Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Birgit Weberndörfer' 'Helmut Werner' _publ_author_address ; Prof. Dr. Helmut Werner Institut fur Anorganische Chemie Universitat Wurzburg Am Hubland D-97074 Wurzburg Deutschland ; _publ_contact_author 'Prof. Dr. Helmut Werner' _publ_contact_author_address ; Prof. Dr. Helmut Werner Institut fur Anorganische Chemie Universitat Wurzburg Am Hubland D-97074 Wurzburg Deutschland ; _publ_contact_author_phone '049 931 888 5261' _publ_contact_author_fax '049 931 888 4605' _publ_contact_author_email helmut.werner@mail.uni-wuerzburg.de _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in "J. Chem. Soc., Dalton Trans." ; _publ_section_title ; Synthesis, molecular structure, and reactivity of allenylideneosmium complexes of the half-sandwich-type ; _publ_section_abstract ; The reaction of the areneosmium(II) compunds [(arene)OsX2(L)] 2a-2e, 3, 4 with propargylic alcohols HC(CCR2(OH) (where R = phenyl or p-tolyl) in the presence of AgPF6 leads to the formation of the cationic osmium allenylidenes [(arene)Os(=C=C=CR2)(L)X]PF6 5a-5h in good to excellent yields. Salt metathesis of 5a (L = PMe3) and 5b (L = PCy3) with NaB(ArF)4 gives [(mes)Os(=C=C=CPh2)(PR3)Cl]B(ArF)4 6a, 6b while treatment of 5b with KBr, NaI and CF3CO2Ag affords the corresponding bromo, iodo and trifluoracetato complexes [(mes)Os(=C=C=CPh2)(PCy3)X]PF6 7a-7c. Compound 5a reacts with MeOH and EtOH to give the Fischer-type osmium carbenes [(mes)Os{=C(OR)CH=CPh2} (PMe3)Cl]PF6 8a and 8b, of which 8a has been converted by treatment with NaH to the neutral allenyl complex [(mes)Os{C(OMe)=C=CPh2}(PMe3)Cl] 9. The reaction of 5a and 5b with tertiary phosphines PR'3 yields a mixture of [(mes)Os{C(PR'3)=C=CPh2}(PR3)Cl]PF6 10a-10c and [(mes)Os(PR3)(PR'3)Cl]PF6 11a-11c, which could not be separated by analytical tools. The cationic bis(phosphine) compounds 11a-11c were prepared independently from 2a-2c and PMe3 in the presence of NH4PF6. The molecular structures of 5a and 8b were determined crystallographically. ; data_bw3wb _database_code_CSD 172105 _publ_section_exptl_prep ; Crystals were grown from a dichloromethane layerde with hexane at room temperature ; _publ_section_exptl_refinement ; The four highest peaks of the final differential Fuorier-synthesis are less than 1.1 A from the Osmium atom away. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H31 Cl F6 Os P2' _chemical_formula_weight 757.11 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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_Int_Tables_number 14 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 8.424(3) _cell_length_b 14.521(2) _cell_length_c 23.448(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.043(15) _cell_angle_gamma 90.00 _cell_volume 2832.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour violett _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 4.764 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; empirical absorption correction by psi-scans from 7 reflections with chi-angles near 90 degrees ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 (Enraf-Nonius)' _diffrn_measurement_method 'Omega-Theta-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0.02 _diffrn_reflns_number 5483 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4957 _reflns_number_gt 3479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'CAD4 (Enraf-Nonius)' _computing_data_reduction 'CAD4 (Enraf-Nonius)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+18.5126P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 4957 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0885 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _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 Os Os 0.41082(5) 0.28303(3) 0.114222(18) 0.02953(14) Uani 1 1 d . . . P1 P 0.2576(3) 0.3394(2) 0.03074(13) 0.0387(7) Uani 1 1 d . . . Cl Cl 0.6303(3) 0.3325(2) 0.06903(14) 0.0477(8) Uani 1 1 d . . . C1 C 0.3752(11) 0.1670(8) 0.0774(4) 0.033(3) Uani 1 1 d . . . C2 C 0.3410(12) 0.0867(7) 0.0580(4) 0.030(2) Uani 1 1 d . . . C3 C 0.3135(11) -0.0016(7) 0.0382(5) 0.033(3) Uani 1 1 d . . . C4 C 0.2250(12) -0.0190(7) -0.0202(5) 0.034(3) Uani 1 1 d . . . C5 C 0.1271(12) 0.0503(8) -0.0476(5) 0.039(3) Uani 1 1 d . . . H5 H 0.1158 0.1065 -0.0279 0.047 Uiso 1 1 calc R . . C6 C 0.0471(13) 0.0383(9) -0.1026(5) 0.049(3) Uani 1 1 d . . . H6 H -0.0206 0.0857 -0.1207 0.059 Uiso 1 1 calc R . . C7 C 0.0646(14) -0.0429(10) -0.1319(5) 0.050(3) Uani 1 1 d . . . H7 H 0.0100 -0.0515 -0.1702 0.060 Uiso 1 1 calc R . . C8 C 0.1612(14) -0.1103(9) -0.1052(5) 0.046(3) Uani 1 1 d . . . H8 H 0.1728 -0.1660 -0.1254 0.056 Uiso 1 1 calc R . . C9 C 0.2432(12) -0.1004(8) -0.0494(5) 0.039(3) Uani 1 1 d . . . H9 H 0.3103 -0.1482 -0.0316 0.047 Uiso 1 1 calc R . . C10 C 0.3780(12) -0.0781(8) 0.0764(4) 0.034(3) Uani 1 1 d . . . C11 C 0.5250(13) -0.0694(8) 0.1140(5) 0.043(3) Uani 1 1 d . . . H11 H 0.5830 -0.0132 0.1151 0.052 Uiso 1 1 calc R . . C12 C 0.5853(15) -0.1403(9) 0.1489(5) 0.050(3) Uani 1 1 d . . . H12 H 0.6855 -0.1342 0.1736 0.060 Uiso 1 1 