(3) . . . . ? C14 Os2 Os3 C12 -63.0(2) . . . . ? Os1 Os2 Os3 C12 44.63(14) . . . . ? C5 Os2 Os3 Os1 -86.9(4) . . . . ? C4 Os2 Os3 Os1 166.39(18) . . . . ? C6 Os2 Os3 Os1 75.8(2) . . . . ? C14 Os2 Os3 Os1 -107.62(19) . . . . ? C1 Os1 Os3 C8 -76.7(3) . . . . ? C3 Os1 Os3 C8 19.9(3) . . . . ? C12 Os1 Os3 C8 -160.3(3) . . . . ? P1 Os1 Os3 C8 174.2(2) . . . . ? Os2 Os1 Os3 C8 93.65(18) . . . . ? C1 Os1 Os3 C9 14.4(3) . . . . ? C3 Os1 Os3 C9 111.1(3) . . . . ? C12 Os1 Os3 C9 -69.2(3) . . . . ? P1 Os1 Os3 C9 -94.7(2) . . . . ? Os2 Os1 Os3 C9 -175.2(2) . . . . ? C1 Os1 Os3 C7 -151.0(6) . . . . ? C3 Os1 Os3 C7 -54.3(6) . . . . ? C12 Os1 Os3 C7 125.4(6) . . . . ? P1 Os1 Os3 C7 99.9(5) . . . . ? Os2 Os1 Os3 C7 19.4(5) . . . . ? C1 Os1 Os3 C13 111.0(2) . . . . ? C3 Os1 Os3 C13 -152.3(2) . . . . ? C12 Os1 Os3 C13 27.5(2) . . . . ? P1 Os1 Os3 C13 1.96(17) . . . . ? Os2 Os1 Os3 C13 -78.61(15) . . . . ? C1 Os1 Os3 C14 144.9(2) . . . . ? C3 Os1 Os3 C14 -118.4(2) . . . . ? C12 Os1 Os3 C14 61.3(2) . . . . ? P1 Os1 Os3 C14 35.84(16) . . . . ? Os2 Os1 Os3 C14 -44.73(14) . . . . ? C1 Os1 Os3 C12 83.6(3) . . . . ? C3 Os1 Os3 C12 -179.8(3) . . . . ? P1 Os1 Os3 C12 -25.5(2) . . . . ? Os2 Os1 Os3 C12 -106.1(2) . . . . ? C1 Os1 Os3 Os2 -170.37(18) . . . . ? C3 Os1 Os3 Os2 -73.70(18) . . . . ? C12 Os1 Os3 Os2 106.1(2) . . . . ? P1 Os1 Os3 Os2 80.57(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.871 _refine_diff_density_min -1.497 _refine_diff_density_rms 0.176 #===END======================================================================== data_VIII _database_code_depnum_ccdc_archive 'CCDC 228040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Os3(CO)9(C6H6O)(PEt3) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H21 O10 Os3 P' _chemical_formula_weight 1034.95 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 'P 21/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 10.33170(10) _cell_length_b 15.5444(2) _cell_length_c 15.7323(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.3000(8) _cell_angle_gamma 90.00 _cell_volume 2506.13(5) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 15.289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.06670 _exptl_absorpt_correction_T_max 0.17688 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.12 (Bruker AXS, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31146 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5284 _reflns_number_gt 4699 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. The idealized position of the hydride hydrogen H(1) was estimated with XHYDEX program. Other hydrogens were placed in idealized position and constrained to ride on their parent