#------------------------------------------------------------------------------ #$Date: 2016-03-21 08:19:19 +0000 (Mon, 21 Mar 2016) $ #$Revision: 178645 $ #$URL: svn://www.crystallography.net/cod/cif/4/07/56/4075660.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4075660 loop_ _publ_author_name 'Eguillor, Beatriz' 'Esteruelas, Miguel A.' 'Oliv\'an, Montserrat' 'O\~nate, Enrique' _publ_section_title ; C(sp2)−H Activation of RCHE−py (E = CH, N) and RCHCHC(O)R‘ Substrates Promoted by a Highly Unsaturated Osmium−Monohydride Complex ; _journal_issue 7 _journal_name_full Organometallics _journal_page_first 1428 _journal_paper_doi 10.1021/om049064z _journal_volume 24 _journal_year 2005 _chemical_formula_sum 'C37 H60 Cl N Os P2 Sn' _chemical_formula_weight 925.14 _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 102.092(2) _cell_angle_beta 91.235(2) _cell_angle_gamma 117.825(2) _cell_formula_units_Z 2 _cell_length_a 11.0322(12) _cell_length_b 11.7494(13) _cell_length_c 16.8982(18) _cell_measurement_reflns_used 5447 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28 _cell_measurement_theta_min 2 _cell_volume 1876.0(4) _computing_cell_refinement 'SAINT+ v. 6.1 (Bruker AXS, 2000)' _computing_data_collection 'SMART v. 5.625 (Bruker AXS, 2000)' _computing_data_reduction 'SAINT+ v. 6.1 (Bruker AXS, 2000)' _computing_molecular_graphics 'XP, SHELXTL v. 6.1 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.1 (Bruker, 2000)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.26 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.903 _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 18845 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 28.77 _diffrn_reflns_theta_min 1.24 _diffrn_standards_decay_% 'no decay' _exptl_absorpt_coefficient_mu 4.231 _exptl_absorpt_correction_T_max 0.694 _exptl_absorpt_correction_T_min 0.627 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Absorption correction performed with SADABS program. This is based on the method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33. SADABS: Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.1 (2000). ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 924 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _refine_diff_density_max 1.209 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.118 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.782 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 414 _refine_ls_number_reflns 8787 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.782 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0278 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0036P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0417 _reflns_number_gt 7162 _reflns_number_total 8787 _reflns_threshold_expression >2sigma(I) _cod_data_source_file om049064zsi20060522_040723.cif _cod_data_source_block mae114s _cod_original_sg_symbol_H-M P-1 _cod_database_code 4075660 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 H01 H 0.737(3) 0.616(3) 0.126(2) 0.030(10) Uiso 1 1 d . H02 H 0.691(4) 0.632(3) 0.196(2) 0.060(13) Uiso 1 1 d . Os Os 0.826332(15) 0.715116(13) 0.193695(9) 0.01331(4) Uani 1 1 d . Sn Sn 0.71463(2) 0.74927(2) 0.331327(14) 0.01497(6) Uani 1 1 d . Cl Cl 0.84108(9) 0.75461(8) 0.45454(5) 0.0206(2) Uani 1 1 d . P1 P 0.88047(9) 0.55152(8) 0.22225(6) 0.0159(2) Uani 1 1 d . P2 P 0.74806(10) 0.84211(8) 0.13656(6) 0.0157(2) Uani 1 1 d . N N 1.0314(3) 0.8789(2) 0.25079(17) 0.0142(6) Uani 1 1 d . C1 C 1.1293(3) 0.9132(3) 0.1994(2) 0.0155(8) Uani 1 1 d . C2 C 1.0818(4) 0.8321(3) 0.1175(2) 0.0165(8) Uani 1 1 d . H2 H 1.149(3) 0.850(3) 0.0803(18) 0.020 Uiso 1 1 d . C3 C 0.9497(4) 0.7366(3) 0.1016(2) 0.0172(8) Uani 1 1 d . H3 H 0.919(3) 0.690(3) 0.0509(19) 0.021 Uiso 1 1 d . C4 C 1.2621(3) 1.0194(3) 0.2269(2) 0.0192(8) Uani 1 1 d . H4 H 1.3262 1.0430 0.1903 0.023 Uiso 1 1 calc R C5 C 1.2993(4) 