calc R . . C13 C 0.4978(16) -0.2219(10) 0.1477(6) 0.059(4) Uani 1 1 d . . . H13 H 0.5380 -0.2713 0.1723 0.071 Uiso 1 1 calc R . . C14 C 0.3515(16) -0.2318(9) 0.1106(6) 0.057(4) Uani 1 1 d . . . H14 H 0.2923 -0.2877 0.1088 0.068 Uiso 1 1 calc R . . C15 C 0.2989(13) -0.1601(8) 0.0782(5) 0.042(3) Uani 1 1 d . . . H15 H 0.1977 -0.1661 0.0541 0.050 Uiso 1 1 calc R . . C16 C 0.3263(16) 0.3039(10) -0.0355(5) 0.063(4) Uani 1 1 d . . . H16A H 0.2422 0.3165 -0.0685 0.094 Uiso 1 1 calc R . . H16B H 0.3501 0.2378 -0.0338 0.094 Uiso 1 1 calc R . . H16C H 0.4237 0.3382 -0.0401 0.094 Uiso 1 1 calc R . . C17 C 0.0466(14) 0.3082(9) 0.0191(5) 0.057(4) Uani 1 1 d . . . H17A H -0.0072 0.3384 0.0482 0.085 Uiso 1 1 calc R . . H17B H 0.0363 0.2412 0.0224 0.085 Uiso 1 1 calc R . . H17C H -0.0033 0.3280 -0.0195 0.085 Uiso 1 1 calc R . . C18 C 0.2524(18) 0.4637(9) 0.0265(6) 0.068(4) Uani 1 1 d . . . H18A H 0.3625 0.4878 0.0324 0.102 Uiso 1 1 calc R . . H18B H 0.1950 0.4882 0.0565 0.102 Uiso 1 1 calc R . . H18C H 0.1969 0.4826 -0.0116 0.102 Uiso 1 1 calc R . . C19 C 0.2442(13) 0.3264(8) 0.1761(5) 0.038(3) Uani 1 1 d . . . C20 C 0.3669(13) 0.3963(9) 0.1796(5) 0.049(3) Uani 1 1 d . . . H20 H 0.3373 0.4589 0.1724 0.058 Uiso 1 1 calc R . . C21 C 0.5276(14) 0.3727(8) 0.1934(5) 0.045(3) Uani 1 1 d . . . C22 C 0.5729(14) 0.2790(10) 0.2016(5) 0.053(3) Uani 1 1 d . . . H22 H 0.6836 0.2629 0.2075 0.063 Uiso 1 1 calc R . . C23 C 0.4586(15) 0.2108(9) 0.2011(5) 0.047(3) Uani 1 1 d . . . C24 C 0.2958(14) 0.2355(9) 0.1880(5) 0.047(3) Uani 1 1 d . . . H24 H 0.2170 0.1885 0.1871 0.057 Uiso 1 1 calc R . . C25 C 0.0713(13) 0.3517(10) 0.1660(6) 0.058(4) Uani 1 1 d . . . H25A H 0.0071 0.2983 0.1507 0.087 Uiso 1 1 calc R . . H25B H 0.0538 0.4024 0.1381 0.087 Uiso 1 1 calc R . . H25C H 0.0388 0.3712 0.2025 0.087 Uiso 1 1 calc R . . C26 C 0.6556(16) 0.4449(11) 0.1946(7) 0.084(5) Uani 1 1 d . . . H26A H 0.6086 0.5009 0.1756 0.126 Uiso 1 1 calc R . . H26B H 0.7406 0.4221 0.1742 0.126 Uiso 1 1 calc R . . H26C H 0.7011 0.4589 0.2347 0.126 Uiso 1 1 calc R . . C27 C 0.5079(17) 0.1137(9) 0.2137(5) 0.063(4) Uani 1 1 d . . . H27A H 0.6139 0.1032 0.2027 0.095 Uiso 1 1 calc R . . H27B H 0.4292 0.0723 0.1917 0.095 Uiso 1 1 calc R . . H27C H 0.5130 0.1018 0.2551 0.095 Uiso 1 1 calc R . . P2 P 0.0063(4) 0.6355(3) 0.18881(15) 0.0514(9) Uani 1 1 d . . . F1 F 0.0071(11) 0.5440(6) 0.2256(3) 0.080(3) Uani 1 1 d . . . F2 F -0.1725(9) 0.6547(8) 0.1965(4) 0.102(3) Uani 1 1 d . . . F3 F 0.0685(11) 0.6893(6) 0.2464(4) 0.102(3) Uani 1 1 d . . . F4 F 0.0048(10) 0.7226(6) 0.1499(5) 0.098(3) Uani 1 1 d . . . F5 F 0.1843(9) 0.6128(7) 0.1819(5) 0.106(4) Uani 1 1 d . . . F6 F -0.0579(12) 0.5754(7) 0.1328(3) 0.101(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os 0.0261(2) 0.0297(2) 0.0343(2) -0.0036(2) 0.00935(15) -0.0024(2) P1 0.0365(16) 0.0343(17) 0.0467(18) 0.0064(15) 0.0105(13) 0.0047(14) Cl 0.0352(15) 0.0494(18) 0.063(2) 0.0010(16) 0.0228(14) -0.0073(14) C1 0.022(5) 0.047(7) 0.033(6) 0.002(5) 0.011(4) 0.002(5) C2 0.031(6) 0.036(7) 0.022(5) 0.005(5) -0.001(4) -0.003(5) C3 0.026(5) 0.037(6) 0.039(6) -0.011(5) 0.018(5) -0.001(5) C4 0.028(5) 0.036(6) 0.042(7) -0.004(5) 0.015(5) -0.007(5) C5 0.039(6) 0.036(6) 0.041(7) -0.006(5) 0.004(5) 0.001(5) C6 0.037(7) 0.059(8) 0.051(8) -0.017(7) 0.009(6) 0.002(6) C7 0.041(7) 0.074(10) 0.035(7) 0.003(7) 0.011(5) -0.011(7) C8 0.045(7) 0.055(8) 0.043(7) -0.013(6) 0.018(6) -0.019(6) C9 0.029(6) 0.037(7) 0.055(8) -0.005(6) 0.019(5) -0.007(5) C10 0.035(6) 0.037(6) 0.032(6) -0.007(5) 0.014(5) 0.004(5) C11 0.048(7) 0.043(7) 0.043(7) -0.017(6) 0.027(6) -0.017(6) C12 0.055(8) 0.052(8) 0.043(7) 0.009(7) 0.008(6) 0.020(7) C13 0.068(9) 0.061(9) 0.056(8) 0.027(8) 0.032(7) 0.016(8) C14 0.057(8) 0.052(9) 0.072(9) 0.012(7) 0.040(7) -0.005(7) C15 0.036(6) 0.036(7) 0.057(8) -0.004(6) 0.020(6) 0.000(5) C16 0.067(9) 0.082(11) 0.041(7) 0.024(7) 0.012(6) 0.009(8) C17 0.048(7) 0.071(10) 0.049(8) -0.008(7) 0.000(6) 0.000(7) C18 0.092(11) 0.040(8) 0.073(10) 0.022(7) 0.010(8) 0.012(8) C19 0.038(6) 0.046(7) 0.036(7) -0.014(6) 0.023(5) 0.000(5) C20 0.042(7) 0.048(8) 0.061(8) -0.012(7) 0.023(6) -0.001(6) C21 0.047(7) 0.042(7) 0.051(8) -0.026(6) 0.021(6) -0.004(6) C22 0.039(6) 0.086(10) 0.030(6) -0.023(7) -0.007(5) 0.013(8) C23 0.059(8) 0.054(8) 0.026(6) -0.008(6) 0.001(5) 0.003(7) C24 0.048(7) 0.064(9) 0.033(6) -0.009(6) 0.017(5) -0.025(7) C25 0.043(7) 0.068(9) 0.068(9) -0.019(8) 0.022(6) -0.005(7) C26 0.056(9) 0.084(12) 0.121(14) -0.062(11) 0.045(9) -0.033(8) C27 0.090(10) 0.069(10) 0.030(7) 0.017(7) 0.005(7) 0.021(8) P2 0.0447(18) 0.056(2) 0.054(2) 0.0091(18) 0.0090(16) -0.0039(16) F1 0.122(7) 0.069(6) 0.047(5) 0.007(4) 0.008(5) -0.028(5) F2 0.053(5) 0.142(9) 0.116(8) -0.020(7) 0.030(5) -0.010(6) F3 0.095(7) 0.076(7) 0.120(8) -0.037(6) -0.026(6) -0.011(5) F4 0.080(6) 0.071(6) 0.144(9) 0.055(6) 0.024(6) 0.011(5) F5 0.063(5) 0.107(8) 0.159(9) 0.066(7) 0.050(6) 0.026(5) F6 0.154(9) 0.093(7) 0.048(5) -0.001(5) -0.005(5) 0.020(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 Os C1 1.896(11) . ? Os C24 2.221(11) . ? Os C19 2.261(10) . ? Os