atom. ; _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^)+(0.0204P)^2^+8.8475P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 5284 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0607 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0845(7) 0.8207(4) 0.6569(4) 0.0320(14) Uani 1 1 d . . . C2 C 0.8894(6) 0.7013(4) 0.6416(4) 0.0313(14) Uani 1 1 d . . . C3 C 1.0357(6) 0.7420(4) 0.8026(4) 0.0283(13) Uani 1 1 d . . . C4 C 0.7250(6) 0.9395(4) 0.8860(4) 0.0276(13) Uani 1 1 d . . . C5 C 0.6879(6) 0.7417(4) 0.7364(4) 0.0290(13) Uani 1 1 d . . . C6 C 0.8184(6) 0.7730(4) 0.9023(4) 0.0278(13) Uani 1 1 d . . . C7 C 0.8351(6) 1.0710(4) 0.7987(4) 0.0299(13) Uani 1 1 d . . . C8 C 1.0218(6) 0.9388(4) 0.8752(5) 0.0333(14) Uani 1 1 d . . . C9 C 1.0447(7) 1.0163(4) 0.7194(4) 0.0336(14) Uani 1 1 d . . . C14 C 0.6273(6) 0.9192(4) 0.7059(4) 0.0274(13) Uani 1 1 d . . . H1 H 0.5849 0.9701 0.7297 0.033 Uiso 1 1 calc R . . C13 C 0.7366(6) 0.9493(3) 0.6619(4) 0.0249(12) Uani 1 1 d . . . C11 C 0.8758(6) 0.9459(4) 0.5606(4) 0.0297(13) Uani 1 1 d . . . H11 H 0.9440 0.9306 0.5283 0.036 Uiso 1 1 calc R . . C10 C 0.7923(6) 1.0125(4) 0.5444(4) 0.0348(15) Uani 1 1 d . . . H10 H 0.7925 1.0502 0.4969 0.042 Uiso 1 1 calc R . . C16 C 0.5280(6) 0.8764(4) 0.6357(4) 0.0378(15) Uani 1 1 d . . . H16A H 0.5732 0.8339 0.6041 0.057 Uiso 1 1 calc R . . H16B H 0.4890 0.9206 0.5959 0.057 Uiso 1 1 calc R . . H16C H 0.4592 0.8478 0.6628 0.057 Uiso 1 1 calc R . . C20 C 0.5294(6) 0.8208(4) 0.9833(4) 0.0329(14) Uani 1 1 d . . . H20A H 0.5979 0.7815 1.0105 0.040 Uiso 1 1 calc R . . H20B H 0.5573 0.8803 0.9987 0.040 Uiso 1 1 calc R . . C21 C 0.4026(7) 0.8023(5) 1.0205(5) 0.0414(17) Uani 1 1 d . . . H21A H 0.3768 0.7424 1.0089 0.062 Uiso 1 1 calc R . . H21B H 0.3338 0.8406 0.9939 0.062 Uiso 1 1 calc R . . H21C H 0.4159 0.8121 1.0825 0.062 Uiso 1 1 calc R . . C26 C 0.3761(6) 0.8739(5) 0.8284(5) 0.0398(16) Uani 1 1 d . . . H26A H 0.3618 0.8710 0.7650 0.048 Uiso 1 1 calc R . . H26B H 0.2989 0.8480 0.8498 0.048 Uiso 1 1 calc R . . C27 C 0.3843(8) 0.9675(5) 0.8548(5) 0.0487(19) Uani 1 1 d . . . H27A H 0.4679 0.9915 0.8430 0.073 Uiso 1 1 calc R . . H27B H 0.3776 0.9721 0.9162 0.073 Uiso 1 1 calc R . . H27C H 0.3127 0.9995 0.8224 0.073 Uiso 1 1 calc R . . C32 C 0.4627(7) 0.6982(4) 0.8457(6) 0.0455(19) Uani 1 1 d . . . H32A H 0.3781 0.6906 0.8682 0.055 Uiso 1 1 calc R . . H32B H 0.4476 0.6888 0.7830 0.055 Uiso 1 1 calc R . . C33 C 0.5583(8) 0.6302(4) 0.8861(5) 0.0491(19) Uani 1 1 d . . . H33A H 0.5814 0.6428 0.9472 0.074 Uiso 1 1 calc R . . H33B H 0.6374 0.6310 0.8576 0.074 Uiso 1 1 calc R . . H33C H 0.5176 0.5733 0.8793 0.074 Uiso 1 1 calc R . . O1 O 1.1750(5) 