C23 2.271(12) . ? Os C22 2.277(10) . ? Os C20 2.318(12) . ? Os P1 2.318(3) . ? Os C21 2.354(11) . ? Os Cl 2.382(3) . ? P1 C18 1.808(12) . ? P1 C17 1.813(12) . ? P1 C16 1.816(13) . ? C1 C2 1.268(14) . ? C2 C3 1.370(14) . ? C3 C10 1.476(15) . ? C3 C4 1.476(14) . ? C4 C9 1.386(14) . ? C4 C5 1.392(15) . ? C5 C6 1.369(15) . ? C6 C7 1.384(17) . ? C7 C8 1.361(17) . ? C8 C9 1.388(15) . ? C10 C15 1.368(15) . ? C10 C11 1.408(15) . ? C11 C12 1.362(16) . ? C12 C13 1.393(18) . ? C13 C14 1.399(18) . ? C14 C15 1.324(16) . ? C19 C24 1.405(16) . ? C19 C20 1.442(15) . ? C19 C25 1.484(15) . ? C20 C21 1.384(16) . ? C21 C22 1.419(17) . ? C21 C26 1.501(16) . ? C22 C23 1.380(17) . ? C23 C24 1.404(16) . ? C23 C27 1.485(17) . ? P2 F4 1.559(9) . ? P2 F5 1.568(8) . ? P2 F2 1.570(8) . ? P2 F3 1.578(9) . ? P2 F1 1.583(8) . ? P2 F6 1.598(9) . ? 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 C1 Os C24 91.2(4) . . ? C1 Os C19 118.0(4) . . ? C24 Os C19 36.5(4) . . ? C1 Os C23 89.5(4) . . ? C24 Os C23 36.4(4) . . ? C19 Os C23 66.0(4) . . ? C1 Os C22 114.6(5) . . ? C24 Os C22 64.2(4) . . ? C19 Os C22 77.0(4) . . ? C23 Os C22 35.3(4) . . ? C1 Os C20 154.4(4) . . ? C24 Os C20 64.6(4) . . ? C19 Os C20 36.7(4) . . ? C23 Os C20 76.0(5) . . ? C22 Os C20 63.8(4) . . ? C1 Os P1 84.4(3) . . ? C24 Os P1 121.0(3) . . ? C19 Os P1 97.1(3) . . ? C23 Os P1 156.6(3) . . ? C22 Os P1 160.8(4) . . ? C20 Os P1 100.5(3) . . ? C1 Os C21 150.2(4) . . ? C24 Os C21 74.8(4) . . ? C19 Os C21 64.2(4) . . ? C23 Os C21 63.6(5) . . ? C22 Os C21 35.6(4) . . ? C20 Os C21 34.5(4) . . ? P1 Os C21 125.4(3) . . ? C1 Os Cl 98.3(3) . . ? C24 Os Cl 154.7(3) . . ? C19 Os Cl 143.6(3) . . ? C23 Os Cl 119.9(3) . . ? C22 Os Cl 90.6(3) . . ? C20 Os Cl 107.2(3) . . ? P1 Os Cl 83.44(11) . . ? C21 Os Cl 85.8(3) . . ? C18 P1 C17 103.1(7) . . ? C18 P1 C16 104.2(7) . . ? C17 P1 C16 103.7(6) . . ? C18 P1 Os 113.9(5) . . ? C17 P1 Os 116.2(4) . . ? C16 P1 Os 114.4(4) . . ? C2 C1 Os 172.5(9) . . ? C1 C2 C3 176.6(11) . . ? C2 C3 C10 118.3(9) . . ? C2 C3 C4 120.5(10) . . ? C10 C3 C4 121.2(9) . . ? C9 C4 C5 119.5(10) . . ? C9 C4 C3 121.7(10) . . ? C5 C4 C3 118.8(10) . . ? C6 C5 C4 120.7(11) . . ? C5 C6 C7 120.0(12) . . ? C8 C7 C6 119.1(12) . . ? C7 C8 C9 122.1(12) . . ? C4 C9 C8 118.5(11) . . ? C15 C10 C11 116.3(11) . . ? C15 C10 C3 122.6(10) . . ? C11 C10 C3 121.1(10) . . ? C12 C11 C10 121.1(11) . . ? C11 C12 C13 119.0(12) . . ? C12 C13 C14 120.8(12) . . ? C15 C14 C13 117.3(12) . . ? C14 C15 C10 125.5(12) . . ? C24 C19 C20 117.0(10) . . ? C24 C19 C25 122.0(11) . . ? C20 C19 C25 120.8(11) . . ? C24 C19 Os 70.2(6) . . ? C20 C19 Os 73.8(6) . . ? C25 C19 Os 131.2(8) . . ? C21 C20 C19 120.4(12) . . ? C21 C20 Os 74.2(7) . . ? C19 C20 Os 69.5(6) . . ? C20 C21 C22 120.1(11) . . ? C20 C21 C26 120.3(12) . . ? C22 C21 C26 119.4(12) . . ? C20 C21 Os 71.3(7) . . ? C22 C21 Os 69.2(6) . . ? C26 C21 Os 127.6(9) . . ? C23 C22 C21 121.0(11) . . ? C23 C22 Os 72.1(6) . . ? C21 C22 Os 75.1(7) . . ? C22 C23 C24 118.3(12) . . ? C22 C23 C27 120.4(12) . . ? C24 C23 C27 121.2(12) . . ? C22 C23 Os 72.6(7) . . ? C24 C23 Os 69.9(6) . . ? C27 C23 Os 128.5(8) . . ? C23 C24 C19 123.0(11) . . ? C23 C24 Os 73.7(7) . . ? C19 C24 Os 73.3(7) . . ? F4 P2 F5 91.7(5) . . ? F4 P2 F2 90.2(6) . . ? F5 P2 F2 178.0(6) . . ? F4 P2 F3 94.0(6) . . ? F5 P2 F3 89.9(6) . . ? F2 P2 F3 90.5(5) . . ? F4 P2 F1 177.2(6) . . ? F5 P2 F1 87.6(5) . . ? F2 P2 F1 90.5(5) . . ? F3 P2 F1 88.7(5) . . ? F4 P2 F6 89.5(5) . . ? F5 P2 F6 90.4(6) . . ? F2 P2 F6 89.1(5) . . ? F3 P2 F6 176.4(6) . . ? F1 P2 F6 87.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Os P1 C18 -172.0(6) . . . . ? C24 Os P1 C18 99.9(7) . . . . ? C19 Os P1 C18 70.3(6) . . . . ? C23 Os P1 C18 112.5(10) . . . . ? C22 Os P1 C18 -0.4(11) . . . . ? C20 Os P1 C18 33.3(6) . . . . ? C21 Os P1 C18 7.1(7) . . . . ? Cl Os P1 C18 -73.0(5) . . . . ? C1 Os P1 C17 68.4(6) . . . . ? C24 Os P1 C17 -19.6(6) . . . . ? C19 Os P1 C17 -49.2(6) . . . . ? C23 Os P1 C17 -7.1(10) . . . . ? C22 Os P1 C17 -119.9(10) . . . . ? C20 Os P1 C17 -86.2(6) . . . . ? C21 Os P1 C17 -112.5(6) . . . . ? Cl Os P1 C17 167.4(5) . . . . ? C1 Os P1 C16 -52.4(6) . . . . ? C24 Os P1 C16 -140.5(6) . . . . ? C19 Os P1 C16 -170.0(6) . . . . ? C23 Os P1 C16 -127.9(9) . . . . ? C22 Os P1 C16 119.2(11) . . . . ? C20 Os P1 C16 153.0(6) . . . . ? C21 Os P1 C16 126.7(6) . . . . ? Cl Os P1 C16 46.6(5) . . . . ? C24 Os C1 C2 6(7) . . . . ? C19 Os C1 C2 -20(7) . . . . ? C23 Os C1 C2 43(7) . . . . ? C22 Os C1 C2 68(7) . . . . ? C20 Os C1 C2 -12(7) . . . . ? P1 Os C1 C2 -115(7) . . . . ? C21 Os C1 C2 67(7) . . . . ? Cl Os C1 C2 163(7) . . . . ? Os C1 C2 C3 -105(18) . . . . ? C1 C2 C3 C10 44(19) . . . . ? C1 C2 C3 C4 -135(18) . . . . ? C2 C3 C4 C9 156.4(10) . . . . ? C10 C3 C4 C9 -22.1(14) . . . . ? C2 C3 C4 C5 -20.4(14) . . . . ? C10 C3 C4 C5 161.2(9) . . . . ? C9 C4 C5 C6 1.0(16) . . . . ? C3 C4 C5 C6 177.8(10) . . . . ? C4 C5 C6 C7 -0.9(17) . . . . ? C5 C6 C7 C8 0.4(17) . . . . ? C6 C7 C8 C9 -0.1(17) . . . . ? C5 C4 C9 C8 -0.6(15) . . . . ? C3 C4 C9 C8 -177.3(9) . . . . ? C7 C8 C9 C4 0.2(16) . . . . ? C2 