0.8342(3) 0.6233(3) 0.0414(11) Uani 1 1 d . . . O2 O 0.8657(5) 0.6417(3) 0.5996(3) 0.0377(11) Uani 1 1 d . . . O3 O 1.1035(5) 0.7107(3) 0.8576(3) 0.0416(11) Uani 1 1 d . . . O4 O 0.7119(5) 0.9933(3) 0.9354(3) 0.0392(11) Uani 1 1 d . . . O5 O 0.6448(4) 0.6834(3) 0.6970(3) 0.0369(11) Uani 1 1 d . . . O6 O 0.8754(5) 0.7323(3) 0.9553(3) 0.0385(11) Uani 1 1 d . . . O7 O 0.7916(5) 1.1356(3) 0.8150(3) 0.0406(11) Uani 1 1 d . . . O8 O 1.0833(5) 0.9224(3) 0.9382(3) 0.0461(12) Uani 1 1 d . . . O9 O 1.1257(5) 1.0484(3) 0.6865(3) 0.0442(12) Uani 1 1 d . . . O10 O 0.7081(4) 1.0195(3) 0.6034(3) 0.0323(10) Uani 1 1 d . . . C12 C 0.8423(6) 0.9022(4) 0.6360(4) 0.0257(12) Uani 1 1 d . . . P1 P 0.51871(15) 0.80872(10) 0.86632(11) 0.0278(3) Uani 1 1 d . . . Os1 Os 0.93436(2) 0.801586(13) 0.709254(15) 0.02291(7) Uani 1 1 d . . . Os2 Os 0.71948(2) 0.839200(13) 0.813620(14) 0.02163(6) Uani 1 1 d . . . Os3 Os 0.91000(2) 0.963197(13) 0.771441(15) 0.02367(7) 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 C1 0.037(4) 0.028(3) 0.030(3) 0.003(2) 0.003(3) 0.004(3) C2 0.030(3) 0.024(3) 0.039(4) 0.003(3) 0.003(3) 0.003(2) C3 0.027(3) 0.025(3) 0.033(3) -0.004(2) 0.005(3) 0.000(2) C4 0.027(3) 0.024(3) 0.032(3) 0.001(2) 0.005(3) -0.004(2) C5 0.026(3) 0.027(3) 0.033(3) 0.002(2) 0.002(3) 0.005(2) C6 0.031(3) 0.025(3) 0.027(3) -0.002(2) 0.005(3) -0.001(2) C7 0.023(3) 0.026(3) 0.041(4) 0.004(3) 0.006(3) -0.005(2) C8 0.027(3) 0.029(3) 0.044(4) -0.006(3) 0.006(3) -0.008(3) C9 0.036(3) 0.027(3) 0.037(4) -0.005(3) 0.004(3) 0.003(3) C14 0.027(3) 0.021(3) 0.034(3) -0.003(2) -0.002(3) 0.001(2) C13 0.025(3) 0.020(3) 0.028(3) 0.000(2) -0.001(3) 0.004(2) C11 0.030(3) 0.028(3) 0.032(3) 0.002(2) 0.007(3) 0.001(2) C10 0.036(3) 0.032(3) 0.036(4) 0.007(3) 0.006(3) -0.004(3) C16 0.034(3) 0.039(4) 0.039(4) -0.007(3) -0.004(3) -0.006(3) C20 0.030(3) 0.041(3) 0.029(3) 0.003(3) 0.007(3) 0.003(3) C21 0.033(4) 0.051(4) 0.042(4) 0.009(3) 0.014(3) 0.002(3) C26 0.025(3) 0.058(4) 0.037(4) 0.002(3) 0.003(3) 0.006(3) C27 0.044(4) 0.047(4) 0.058(5) 0.012(4) 0.019(4) 0.018(3) C32 0.033(4) 0.040(4) 0.065(5) -0.011(3) 0.010(4) -0.019(3) C33 0.058(5) 0.030(4) 0.062(5) 0.001(3) 0.017(4) -0.008(3) O1 0.037(3) 0.043(3) 0.047(3) 0.010(2) 0.015(2) 0.004(2) O2 0.043(3) 0.029(2) 0.040(3) -0.007(2) 0.002(2) 0.000(2) O3 0.039(3) 0.041(3) 0.044(3) 0.008(2) 0.002(2) 0.007(2) O4 0.045(3) 0.031(2) 0.044(3) -0.014(2) 0.015(2) -0.011(2) O5 0.034(2) 0.028(2) 0.049(3) -0.015(2) 0.005(2) -0.0094(19) O6 0.044(3) 0.040(3) 0.032(3) 0.006(2) 0.006(2) 0.009(2) O7 0.038(3) 0.027(2) 0.059(3) -0.002(2) 0.015(2) -0.001(2) O8 0.036(3) 0.058(3) 0.041(3) 0.000(2) -0.011(2) -0.004(2) O9 0.035(3) 0.045(3) 