C3 C10 C15 144.8(10) . . . . ? C4 C3 C10 C15 -36.8(14) . . . . ? C2 C3 C10 C11 -34.0(14) . . . . ? C4 C3 C10 C11 144.4(10) . . . . ? C15 C10 C11 C12 1.7(15) . . . . ? C3 C10 C11 C12 -179.5(10) . . . . ? C10 C11 C12 C13 -1.2(17) . . . . ? C11 C12 C13 C14 1.1(18) . . . . ? C12 C13 C14 C15 -1.6(18) . . . . ? C13 C14 C15 C10 2.3(19) . . . . ? C11 C10 C15 C14 -2.3(17) . . . . ? C3 C10 C15 C14 178.8(11) . . . . ? C1 Os C19 C24 47.2(8) . . . . ? C23 Os C19 C24 -28.4(7) . . . . ? C22 Os C19 C24 -64.0(7) . . . . ? C20 Os C19 C24 -127.3(10) . . . . ? P1 Os C19 C24 134.6(6) . . . . ? C21 Os C19 C24 -99.4(8) . . . . ? Cl Os C19 C24 -136.8(6) . . . . ? C1 Os C19 C20 174.6(7) . . . . ? C24 Os C19 C20 127.3(10) . . . . ? C23 Os C19 C20 98.9(8) . . . . ? C22 Os C19 C20 63.4(8) . . . . ? P1 Os C19 C20 -98.1(7) . . . . ? C21 Os C19 C20 27.9(7) . . . . ? Cl Os C19 C20 -9.5(10) . . . . ? C1 Os C19 C25 -68.5(13) . . . . ? C24 Os C19 C25 -115.7(14) . . . . ? C23 Os C19 C25 -144.1(13) . . . . ? C22 Os C19 C25 -179.7(13) . . . . ? C20 Os C19 C25 117.0(15) . . . . ? P1 Os C19 C25 18.9(12) . . . . ? C21 Os C19 C25 144.9(13) . . . . ? Cl Os C19 C25 107.5(11) . . . . ? C24 C19 C20 C21 0.9(16) . . . . ? C25 C19 C20 C21 175.0(11) . . . . ? Os C19 C20 C21 -56.2(10) . . . . ? C24 C19 C20 Os 57.1(9) . . . . ? C25 C19 C20 Os -128.7(11) . . . . ? C1 Os C20 C21 120.6(10) . . . . ? C24 Os C20 C21 100.2(8) . . . . ? C19 Os C20 C21 131.8(11) . . . . ? C23 Os C20 C21 63.4(8) . . . . ? C22 Os C20 C21 27.9(8) . . . . ? P1 Os C20 C21 -140.4(7) . . . . ? Cl Os C20 C21 -54.0(8) . . . . ? C1 Os C20 C19 -11.2(14) . . . . ? C24 Os C20 C19 -31.6(7) . . . . ? C23 Os C20 C19 -68.5(7) . . . . ? C22 Os C20 C19 -103.9(8) . . . . ? P1 Os C20 C19 87.8(7) . . . . ? C21 Os C20 C19 -131.8(11) . . . . ? Cl Os C20 C19 174.1(6) . . . . ? C19 C20 C21 C22 2.9(17) . . . . ? Os C20 C21 C22 -51.1(10) . . . . ? C19 C20 C21 C26 177.3(11) . . . . ? Os C20 C21 C26 123.3(11) . . . . ? C19 C20 C21 Os 54.0(10) . . . . ? C1 Os C21 C20 -131.5(9) . . . . ? C24 Os C21 C20 -67.1(8) . . . . ? C19 Os C21 C20 -29.6(7) . . . . ? C23 Os C21 C20 -104.4(8) . . . . ? C22 Os C21 C20 -133.9(11) . . . . ? P1 Os C21 C20 50.3(8) . . . . ? Cl Os C21 C20 129.2(7) . . . . ? C1 Os C21 C22 2.4(12) . . . . ? C24 Os C21 C22 66.8(8) . . . . ? C19 Os C21 C22 104.3(8) . . . . ? C23 Os C21 C22 29.5(7) . . . . ? C20 Os C21 C22 133.9(11) . . . . ? P1 Os C21 C22 -175.8(6) . . . . ? Cl Os C21 C22 -96.9(7) . . . . ? C1 Os C21 C26 114.1(13) . . . . ? C24 Os C21 C26 178.5(13) . . . . ? C19 Os C21 C26 -144.0(13) . . . . ? C23 Os C21 C26 141.3(13) . . . . ? C22 Os C21 C26 111.7(14) . . . . ? C20 Os C21 C26 -114.4(15) . . . . ? P1 Os C21 C26 -64.1(12) . . . . ? Cl Os C21 C26 14.8(11) . . . . ? C20 C21 C22 C23 -5.8(17) . . . . ? C26 C21 C22 C23 179.7(11) . . . . ? Os C21 C22 C23 -57.9(10) . . . . ? C20 C21 C22 Os 52.1(10) . . . . ? C26 C21 C22 Os -122.4(11) . . . . ? C1 Os C22 C23 -48.4(8) . . . . ? C24 Os C22 C23 30.3(7) . . . . ? C19 Os C22 C23 66.7(7) . . . . ? C20 Os C22 C23 103.2(8) . . . . ? P1 Os C22 C23 140.7(9) . . . . ? C21 Os C22 C23 130.3(11) . . . . ? Cl Os C22 C23 -147.8(7) . . . . ? C1 Os C22 C21 -178.7(6) . . . . ? C24 Os C22 C21 -100.0(8) . . . . ? C19 Os C22 C21 -63.6(7) . . . . ? C23 Os C22 C21 -130.3(11) . . . . ? C20 Os C22 C21 -27.0(6) . . . . ? P1 Os C22 C21 10.4(14) . . . . ? Cl Os C22 C21 81.9(7) . . . . ? C21 C22 C23 C24 4.7(16) . . . . ? Os C22 C23 C24 -54.7(9) . . . . ? C21 C22 C23 C27 -175.7(11) . . . . ? Os C22 C23 C27 124.9(11) . . . . ? C21 C22 C23 Os 59.4(10) . . . . ? C1 Os C23 C22 137.1(7) . . . . ? C24 Os C23 C22 -130.1(11) . . . . ? C19 Os C23 C22 -101.6(8) . . . . ? C20 Os C23 C22 -64.2(7) . . . . ? P1 Os C23 C22 -148.4(7) . . . . ? C21 Os C23 C22 -29.8(7) . . . . ? Cl Os C23 C22 37.9(8) . . . . ? C1 Os C23 C24 -92.7(8) . . . . ? C19 Os C23 C24 28.5(7) . . . . ? C22 Os C23 C24 130.1(11) . . . . ? C20 Os C23 C24 65.9(7) . . . . ? P1 Os C23 C24 -18.3(13) . . . . ? C21 Os C23 C24 100.3(8) . . . . ? Cl Os C23 C24 168.0(6) . . . . ? C1 Os C23 C27 21.7(12) . . . . ? C24 Os C23 C27 114.5(15) . . . . ? C19 Os C23 C27 143.0(13) . . . . ? C22 Os C23 C27 -115.4(15) . . . . ? C20 Os C23 C27 -179.6(13) . . . . ? P1 Os C23 C27 96.2(13) . . . . ? C21 Os C23 C27 -145.2(13) . . . . ? Cl Os C23 C27 -77.5(12) . . . . ? C22 C23 C24 C19 -0.8(17) . . . . ? C27 C23 C24 C19 179.7(11) . . . . ? Os C23 C24 C19 -56.8(10) . . . . ? C22 C23 C24 Os 56.0(9) . . . . ? C27 C23 C24 Os -123.5(10) . . . . ? C20 C19 C24 C23 -2.0(16) . . . . ? C25 C19 C24 C23 -176.1(10) . . . . ? Os C19 C24 C23 57.0(10) . . . . ? C20 C19 C24 Os -59.0(9) . . . . ? C25 C19 C24 Os 127.0(11) . . . . ? C1 Os C24 C23 87.5(8) . . . . ? C19 Os C24 C23 -132.9(11) . . . . ? C22 Os C24 C23 -29.4(7) . . . . ? C20 Os C24 C23 -101.2(8) . . . . ? P1 Os C24 C23 171.6(6) . . . . ? C21 Os C24 C23 -65.9(7) . . . . ? Cl Os C24 C23 -25.0(13) . . . . ? C1 Os C24 C19 -139.6(7) . . . . ? C23 Os C24 C19 132.9(11) . . . . ? C22 Os C24 C19 103.5(8) . . . . ? C20 Os C24 C19 31.7(6) . . . . ? P1 Os C24 C19 -55.4(7) . . . . ? C21 Os C24 C19 67.0(7) . . . . ? Cl Os C24 C19 107.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.423 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.179 #===END data_bw5wb _database_code_CSD 172106 _publ_section_exptl_prep ; Crystals were grown from dichloromethane layered with hexane at room temperature. ; _publ_section_exptl_refinement ; The methyl group C17 of the ethoxy substituent was found rotation-disordered with the methylene carbon atom C16 as rotation centre. Two independent positions were found and refined with constraints (ISOR) with the occupancy factors 67.2 : 32.8. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point '145 (dec.)' _chemical_formula_moiety ? _chemical_formula_sum 'C29 H37 Cl F6 O Os P2' _chemical_formula_weight 803.18 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_Int_Tables_number 14 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 10.164(3) _cell_length_b 16.6152(19) _cell_length_c 18.957(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.362(13) _cell_angle_gamma 90.00 _cell_volume 3138.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 4.307 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; empirical absorption correction by psi-scans from 6 reflections with chi-angles near 90 degrees ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 (Enraf-Nonius)' _diffrn_measurement_method 'omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 3600 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.7 _diffrn_reflns_number 5943 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5525 _reflns_number_gt 4168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'CAD4 (Enraf-Nonius)' _computing_data_reduction 'BEGIN (SDP)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0186P)^2^+7.2093P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 5525 _refine_ls_number_parameters 378 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _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 Os Os 0.04792(3) 0.043227(15) 0.811148(12) 0.03151(8) Uani 1 1 d . . . P1 P 0.19904(19) 0.10824(10) 0.75142(9) 0.0387(4) Uani 1 1 d . . . P2 P 0.5471(2) -0.15927(13) 0.85475(11) 0.0592(6) Uani 1 1 d . . . Cl Cl -0.0794(2) 0.16298(12) 0.77283(11) 0.0640(6) Uani 1 1 d . . . O O -0.1472(4) -0.0345(3) 0.6929(2) 0.0577(14) Uani 1 1 d . B . C1 C -0.0215(7) -0.0185(4) 0.7219(3) 0.0386(16) Uani 1 1 d . . . C2 C 0.0679(7) -0.0635(4) 0.6840(3) 0.0382(16) Uani 1 1 d . . . H2 H 0.1596 -0.0636 0.7075 0.046 Uiso 1 1 calc R . . C3 C 0.0414(6) -0.1050(4) 0.6212(3) 0.0320(14) Uani 1 1 d . . . C4 C 0.1483(6) -0.1506(4) 0.5956(3) 0.0339(15) Uani 1 1 d . . . C5 C 0.2630(7) -0.1745(5) 0.6424(4) 0.056(2) Uani 1 1 d . . . H5 H 0.2713 -0.1644 0.6924 0.067 Uiso 1 1 calc R . . C6 C 0.3656(8) -0.2125(5) 0.6183(5) 0.072(3) Uani 1 1 d . . . H6 H 0.4444 -0.2276 0.6515 0.087 Uiso 1 1 calc R . . C7 C 0.3545(8) -0.2288(5) 0.5457(5) 0.071(3) Uani 1 1 d . . . H7 H 0.4253 -0.2552 0.5289 0.085 Uiso 1 1 calc R . . C8 C 0.2409(9) -0.2065(5) 0.4986(4) 0.062(2) Uani 1 1 d . . . H8 H 0.2329 -0.2173 0.4488 0.075 Uiso 1 1 calc R . . C9 C 0.1377(8) -0.1687(4) 0.5227(4) 0.0462(18) Uani 1 1 d . . . H9 H 0.0584 -0.1546 0.4894 0.055 Uiso 1 1 calc R . . C10 C -0.0935(7) -0.1051(4) 0.5715(3) 0.0352(15) Uani 1 1 d . . . C11 C -0.1473(7) -0.0353(4) 0.5364(3) 0.0431(16) Uani 1 1 d . . . H11 H -0.0991 0.0139 0.5441 0.052 Uiso 1 1 calc R . . C12 C -0.2712(7) -0.0380(5) 0.4902(4) 0.0523(19) Uani 1 1 d . . . H12 H -0.3077 0.0096 0.4663 0.063 Uiso 1 1 calc R . . C13 C -0.3416(7) -0.1086(6) 0.4787(4) 0.058(2) Uani 1 1 d . . . H13 H -0.4268 -0.1099 0.4473 0.070 Uiso 1 1 calc R . . C14 C -0.2876(8) -0.1780(5) 0.5133(4) 0.056(2) Uani 1 1 d . . . H14 H -0.3364 -0.2271 0.5059 0.068 Uiso 1 1 calc R . . C15 C -0.1633(7) -0.1761(4) 0.5582(3) 0.0419(17) Uani 1 1 d . . . H15 H -0.1254 -0.2244 0.5803 0.050 Uiso 1 1 calc R . . C16 C -0.2631(7) 0.0043(7) 0.7150(4) 0.082(3) Uani 1 1 d . . . H16A H -0.2325 0.0352 0.7599 0.098 Uiso 1 1 calc R A 1 H16B H -0.3273 -0.0372 0.7244 0.098 Uiso 1 1 calc R A 1 C17 C -0.3318(17) 0.0606(14) 0.6556(8) 0.142(9) Uani 0.67 1 d PU B 1 H17A H -0.2675 0.1010 0.6459 0.213 Uiso 0.67 1 calc PR B 1 H17B H -0.4074 0.0874 0.6708 0.213 Uiso 0.67 1 calc PR B 1 H17C H -0.3648 0.0294 0.6118 0.213 Uiso 0.67 1 calc PR B 1 C17' C -0.376(2) -0.0250(19) 0.6566(12) 0.067(8) Uani 0.33 1 d PU B 2 H17D H -0.3652 -0.0031 0.6101 0.101 Uiso 0.33 1 calc PR B 2 H17E H -0.4621 -0.0071 0.6671 0.101 Uiso 0.33 1 calc PR B 2 H17F H -0.3746 -0.0839 0.6547 0.101 Uiso 0.33 1 calc PR B 2 C20 C 0.0454(8) -0.0758(4) 0.8662(3) 0.0415(17) Uani 1 1 d . . . C21 C -0.0616(7) -0.0286(4) 0.8830(3) 0.0473(18) Uani 1 1 d . . . H21 H -0.1501 -0.0498 0.8733 0.057 Uiso 1 1 calc R . . C22 C -0.0393(7) 0.0478(4) 0.9135(3) 0.0448(17) Uani 1 1 d . . . C23 C 0.0953(8) 0.0766(4) 0.9321(3) 0.0481(19) Uani 1 1 d . . . H23 H 0.1119 0.1271 0.9555 0.058 Uiso 1 1 calc R . . C24 C 0.2019(7) 0.0331(4) 0.9170(3) 0.0420(16) Uani 1 1 d . . . C25 C 0.1762(7) -0.0430(5) 0.8822(3) 0.0441(16) Uani 1 1 d . . . H25 H 0.2484 -0.0721 0.8694 0.053 