0.056(3) 0.002(2) 0.017(3) -0.012(2) O10 0.032(2) 0.028(2) 0.037(2) 0.0076(18) 0.004(2) 0.0038(17) C12 0.027(3) 0.023(3) 0.028(3) -0.007(2) 0.003(3) -0.001(2) P1 0.0222(7) 0.0293(8) 0.0317(9) -0.0007(6) 0.0026(7) -0.0034(6) Os1 0.02312(12) 0.01854(11) 0.02712(13) -0.00024(8) 0.00337(10) 0.00134(8) Os2 0.02078(11) 0.01935(11) 0.02454(12) -0.00115(8) 0.00205(9) -0.00212(8) Os3 0.02141(12) 0.01898(11) 0.03042(13) -0.00208(8) 0.00257(10) -0.00283(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.150(8) . ? C1 Os1 1.871(7) . ? C2 O2 1.147(7) . ? C2 Os1 1.911(6) . ? C3 O3 1.150(7) . ? C3 Os1 1.929(6) . ? C4 O4 1.161(7) . ? C4 Os2 1.927(6) . ? C5 O5 1.155(7) . ? C5 Os2 1.943(6) . ? C6 O6 1.148(7) . ? C6 Os2 1.921(6) . ? C7 O7 1.143(7) . ? C7 Os3 1.917(6) . ? C8 O8 1.135(8) . ? C8 Os3 1.914(7) . ? C9 O9 1.151(8) . ? C9 Os3 1.892(7) . ? C14 C13 1.473(8) . ? C14 C16 1.558(8) . ? C14 Os2 2.218(6) . ? C14 H1 1.0000 . ? C13 C12 1.417(8) . ? C13 O10 1.434(7) . ? C13 Os3 2.333(6) . ? C11 C10 1.350(9) . ? C11 C12 1.447(8) . ? C11 H11 0.9500 . ? C10 O10 1.355(8) . ? C10 H10 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C20 C21 1.529(9) . ? C20 P1 1.839(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C26 C27 1.513(10) . ? C26 P1 1.824(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C32 C33 1.529(11) . ? C32 P1 1.828(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C12 Os1 2.097(6) . ? C12 Os3 2.355(6) . ? P1 Os2 2.3773(16) . ? Os1 Os3 2.7192(3) . ? Os1 Os2 2.9820(3) . ? Os2 Os3 2.8917(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Os1 178.1(6) . . ? O2 C2 Os1 177.9(6) . . ? O3 C3 Os1 174.9(5) . . ? O4 C4 Os2 168.7(5) . . ? O5 C5 Os2 166.0(5) . . ? O6 C6 Os2 178.7(5) . . ? O7 C7 Os3 179.3(5) . . ? O8 C8 Os3 176.8(6) . . ? O9 C9 Os3 179.0(6) . . ? C13 C14 C16 106.1(5) . . ? C13 C14 Os2 104.9(4) . . ? C16 C14 Os2 118.8(4) . . ? C13 C14 H1 108.9 . . ? C16 C14 H1 108.9 . . ? Os2 C14 H1 108.9 . . ? C12 C13 O10 108.2(5) . . ? C12 C13 C14 129.5(5) . . ? O10 C13 C14 115.8(5) . . ? C12 C13 Os3 73.3(3) . . ? O10 C13 Os3 118.6(4) . . ? C14 C13 Os3 104.2(4) . . ? C10 C11 C12 107.5(6) . . ? C10 C11 H11 126.2 . . ? C12 C11 H11 126.2 . . ? C11 C10 O10 112.5(6) . . ? C11 C10 H10 123.7 . . ? O10 C10 H10 123.7 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C21 C20 P1 114.7(5) . . ? C21 C20 H20A 108.6 . . ? P1 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? P1 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C26 P1 115.4(5) . . ? C27 C26 H26A 108.4 . . ? P1 C26 H26A 108.4 . . ? C27 C26 H26B 108.4 . . ? P1 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C32 P1 113.7(5) . . ? C33 C32 H32A 108.8 . . ? P1 C32 H32A 108.8 . . ? C33 C32 H32B 108.8 . . ? P1 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C10 O10 C13 106.3(5) . . ? C13 C12 C11 105.4(5) . . ? C13 C12 Os1 122.7(4) . . ? C11 C12 Os1 131.4(4) . . ? C13 C12 Os3 71.5(3) . . ? C11 C12 Os3 118.6(4) . . ? Os1 C12 Os3 75.03(19) . . ? C26 P1 C32 103.8(3) . . ? C26 P1 C20 102.4(3) . . ? C32 P1 C20 104.5(4) . . ? C26 P1 Os2 118.6(2) . . ? C32 P1 Os2 113.3(2) . . ? C20 P1 Os2 112.6(2) . . ? C1 Os1 C2 92.3(3) . . ? C1 Os1 C3 90.7(3) . . ? C2 Os1 C3 95.9(3) . . ? C1 Os1 C12 89.0(2) . . ? C2 Os1 C12 103.9(2) . . ? C3 Os1 C12 160.2(2) . . ? C1 Os1 Os3 97.56(19) . . ? C2 Os1 Os3 157.94(19) . . ? C3 Os1 Os3 103.66(17) . . ? C12 Os1 Os3 56.81(15) . . ? C1 Os1 Os2 158.21(19) . . ? C2 Os1 Os2 108.8(2) . . ? C3 Os1 Os2 92.59(18) . . ? C12 Os1 Os2 80.72(16) . . ? Os3 Os1 Os2 60.747(8) . . ? C6 Os2 C4 91.8(3) . . ? C6 Os2 C5 93.9(2) . . ? C4 Os2 C5 171.9(3) . . ? C6 Os2 C14 173.3(2) . . ? C4 Os2 C14 88.6(2) . . ? C5 Os2 C14 86.5(2) . . ? C6 Os2 P1 92.69(19) . . ? C4 Os2 P1 85.23(18) . . ? C5 Os2 P1 88.72(19) . . ? C14 Os2 P1 93.98(16) . . ? C6 Os2 Os3 102.09(18) . . ? C4 Os2 Os3 68.06(18) . . ? C5 Os2 Os3 116.21(18) . . ? C14 Os2 Os3 71.90(15) . . ? P1 Os2 Os3 149.59(4) . . ? C6 Os2 Os1 86.01(18) . . ? C4 Os2 Os1 121.05(18) . . ? C5 Os2 Os1 65.22(18) . . ? C14 Os2 Os1 88.09(16) . . ? P1 Os2 Os1 153.71(4) . . ? Os3 Os2 Os1 55.128(7) . . ? C9 Os3 C8 93.3(3) . . ? C9 Os3 C7 93.2(2) . . ? C8 Os3 C7 101.5(3) . . ? C9 Os3 C13 105.0(3) . . ? C8 Os3 C13 159.3(2) . . ? C7 Os3 C13 87.3(2) . . ? C9 Os3 C12 86.2(2) . . ? C8 Os3 C12 140.3(2) . . ? C7 Os3 C12 118.2(2) . . ? C13 Os3 C12 35.19(19) . . ? C9 Os3 Os1 98.06(18) . . ? C8 Os3 Os1 92.89(18) . . ? C7 Os3 Os1 161.17(18) . . ? C13 Os3 Os1 75.30(13) . . ? C12 Os3 Os1 48.16(14) . . ? C9 Os3 Os2 161.77(18) . . ? C8 Os3 Os2 91.54(18) . . ? C7 Os3 Os2 103.04(17) . . ? C13 Os3 Os2 68.06(14) . . ? C12 Os3 Os2 78.85(14) . . ? Os1 Os3 Os2 64.124(8) . . ? 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 C16 C14 C13 C12 -79.2(7) . . . . ? Os2 C14 C13 C12 47.4(7) . . . . ? C16 C14 C13 O10 68.7(6) . . . . ? Os2 C14 C13 O10 -164.7(4) . . . . ? C16 C14 C13 Os3 -159.1(4) . . . . ? Os2 C14 C13 Os3 -32.5(3) . . . . ? C12 C11 C10 O10 2.0(7) . . . . ? C11 C10 O10 C13 -2.0(7) . . . . ? C12 C13 O10 C10 1.3(6) . . . . ? C14 C13 O10 C10 -153.2(5) . . . . ? Os3 C13 O10 C10 81.8(5) . . . . ? O10 C13 C12 C11 -0.2(6) . . . . ? C14 C13 C12 C11 149.6(6) . . . . ? Os3 C13 C12 C11 -115.5(4) . . . . ? O10 C13 C12 Os1 172.8(4) . . . . ? C14 C13 C12 Os1 -37.4(8) . . . . ? Os3 C13 C12 Os1 57.5(4) . . . . ? O10 C13 C12 Os3 115.4(4) . . . . ? C14 C13 C12 Os3 -94.8(6) . . . . ? C10 C11 C12 C13 -1.0(7) . . . . ? C10 C11 C12 Os1 -173.2(5) . . . . ? C10 C11 C12 Os3 -78.1(6) . . . . ? C27 C26 P1 C32 167.2(6) . . . . ? C27 C26 P1 C20 58.6(6) . . . . ? C27 C26 P1 Os2 -66.0(6) . . . . ? C33 C32 P1 C26 -170.2(6) . . . . ? C33 C32 P1 C20 -63.2(6) . . . . ? C33 C32 P1 Os2 59.8(6) . . . . ? C21 C20 P1 C26 51.2(6) . . . . ? C21 C20 P1 C32 -56.8(6) . . . . ? C21 C20 P1 Os2 179.7(4) . . . . ? O1 C1 Os1 C2 102(19) . . . . ? O1 C1 Os1 C3 -162(19) . . . . ? O1 C1 Os1 C12 -2(19) . . . . ? O1 C1 Os1 Os3 -58(19) . . . . ? O1 C1 Os1 Os2 -63(19) . . . . ? O2 C2 Os1 C1 -4(16) . . . . ? O2 C2 Os1 C3 -95(16) . . . . ? O2 C2 Os1 C12 85(16) . . . . ? O2 C2 Os1 Os3 113(16) . . . . ? O2 C2 Os1 Os2 170(16) . . . . ? O3 C3 Os1 C1 35(6) . . . . ? O3 C3 Os1 C2 128(6) . . . . ? O3 C3 Os1 C12 -54(6) . . . . ? O3 C3 Os1 Os3 -63(6) . . . . ? O3 C3 Os1 Os2 -123(6) . . . . ? C13 C12 Os1 C1 -155.6(5) . . . . ? C11 C12 Os1 C1 15.4(6) . . . . ? Os3 C12 Os1 C1 -99.7(2) . . . . ? C13 C12 Os1 C2 112.3(5) . . . . ? C11 C12 Os1 C2 -76.7(6) . . . . ? Os3 C12 Os1 C2 168.2(2) . . . . ? C13 C12 Os1 C3 -66.3(9) . . . . ? C11 C12 Os1 C3 104.6(8) . . . . ? Os3 C12 Os1 C3 -10.5(8) . . . . ? C13 C12 Os1 Os3 -55.9(4) . . . . ? C11 C12 Os1 Os3 115.1(6) . . . . ? C13 C12 Os1 Os2 5.1(4) . . . . ? C11 C12 Os1 Os2 176.1(6) . . . . ? Os3 C12 Os1 Os2 61.00(10) . . . . ? O6 C6 Os2 C4 117(24) . . . . ? O6 C6 Os2 C5 -57(24) . . . . ? O6 C6 Os2 C14 -150(23) . . . . ? O6 C6 Os2 P1 32(24) . . . . ? O6 C6 Os2 Os3 -175(100) . . . . ? O6 C6 Os2 Os1 -122(24) . . . . ? O4 C4 Os2 C6 -80(3) . . . . ? O4 C4 Os2 C5 55(4) . . . . ? O4 C4 Os2 C14 107(3) . . . . ? O4 C4 Os2 P1 13(3) . . . . ? O4 C4 Os2 Os3 178(3) . . . . ? O4 C4 Os2 Os1 -166(3) . . . . ? O5 C5 Os2 C6 99(2) . . . . ? O5 C5 Os2 C4 -35(3) . . . . ? O5 C5 Os2 C14 -88(2) . . . . ? O5 C5 Os2 P1 6(2) . . . . ? O5 C5 Os2 Os3 -156(2) . . . . ? O5 C5 Os2 Os1 -177(2) . . . . ? C13 C14 Os2 C6 0(2) . . . . ? C16 C14 Os2 C6 118.5(19) . . . . ? C13 C14 Os2 C4 93.6(4) . . . . ? C16 C14 Os2 C4 -148.1(5) . . . . ? C13 C14 Os2 C5 -92.8(4) . . . . ? C16 C14 Os2 C5 25.5(5) . . . . ? C13 C14 Os2 P1 178.7(3) . . . . ? C16 C14 Os2 P1 -63.0(5) . . . . ? C13 C14 Os2 Os3 26.2(3) . . . . ? C16 C14 Os2 Os3 144.5(5) . . . . ? C13 C14 Os2 Os1 -27.6(3) . . . . ? C16 C14 Os2 Os1 90.7(5) . . . . ? C26 P1 Os2 C6 164.7(3) . . . . ? C32 P1 Os2 C6 -73.1(3) . . . . ? C20 P1 Os2 C6 45.3(3) . . . . ? C26 P1 Os2 C4 73.1(3) . . . . ? C32 P1 Os2 C4 -164.7(4) . . . . ? C20 P1 Os2 C4 -46.3(3) . . . . ? C26 P1 Os2 C5 -101.5(3) . . . . ? C32 P1 Os2 C5 20.7(3) . . . . ? C20 P1 Os2 C5 139.1(3) . . . . ? C26 P1 Os2 C14 -15.1(3) . . . . ? C32 