Uiso 1 1 calc R . . C26 C 0.0214(10) -0.1594(4) 0.8355(4) 0.074(3) Uani 1 1 d . . . H26A H 0.0971 -0.1755 0.8137 0.111 Uiso 1 1 calc R . . H26B H -0.0614 -0.1600 0.7989 0.111 Uiso 1 1 calc R . . H26C H 0.0129 -0.1971 0.8741 0.111 Uiso 1 1 calc R . . C27 C -0.1554(9) 0.0972(5) 0.9271(4) 0.076(3) Uani 1 1 d . . . H27A H -0.2397 0.0711 0.9047 0.114 Uiso 1 1 calc R . . H27B H -0.1513 0.1510 0.9065 0.114 Uiso 1 1 calc R . . H27C H -0.1510 0.1017 0.9791 0.114 Uiso 1 1 calc R . . C28 C 0.3441(8) 0.0619(5) 0.9417(4) 0.070(3) Uani 1 1 d . . . H28A H 0.3449 0.1207 0.9456 0.105 Uiso 1 1 calc R . . H28B H 0.3982 0.0453 0.9068 0.105 Uiso 1 1 calc R . . H28C H 0.3816 0.0383 0.9888 0.105 Uiso 1 1 calc R . . C30 C 0.1328(8) 0.1349(4) 0.6585(3) 0.0520(19) Uani 1 1 d . . . H30A H 0.1974 0.1693 0.6406 0.078 Uiso 1 1 calc R . . H30B H 0.0480 0.1640 0.6554 0.078 Uiso 1 1 calc R . . H30C H 0.1171 0.0859 0.6293 0.078 Uiso 1 1 calc R . . C31 C 0.2533(8) 0.2042(4) 0.7931(4) 0.061(2) Uani 1 1 d . . . H31A H 0.3075 0.1949 0.8412 0.091 Uiso 1 1 calc R . . H31B H 0.1746 0.2367 0.7971 0.091 Uiso 1 1 calc R . . H31C H 0.3072 0.2329 0.7636 0.091 Uiso 1 1 calc R . . C32 C 0.3559(7) 0.0590(5) 0.7458(4) 0.057(2) Uani 1 1 d . . . H32A H 0.4090 0.0942 0.7208 0.086 Uiso 1 1 calc R . . H32B H 0.3372 0.0083 0.7192 0.086 Uiso 1 1 calc R . . H32C H 0.4063 0.0478 0.7944 0.086 Uiso 1 1 calc R . . F1 F 0.4006(6) -0.1454(4) 0.8122(3) 0.122(2) Uani 1 1 d . . . F2 F 0.4940(5) -0.1694(3) 0.9255(2) 0.0849(16) Uani 1 1 d . . . F3 F 0.6945(5) -0.1706(3) 0.8962(4) 0.113(2) Uani 1 1 d . . . F4 F 0.5995(9) -0.1481(4) 0.7827(3) 0.152(3) Uani 1 1 d . . . F5 F 0.5637(6) -0.0644(3) 0.8684(3) 0.1008(19) Uani 1 1 d . . . F6 F 0.5348(5) -0.2524(3) 0.8402(3) 0.0921(17) 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 Os 0.04307(15) 0.02712(13) 0.02569(12) 0.00109(13) 0.01008(10) 0.00355(14) P1 0.0505(11) 0.0350(10) 0.0335(9) 0.0012(8) 0.0156(8) 0.0004(8) P2 0.0765(16) 0.0523(13) 0.0505(12) 0.0094(10) 0.0171(11) 0.0209(12) Cl 0.0815(15) 0.0560(12) 0.0656(12) 0.0296(10) 0.0416(11) 0.0361(11) O 0.037(3) 0.092(4) 0.042(3) -0.017(3) 0.003(2) 0.000(3) C1 0.038(4) 0.047(4) 0.030(3) -0.001(3) 0.006(3) -0.003(3) C2 0.036(4) 0.042(4) 0.035(3) -0.002(3) 0.002(3) 0.003(3) C3 0.039(4) 0.031(3) 0.026(3) 0.005(3) 0.005(3) -0.004(3) C4 0.040(4) 0.029(3) 0.036(3) -0.008(3) 0.014(3) -0.010(3) C5 0.048(5) 0.064(5) 0.050(4) -0.023(4) -0.002(4) 0.005(4) C6 0.050(5) 0.081(6) 0.081(6) -0.033(5) -0.001(5) 0.013(5) C7 0.044(5) 0.078(6) 0.097(7) -0.046(6) 0.031(5) -0.010(5) C8 0.077(6) 0.064(5) 0.057(5) -0.022(4) 0.040(5) -0.017(5) C9 0.064(5) 0.034(4) 0.041(4) 0.001(3) 0.013(4) -0.001(4) C10 0.046(4) 0.035(4) 0.025(3) -0.007(3) 0.010(3) -0.009(3) C11 0.046(4) 0.047(4) 0.036(4) 0.003(3) 0.007(3) -0.008(4) C12 0.053(5) 0.061(5) 0.039(4) 0.005(4) 0.001(3) 0.001(4) C13 0.037(4) 0.097(7) 0.038(4) -0.006(4) 0.003(3) -0.014(5) C14 0.058(5) 0.058(5) 0.051(5) -0.012(4) 0.005(4) -0.023(4) C15 0.050(4) 0.036(4) 0.039(4) -0.002(3) 0.007(3) -0.015(3) C16 0.029(4) 0.156(10) 0.063(5) -0.026(6) 0.019(4) 0.001(5) C17 0.112(15) 0.26(3) 0.051(9) 0.019(14) 0.013(9) 0.121(18) C17' 0.048(15) 0.11(2) 0.039(13) -0.020(16) 0.007(11) 0.034(17) C20 0.063(5) 0.025(3) 0.032(4) -0.004(3) 0.000(3) 0.000(3) C21 0.058(5) 0.056(5) 0.028(3) 0.008(3) 0.010(3) -0.008(4) C22 0.070(5) 0.043(4) 0.027(3) 0.014(3) 0.023(3) 0.013(4) C23 0.080(6) 0.033(4) 0.033(4) -0.003(3) 0.014(4) -0.009(4) C24 0.054(4) 0.044(4) 0.028(3) 0.001(3) 0.007(3) -0.004(4) C25 0.053(4) 0.051(4) 0.026(3) 0.000(3) 0.001(3) 0.008(4) C26 0.125(8) 0.031(4) 0.063(5) -0.009(4) 0.007(5) -0.002(5) C27 0.107(7) 0.075(6) 0.060(5) 0.013(5) 0.050(5) 0.028(6) C28 0.070(6) 0.081(7) 0.047(5) 0.003(4) -0.017(4) -0.018(5) C30 0.081(6) 0.045(4) 0.032(4) 0.009(3) 0.017(4) 0.003(4) C31 0.088(6) 0.052(5) 0.049(5) -0.004(4) 0.029(4) -0.012(5) C32 0.044(4) 0.068(6) 0.062(5) 0.000(4) 0.017(4) -0.002(4) F1 0.126(5) 0.138(5) 0.077(4) -0.031(4) -0.041(3) 0.072(4) F2 0.083(4) 0.122(5) 0.052(3) 0.002(3) 0.019(3) -0.019(3) F3 0.053(3) 0.094(4) 0.187(6) 0.035(4) 0.012(4) 0.002(3) F4 0.280(9) 0.098(5) 0.114(5) 0.012(4) 0.129(6) 0.035(6) F5 0.164(6) 0.051(3) 0.091(4) 0.008(3) 0.033(4) 0.026(3) F6 0.102(4) 0.058(3) 0.116(4) -0.007(3) 0.021(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os C1 1.985(6) . ? Os C25 2.207(7) . ? Os C20 2.238(6) . ? Os C21 2.262(6) . ? Os C22 2.287(6) . ? Os C24 2.295(6) . ? Os C23 2.315(6) . ? Os P1 2.3438(18) . ? Os Cl 2.4064(18) . ? P1 C30 1.812(6) . ? P1 C32 1.814(7) . ? P1 C31 1.817(7) . ? P2 F2 1.551(5) . ? P2 F3 1.560(6) . ? P2 F1 1.565(6) . ? P2 F4 1.572(5) . ? P2 F6 1.572(5) . ? P2 F5 1.600(5) . ? O C1 1.315(7) . ? O C16 1.474(8) . ? C1 C2 1.469(8) . ? C2 C3 1.358(8) . ? C3 C4 1.482(8) . ? C3 C10 1.503(8) . ? C4 C5 1.378(9) . ? C4 C9 1.397(8) . ? C5 C6 1.371(10) . ? C6 C7 1.386(11) . ? C7 C8 1.364(11) . ? C8 C9 1.376(10) . ? C10 C15 1.375(8) . ? C10 C11 1.394(9) . ? C11 C12 1.386(9) . ? C12 C13 1.369(10) . ? C13 C14 1.386(11) . ? C14 C15 1.379(9) . ? C16 C17' 1.51(3) . ? C16 C17 1.523(17) . ? C20 C25 1.413(9) . ? C20 C21 1.427(9) . ? C20 C26 1.507(9) . ? C21 C22 1.394(10) . ? C22 C23 1.426(10) . ? C22 C27 1.501(10) . ? C23 C24 1.378(9) . ? C24 C25 1.426(9) . ? C24 C28 1.507(9) . ? 