P1 Os2 C14 107.1(3) . . . . ? C20 P1 Os2 C14 -134.6(3) . . . . ? C26 P1 Os2 Os3 45.1(3) . . . . ? C32 P1 Os2 Os3 167.3(3) . . . . ? C20 P1 Os2 Os3 -74.4(3) . . . . ? C26 P1 Os2 Os1 -108.8(3) . . . . ? C32 P1 Os2 Os1 13.3(3) . . . . ? C20 P1 Os2 Os1 131.7(2) . . . . ? C1 Os1 Os2 C6 -101.8(5) . . . . ? C2 Os1 Os2 C6 93.6(3) . . . . ? C3 Os1 Os2 C6 -3.5(2) . . . . ? C12 Os1 Os2 C6 -164.7(2) . . . . ? Os3 Os1 Os2 C6 -107.72(17) . . . . ? C1 Os1 Os2 C4 -12.1(6) . . . . ? C2 Os1 Os2 C4 -176.7(3) . . . . ? C3 Os1 Os2 C4 86.2(3) . . . . ? C12 Os1 Os2 C4 -75.0(3) . . . . ? Os3 Os1 Os2 C4 -18.0(2) . . . . ? C1 Os1 Os2 C5 162.1(5) . . . . ? C2 Os1 Os2 C5 -2.5(3) . . . . ? C3 Os1 Os2 C5 -99.6(3) . . . . ? C12 Os1 Os2 C5 99.1(2) . . . . ? Os3 Os1 Os2 C5 156.15(19) . . . . ? C1 Os1 Os2 C14 75.1(5) . . . . ? C2 Os1 Os2 C14 -89.5(2) . . . . ? C3 Os1 Os2 C14 173.4(2) . . . . ? C12 Os1 Os2 C14 12.2(2) . . . . ? Os3 Os1 Os2 C14 69.17(14) . . . . ? C1 Os1 Os2 P1 170.2(5) . . . . ? C2 Os1 Os2 P1 5.6(2) . . . . ? C3 Os1 Os2 P1 -91.51(19) . . . . ? C12 Os1 Os2 P1 107.26(18) . . . . ? Os3 Os1 Os2 P1 164.28(9) . . . . ? C1 Os1 Os2 Os3 5.9(5) . . . . ? C2 Os1 Os2 Os3 -158.7(2) . . . . ? C3 Os1 Os2 Os3 104.21(17) . . . . ? C12 Os1 Os2 Os3 -57.02(15) . . . . ? O9 C9 Os3 C8 162(32) . . . . ? O9 C9 Os3 C7 -96(32) . . . . ? O9 C9 Os3 C13 -8(32) . . . . ? O9 C9 Os3 C12 22(32) . . . . ? O9 C9 Os3 Os1 69(32) . . . . ? O9 C9 Os3 Os2 57(32) . . . . ? O8 C8 Os3 C9 -177(100) . . . . ? O8 C8 Os3 C7 89(11) . . . . ? O8 C8 Os3 C13 -25(11) . . . . ? O8 C8 Os3 C12 -89(11) . . . . ? O8 C8 Os3 Os1 -79(11) . . . . ? O8 C8 Os3 Os2 -15(11) . . . . ? O7 C7 Os3 C9 -31(50) . . . . ? O7 C7 Os3 C8 63(50) . . . . ? O7 C7 Os3 C13 -136(50) . . . . ? O7 C7 Os3 C12 -119(50) . . . . ? O7 C7 Os3 Os1 -158(100) . . . . ? O7 C7 Os3 Os2 157(100) . . . . ? C12 C13 Os3 C9 60.1(4) . . . . ? O10 C13 Os3 C9 -41.8(5) . . . . ? C14 C13 Os3 C9 -172.4(4) . . . . ? C12 C13 Os3 C8 -91.4(7) . . . . ? O10 C13 Os3 C8 166.7(6) . . . . ? C14 C13 Os3 C8 36.1(8) . . . . ? C12 C13 Os3 C7 152.7(4) . . . . ? O10 C13 Os3 C7 50.8(4) . . . . ? C14 C13 Os3 C7 -79.8(4) . . . . ? O10 C13 Os3 C12 -101.9(6) . . . . ? C14 C13 Os3 C12 127.5(5) . . . . ? C12 C13 Os3 Os1 -34.5(3) . . . . ? O10 C13 Os3 Os1 -136.4(4) . . . . ? C14 C13 Os3 Os1 93.0(3) . . . . ? C12 C13 Os3 Os2 -102.1(3) . . . . ? O10 C13 Os3 Os2 156.0(5) . . . . ? C14 C13 Os3 Os2 25.4(3) . . . . ? C13 C12 Os3 C9 -122.9(4) . . . . ? C11 C12 Os3 C9 -25.0(5) . . . . ? Os1 C12 Os3 C9 104.3(2) . . . . ? C13 C12 Os3 C8 146.4(4) . . . . ? C11 C12 Os3 C8 -115.7(5) . . . . ? Os1 C12 Os3 C8 13.6(4) . . . . ? C13 C12 Os3 C7 -31.3(4) . . . . ? C11 