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 C1 Os C25 104.6(3) . . ? C1 Os C20 84.6(2) . . ? C25 Os C20 37.1(2) . . ? C1 Os C21 96.1(3) . . ? C25 Os C21 65.9(3) . . ? C20 Os C21 37.0(2) . . ? C1 Os C22 127.4(3) . . ? C25 Os C22 77.6(2) . . ? C20 Os C22 65.9(2) . . ? C21 Os C22 35.7(2) . . ? C1 Os C24 140.7(3) . . ? C25 Os C24 36.9(2) . . ? C20 Os C24 66.2(2) . . ? C21 Os C24 76.5(2) . . ? C22 Os C24 64.7(2) . . ? C1 Os C23 159.6(3) . . ? C25 Os C23 64.4(2) . . ? C20 Os C23 76.6(2) . . ? C21 Os C23 63.9(2) . . ? C22 Os C23 36.1(2) . . ? C24 Os C23 34.8(2) . . ? C1 Os P1 89.03(19) . . ? C25 Os P1 103.24(19) . . ? C20 Os P1 134.5(2) . . ? C21 Os P1 168.86(19) . . ? C22 Os P1 142.6(2) . . ? C24 Os P1 93.30(17) . . ? C23 Os P1 109.88(19) . . ? C1 Os Cl 95.2(2) . . ? C25 Os Cl 159.81(18) . . ? C20 Os Cl 144.7(2) . . ? C21 Os Cl 108.60(19) . . ? C22 Os Cl 87.33(18) . . ? C24 Os Cl 123.93(19) . . ? C23 Os Cl 95.49(19) . . ? P1 Os Cl 80.66(7) . . ? C30 P1 C32 102.5(3) . . ? C30 P1 C31 103.4(3) . . ? C32 P1 C31 103.1(4) . . ? C30 P1 Os 115.4(3) . . ? C32 P1 Os 119.2(3) . . ? C31 P1 Os 111.5(2) . . ? F2 P2 F3 90.9(3) . . ? F2 P2 F1 90.2(3) . . ? F3 P2 F1 178.2(4) . . ? F2 P2 F4 179.2(4) . . ? F3 P2 F4 89.8(4) . . ? F1 P2 F4 89.2(4) . . ? F2 P2 F6 90.9(3) . . ? F3 P2 F6 90.3(3) . . ? F1 P2 F6 91.1(3) . . ? F4 P2 F6 89.5(3) . . ? F2 P2 F5 90.6(3) . . ? F3 P2 F5 88.7(3) . . ? F1 P2 F5 89.9(3) . . ? F4 P2 F5 88.9(3) . . ? F6 P2 F5 178.1(4) . . ? C1 O C16 123.8(6) . . ? O C1 C2 109.6(5) . . ? O C1 Os 127.9(5) . . ? C2 C1 Os 121.9(5) . . ? C3 C2 C1 130.8(6) . . ? C2 C3 C4 121.1(6) . . ? C2 C3 C10 123.3(6) . . ? C4 C3 C10 115.6(5) . . ? C5 C4 C9 117.8(6) . . ? C5 C4 C3 121.2(6) . . ? C9 C4 C3 121.0(6) . . ? C6 C5 C4 121.4(7) . . ? C5 C6 C7 120.2(8) . . ? C8 C7 C6 119.3(7) . . ? C7 C8 C9 120.7(7) . . ? C8 C9 C4 120.7(7) . . ? C15 C10 C11 119.1(6) . . ? C15 C10 C3 119.3(6) . . ? C11 C10 C3 121.5(6) . . ? C12 C11 C10 119.8(7) . . ? C13 C12 C11 120.6(7) . . ? C12 C13 C14 119.5(7) . . ? C15 C14 C13 120.2(7) . . ? C10 C15 C14 120.7(7) . . ? O C16 C17' 100.7(10) . . ? O C16 C17 109.5(8) . . ? C17' C16 C17 59.0(13) . . ? C25 C20 C21 117.8(6) . . ? C25 C20 C26 120.8(7) . . ? C21 C20 C26 121.3(7) . . ? C25 C20 Os 70.3(4) . . ? C21 C20 Os 72.4(4) . . ? C26 C20 Os 130.6(5) . . ? C22 C21 C20 121.6(7) . . ? C22 C21 Os 73.1(4) . . ? C20 C21 Os 70.6(4) . . ? C21 C22 C23 118.5(7) . . ? C21 C22 C27 120.0(7) . . ? C23 C22 C27 121.5(7) . . ? C21 C22 Os 71.2(4) . . ? C23 C22 Os 73.0(4) . . ? C27 C22 Os 127.8(5) . . ? C24 C23 C22 121.9(6) . . ? C24 C23 Os 71.8(4) . . ? C22 C23 Os 70.9(4) . . ? C23 C24 C25 118.8(6) . . ? C23 C24 C28 121.0(7) . . ? C25 C24 C28 120.1(7) . . ? C23 C24 Os 73.4(4) . . ? C25 C24 Os 68.2(4) . . ? C28 C24 Os 134.0(5) . . ? C20 C25 C24 121.3(6) . . ? C20 C25 Os 72.7(4) . . ? C24 C25 Os 74.9(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 C1 Os P1 C30 39.6(3) . . . . ? C25 Os P1 C30 144.4(3) . . . . ? C20 Os P1 C30 121.0(3) . . . . ? C21 Os P1 C30 157.3(10) . . . . ? C22 Os P1 C30 -128.8(4) . . . . ? C24 Os P1 C30 -179.7(3) . . . . ? C23 Os P1 C30 -148.3(3) . . . . ? Cl Os P1 C30 -55.8(3) . . . . ? C1 Os P1 C32 -83.1(3) . . . . ? C25 Os P1 C32 21.8(3) . . . . ? C20 Os P1 C32 -1.6(4) . . . . ? C21 Os P1 C32 34.7(10) . . . . ? C22 Os P1 C32 108.6(4) . . . . ? C24 Os P1 C32 57.7(3) . . . . ? C23 Os P1 C32 89.1(3) . . . . ? Cl Os P1 C32 -178.4(3) . . . . ? C1 Os P1 C31 157.1(4) . . . . ? C25 Os P1 C31 -98.1(3) . . . . ? C20 Os P1 C31 -121.5(4) . . . . ? C21 Os P1 C31 -85.2(10) . . . . ? C22 Os P1 C31 -11.3(4) . . . . ? C24 Os P1 C31 -62.2(3) . . . . ? C23 Os P1 C31 -30.8(4) . . . . ? Cl Os P1 C31 61.7(3) . . . . ? C16 O C1 C2 -176.1(7) . . . . ? C16 O C1 Os 12.2(10) . . . . ? C25 Os C1 O 119.6(6) . . . . ? C20 Os C1 O 88.1(6) . . . . ? C21 Os C1 O 52.9(6) . . . . ? C22 Os C1 O 34.1(7) . . . . ? C24 Os C1 O 129.0(6) . . . . ? C23 Os C1 O 64.7(11) . . . . ? P1 Os C1 O -137.0(6) . . . . ? Cl Os C1 O -56.5(6) . . . . ? C25 Os C1 C2 -51.2(6) . . . . ? C20 Os C1 C2 -82.7(5) . . . . ? C21 Os C1 C2 -117.9(5) . . . . ? C22 Os C1 C2 -136.7(5) . . . . ? C24 Os C1 C2 -41.8(7) . . . . ? C23 Os C1 C2 -106.1(8) . . . . ? P1 Os C1 C2 52.2(5) . . . . ? Cl Os C1 C2 132.7(5) . . . . ? O C1 C2 C3 11.8(10) . . . . ? Os C1 C2 C3 -175.9(5) . . . . ? C1 C2 C3 C4 -176.0(6) . . . . ? C1 C2 C3 C10 7.0(11) . . . . ? C2 C3 C4 C5 21.1(9) . . . . ? C10 C3 C4 C5 -161.6(6) . . . . ? C2 C3 C4 C9 -156.8(6) . . . . ? C10 C3 C4 C9 20.4(8) . . . . ? C9 C4 C5 C6 2.0(11) . . . . ? C3 C4 C5 C6 -176.0(7) . . . . ? C4 C5 C6 C7 -1.0(13) . . . . ? C5 C6 C7 C8 0.1(14) . . . . ? C6 C7 C8 C9 -0.3(13) . . . . ? C7 C8 C9 C4 1.4(12) . . . . ? C5 C4 C9 C8 -2.2(10) . . . . ? C3 C4 C9 C8 175.8(6) . . . . ? C2 C3 C10 C15 -117.3(7) . . . . ? C4 C3 C10 C15 65.5(7) . . . . ? C2 C3 C10 C11 65.3(8) . . . . ? C4 C3 C10 C11 -111.9(7) . . . . ? C15 C10 C11 C12 1.6(9) . . . . ? C3 C10 C11 C12 179.1(6) . . . . ? C10 C11 C12 C13 0.0(10) . . . . ? C11 C12 C13 C14 -0.5(11) . . . . ? C12 C13 C14 C15 -0.7(11) . . . . ? C11 C10 C15 C14 -2.9(10) . . . . ? C3 C10 C15 C14 179.7(6) . . . . ? C13 C14 C15 C10 2.4(11) . . . . ? C1 O C16 C17' 170.5(14) . . . . ? C1 O C16 C17 109.8(12) . . . . ? C1 Os C20 C25 123.1(4) . . . . ? C21 Os C20 C25 -129.3(6) . . . . ? C22 Os C20 C25 -101.6(4) . . . . ? C24 Os C20 C25 -30.0(4) . . . . ? C23 Os C20 C25 -65.1(4) . . . . ? P1 Os C20 C25 39.8(5) . . . . ? Cl Os C20 C25 -145.6(3) . . . . ? C1 Os C20 C21 -107.6(4) . . . . ? C25 Os C20 C21 129.3(6) . . . . ? C22 Os C20 C21 27.7(4) . . . . ? C24 Os C20 C21 99.3(4) . . . . ? C23 Os C20 C21 64.2(4) . . . . ? P1 Os C20 C21 169.1(3) . . . . ? Cl Os C20 C21 -16.3(5) . . . . ? C1 Os C20 C26 8.9(8) . . . . ? C25 Os C20 C26 -114.2(9) . . . . ? C21 Os C20 C26 116.6(9) . . . . ? C22 Os C20 C26 144.2(8) . . . . ? C24 Os C20 C26 -144.2(8) . . . . ? C23 Os C20 C26 -179.3(8) . . . . ? P1 Os C20 C26 -74.4(8) . . . . ? Cl Os C20 C26 100.2(8) . . . . ? C25 C20 C21 C22 0.8(9) . . . . ? C26 C20 C21 C22 177.9(6) . . . . ? Os C20 C21 C22 -54.7(5) . . . . ? C25 C20 C21 Os 55.5(5) . . . . ? C26 C20 C21 Os -127.4(6) . . . . ? C1 Os C21 C22 -154.0(4) . . . . ? C25 Os C21 C22 102.7(5) . . . . ? C20 Os C21 C22 133.4(6) . . . . ? C24 Os C21 C22 65.2(4) . . . . ? C23 Os C21 C22 30.6(4) . . . . ? P1 Os C21 C22 88.9(11) . . . . ? Cl Os C21 C22 -56.4(4) . . . . ? C1 Os C21 C20 72.6(4) . . . . ? C25 Os C21 C20 -30.7(4) . . . . ? C22 Os C21 C20 -133.4(6) . . . . ? C24 Os C21 C20 -68.2(4) . . . . ? C23 Os C21 C20 -102.8(4) . . . . ? P1 Os C21 C20 -44.5(12) . . . . ? Cl Os C21 C20 170.1(3) . . . . ? C20 C21 C22 C23 -4.0(9) . . . . ? Os C21 C22 C23 -57.6(5) . . . . ? C20 C21 C22 C27 177.0(6) . . . . ? Os C21 C22 C27 123.5(6) . . . . ? C20 C21 C22 Os 53.6(5) . . . . ? C1 Os C22 C21 33.3(5) . . . . ? C25 Os C22 C21 -65.8(4) . . . . ? C20 Os C22 C21 -28.6(4) . . . . ? C24 Os C22 C21 -102.4(5) . . . . ? C23 Os C22 C21 -129.2(6) . . . . ? P1 Os C22 C21 -161.4(3) . . . . ? Cl Os C22 C21 127.8(4) . . . . ? C1 Os C22 C23 162.4(4) . . . . ? C25 Os C22 C23 63.4(4) . . . . ? C20 Os C22 C23 100.6(4) . . . . ? C21 Os C22 C23 129.2(6) . . . . ? C24 Os C22 C23 26.7(4) . . . . ? P1 Os C22 C23 -32.3(5) . . . . ? Cl Os C22 C23 -103.1(4) . . . . ? C1 Os C22 C27 -80.5(8) . . . . ? C25 Os C22 C27 -179.6(8) . . . . ? C20 Os C22 C27 -142.4(8) . . . . ? C21 Os C22 C27 -113.8(9) . . . . ? C24 Os C22 C27 143.8(8) . . . . ? C23 Os C22 C27 117.0(9) . . . . ? P1 Os C22 C27 84.7(8) . . . . ? Cl Os C22 C27 13.9(7) . . . . ? C21 C22 C23 C24 3.8(9) . . . . ? C27 C22 C23 C24 -177.2(6) . . . . ? Os C22 C23 C24 -52.8(6) . . . . ? C21 C22 C23 Os 56.7(5) . . . . ? C27 C22 C23 Os -124.4(6) . . . . ? C1 Os C23 C24 91.2(9) . . . . ? C25 Os C23 C24 30.0(4) . . . . ? C20 Os C23 C24 67.3(4) . . . . ? C21 Os C23 C24 104.3(5) . . . . ? C22 Os C23 C24 134.6(6) . . . . ? P1 Os C23 C24 -65.6(4) . . . . ? Cl Os C23 C24 -147.6(4) . . . . ? C1 Os C23 C22 -43.3(10) . . . . ? C25 Os C23 C22 -104.6(5) . . . . ? C20 Os C23 C22 -67.3(4) . . . . ? C21 Os C23 C22 -30.2(4) . . . . ? C24 Os C23 C22 -134.6(6) . . . . ? P1 Os C23 C22 159.8(4) . . . . ? Cl Os C23 C22 77.8(4) . . . . ? C22 C23 C24 C25 -0.3(9) . . . . ? Os C23 C24 C25 -52.7(5) . . . . ? C22 C23 C24 C28 -175.7(6) . . . . ? Os C23 C24 C28 131.8(6) . . . . ? C22 C23 C24 Os 52.4(6) . . . . ? C1 Os C24 C23 -146.6(4) . . . . ? C25 Os C24 C23 -131.3(6) . . . . ? C20 Os C24 C23 -101.2(4) . . . . ? C21 Os C24 C23 -63.5(4) . . . . ? C22 Os C24 C23 -27.7(4) . . . . ? P1 Os C24 C23 120.9(4) . . . . ? Cl Os C24 C23 40.0(5) . . . . ? C1 Os C24 C25 -15.3(6) . . . . ? C20 Os C24 C25 30.1(4) . . . . ? C21 Os C24 C25 67.8(4) . . . . ? C22 Os C24 C25 103.6(4) . . . . ? C23 Os C24 C25 131.3(6) . . . . ? P1 Os C24 C25 -107.8(4) . . . . ? Cl Os C24 C25 171.3(3) . . . . ? C1 Os C24 C28 96.1(8) . . . . ? C25 Os C24 C28 111.4(9) . . . . ? C20 Os C24 C28 141.6(8) . . . . ? C21 Os C24 C28 179.2(8) . . . . ? C22 Os C24 C28 -145.0(8) . . . . ? C23 Os C24 C28 -117.3(9) . . . . ? P1 Os C24 C28 3.6(7) . . . . ? Cl Os C24 C28 -77.3(8) . . . . ? C21 C20 C25 C24 2.9(9) . . . . ? C26 C20 C25 C24 -174.3(6) . . . . ? Os C20 C25 C24 59.4(5) . . . . ? C21 C20 C25 Os -56.5(5) . . . . ? C26 C20 C25 Os 126.3(6) . . . . ? C23 C24 C25 C20 -3.1(9) . . . . ? C28 C24 C25 C20 172.4(6) . . . . ? Os C24 C25 C20 -58.3(5) . . . . ? C23 C24 C25 Os 55.2(5) . . . . ? C28 C24 C25 Os -129.3(6) . . . . ? C1 Os C25 C20 -59.5(4) . . . . ? C21 Os C25 C20 30.7(4) . . . . ? C22 Os C25 C20 66.3(4) . . . . ? C24 Os C25 C20 130.4(6) . . . . ? C23 Os C25 C20 102.0(4) . . . . ? P1 Os C25 C20 -152.0(3) . . . . ? Cl Os C25 C20 108.9(6) . . . . ? C1 Os C25 C24 170.1(4) . . . . ? C20 Os C25 C24 -130.4(6) . . . . ? C21 Os C25 C24 -99.7(4) . . . . ? C22 Os C25 C24 -64.1(4) . . . . ? C23 Os C25 C24 -28.4(4) . . . . ? P1 Os C25 C24 77.6(4) . . . . ? Cl Os C25 C24 -21.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.790 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.120