C12 Os3 C7 66.6(5) . . . . ? Os1 C12 Os3 C7 -164.1(2) . . . . ? C11 C12 Os3 C13 97.9(6) . . . . ? Os1 C12 Os3 C13 -132.7(4) . . . . ? C13 C12 Os3 Os1 132.7(4) . . . . ? C11 C12 Os3 Os1 -129.4(5) . . . . ? C13 C12 Os3 Os2 67.6(3) . . . . ? C11 C12 Os3 Os2 165.5(5) . . . . ? Os1 C12 Os3 Os2 -65.13(12) . . . . ? C1 Os1 Os3 C9 6.3(3) . . . . ? C2 Os1 Os3 C9 -109.5(6) . . . . ? C3 Os1 Os3 C9 98.8(3) . . . . ? C12 Os1 Os3 C9 -77.5(3) . . . . ? Os2 Os1 Os3 C9 -175.9(2) . . . . ? C1 Os1 Os3 C8 -87.5(3) . . . . ? C2 Os1 Os3 C8 156.7(6) . . . . ? C3 Os1 Os3 C8 5.1(3) . . . . ? C12 Os1 Os3 C8 -171.3(3) . . . . ? Os2 Os1 Os3 C8 90.31(19) . . . . ? C1 Os1 Os3 C7 132.4(6) . . . . ? C2 Os1 Os3 C7 16.6(8) . . . . ? C3 Os1 Os3 C7 -135.0(6) . . . . ? C12 Os1 Os3 C7 48.6(6) . . . . ? Os2 Os1 Os3 C7 -49.8(6) . . . . ? C1 Os1 Os3 C13 109.8(2) . . . . ? C2 Os1 Os3 C13 -6.0(5) . . . . ? C3 Os1 Os3 C13 -157.7(2) . . . . ? C12 Os1 Os3 C13 26.0(2) . . . . ? Os2 Os1 Os3 C13 -72.42(15) . . . . ? C1 Os1 Os3 C12 83.8(3) . . . . ? C2 Os1 Os3 C12 -32.0(6) . . . . ? C3 Os1 Os3 C12 176.4(3) . . . . ? Os2 Os1 Os3 C12 -98.38(19) . . . . ? C1 Os1 Os3 Os2 -177.78(19) . . . . ? C2 Os1 Os3 Os2 66.4(5) . . . . ? C3 Os1 Os3 Os2 -85.25(18) . . . . ? C12 Os1 Os3 Os2 98.38(19) . . . . ? C6 Os2 Os3 C9 89.4(7) . . . . ? C4 Os2 Os3 C9 176.5(7) . . . . ? C5 Os2 Os3 C9 -11.1(7) . . . . ? C14 Os2 Os3 C9 -87.6(7) . . . . ? P1 Os2 Os3 C9 -153.2(7) . . . . ? Os1 Os2 Os3 C9 13.1(6) . . . . ? C6 Os2 Os3 C8 -16.1(3) . . . . ? C4 Os2 Os3 C8 70.9(3) . . . . ? C5 Os2 Os3 C8 -116.6(3) . . . . ? C14 Os2 Os3 C8 166.9(2) . . . . ? P1 Os2 Os3 C8 101.2(2) . . . . ? Os1 Os2 Os3 C8 -92.47(19) . . . . ? C6 Os2 Os3 C7 -118.3(3) . . . . ? C4 Os2 Os3 C7 -31.2(3) . . . . ? C5 Os2 Os3 C7 141.2(3) . . . . ? C14 Os2 Os3 C7 64.7(3) . . . . ? P1 Os2 Os3 C7 -0.9(2) . . . . ? Os1 Os2 Os3 C7 165.3(2) . . . . ? C6 Os2 Os3 C13 160.1(2) . . . . ? C4 Os2 Os3 C13 -112.8(2) . . . . ? C5 Os2 Os3 C13 59.6(2) . . . . ? C14 Os2 Os3 C13 -16.9(2) . . . . ? P1 Os2 Os3 C13 -82.53(17) . . . . ? Os1 Os2 Os3 C13 83.76(15) . . . . ? C6 Os2 Os3 C12 125.1(2) . . . . ? C4 Os2 Os3 C12 -147.9(2) . . . . ? C5 Os2 Os3 C12 24.5(2) . . . . ? C14 Os2 Os3 C12 -52.0(2) . . . . ? P1 Os2 Os3 C12 -117.59(16) . . . . ? Os1 Os2 Os3 C12 48.70(14) . . . . ? C6 Os2 Os3 Os1 76.35(18) . . . . ? C4 Os2 Os3 Os1 163.41(19) . . . . ? C5 Os2 Os3 Os1 -24.15(19) . . . . ? C14 Os2 Os3 Os1 -100.66(16) . . . . ? P1 Os2 Os3 Os1 -166.29(8) . . . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 1.121 _refine_diff_density_min -1.492 _refine_diff_density_rms 0.177 #===END========================================================================