1.0893(3) 0.3068(2) 0.0206(9) Uani 1 1 d . H5 H 1.3873 1.1613 0.3250 0.025 Uiso 1 1 calc R C6 C 1.2030(4) 1.0503(3) 0.3599(2) 0.0194(8) Uani 1 1 d . H6 H 1.2258 1.0941 0.4151 0.023 Uiso 1 1 calc R C7 C 1.0728(3) 0.9458(3) 0.3300(2) 0.0168(8) Uani 1 1 d . H7 H 1.0094 0.9197 0.3667 0.020 Uiso 1 1 calc R C8 C 0.5107(4) 0.6016(3) 0.3452(2) 0.0191(8) Uani 1 1 d . C9 C 0.4200(4) 0.4994(3) 0.2801(2) 0.0224(9) Uani 1 1 d . H9 H 0.4427 0.4996 0.2274 0.027 Uiso 1 1 calc R C10 C 0.2974(4) 0.3980(3) 0.2917(2) 0.0260(9) Uani 1 1 d . H10 H 0.2380 0.3314 0.2470 0.031 Uiso 1 1 calc R C11 C 0.2620(4) 0.3943(3) 0.3694(2) 0.0274(10) Uani 1 1 d . H11 H 0.1806 0.3241 0.3774 0.033 Uiso 1 1 calc R C12 C 0.3491(4) 0.4961(3) 0.4350(2) 0.0277(9) Uani 1 1 d . H12 H 0.3250 0.4959 0.4874 0.033 Uiso 1 1 calc R C13 C 0.4720(4) 0.5985(3) 0.4230(2) 0.0237(9) Uani 1 1 d . H13 H 0.5298 0.6663 0.4677 0.028 Uiso 1 1 calc R C14 C 0.7018(4) 0.9252(3) 0.3909(2) 0.0170(8) Uani 1 1 d . C15 C 0.8151(4) 1.0405(3) 0.4384(2) 0.0203(8) Uani 1 1 d . H15 H 0.8991 1.0417 0.4477 0.024 Uiso 1 1 calc R C16 C 0.8040(4) 1.1525(3) 0.4717(2) 0.0261(9) Uani 1 1 d . H16 H 0.8807 1.2284 0.5026 0.031 Uiso 1 1 calc R C17 C 0.6808(4) 1.1528(4) 0.4596(2) 0.0309(10) Uani 1 1 d . H17 H 0.6747 1.2292 0.4815 0.037 Uiso 1 1 calc R C18 C 0.5664(4) 1.0405(4) 0.4151(2) 0.0286(10) Uani 1 1 d . H18 H 0.4824 1.0401 0.4076 0.034 Uiso 1 1 calc R C19 C 0.5768(4) 0.9276(4) 0.3814(2) 0.0236(9) Uani 1 1 d . H19 H 0.4988 0.8516 0.3518 0.028 Uiso 1 1 calc R C20 C 0.8522(4) 1.0270(3) 0.1595(2) 0.0184(8) Uani 1 1 d . H20 H 0.7950 1.0586 0.1362 0.022 Uiso 1 1 calc R C21 C 0.8838(4) 1.0900(3) 0.2515(2) 0.0235(9) Uani 1 1 d . H21A H 0.9398 1.0612 0.2767 0.035 Uiso 1 1 calc R H21B H 0.7988 1.0634 0.2745 0.035 Uiso 1 1 calc R H21C H 0.9328 1.1850 0.2610 0.035 Uiso 1 1 calc R C22 C 0.9852(4) 1.0758(3) 0.1205(2) 0.0236(9) Uani 1 1 d . H22A H 1.0387 1.1707 0.1392 0.035 Uiso 1 1 calc R H22B H 0.9625 1.0514 0.0621 0.035 Uiso 1 1 calc R H22C H 1.0381 1.0361 0.1356 0.035 Uiso 1 1 calc R C23 C 0.7337(4) 0.8028(3) 0.02266(19) 0.0182(8) Uani 1 1 d . H23 H 0.8294 0.8345 0.0113 0.022 Uiso 1 1 calc R C24 C 0.6582(4) 0.6564(3) -0.0231(2) 0.0242(9) Uani 1 1 d . H24A H 0.5604 0.6217 -0.0224 0.036 Uiso 1 1 calc R H24B H 0.6896 0.6079 0.0030 0.036 Uiso 1 1 calc R H24C H 0.6771 0.6476 -0.0785 0.036 Uiso 1 1 calc R C25 C 0.6812(4) 0.8787(3) -0.0192(2) 0.0265(9) Uani 1 1 d . H25A H 0.6955 0.8662 -0.0755 0.040 Uiso 1 1 calc R H25B H 0.7310 0.9716 0.0077 0.040 Uiso 1 1 calc R H25C H 0.5842 0.8457 -0.0159 0.040 Uiso 1 1 calc R C26 C 0.5761(3) 0.8190(3) 0.1625(2) 0.0205(8) Uani 1 1 d . H26 H 0.5784 0.8176 0.2203 0.025 Uiso 1 1 calc R C27 C 0.5356(4) 0.9255(3) 0.1570(2) 0.0315(10) Uani 1 1 d . H27A H 0.5358 0.9354 0.1021 0.047 Uiso 1 1 calc R H27B H 0.6007 1.0085 0.1935 0.047 Uiso 1 1 calc R H27C H 0.4447 0.8993 0.1722 0.047 Uiso 1 1 calc R C28 C 0.4581(3) 0.6832(3) 0.1177(2) 0.0260(9) Uani 1 1 d . H28A H 0.3764 0.6656 0.1433 0.039 Uiso 1 1 calc R H28B H 0.4835 0.6160 0.1199 0.039 Uiso 1 1 calc R H28C H 0.4400 0.6825 0.0617 0.039 Uiso 1 1 calc R C29 C 1.0235(4) 0.6157(3) 0.3075(2) 0.0208(9) Uani 1 1 d . H29 H 1.0120 0.6819 0.3478 0.025 Uiso 1 1 calc R C30 C 1.1665(4) 0.6921(3) 0.2825(2) 0.0277(9) Uani 1 1 d . H30A H 1.2308 0.7528 0.3301 0.041 Uiso 1 1 calc R H30B H 1.1614 0.7408 0.2447 0.041 Uiso 1 1 calc R H30C H 1.1971 0.6308 0.2571 0.041 Uiso 1 1 calc R C31 C 1.0285(4) 0.5193(3) 0.3552(2) 0.0298(10) Uani 1 1 d . H31A H 1.0383 0.4504 0.3187 0.045 Uiso 1 1 calc R H31B H 0.9444 0.4804 0.3786 0.045 Uiso 1 1 calc R H31C H 1.1058 0.5669 0.3979 0.045 Uiso 1 1 calc R C32 C 0.9411(4) 0.4811(3) 0.1329(2) 0.0238(9) Uani 1 1 d . H32 H 1.0226 0.5572 0.1225 0.029 Uiso 1 1 calc R C33 C 0.8398(4) 0.4188(3) 0.0526(2) 0.0321(10) Uani 1 1 d . H33A H 0.8908 0.4231 0.0070 0.048 Uiso 1 1 calc R H33B H 0.7898 0.4667 0.0506 0.048 Uiso 1 1 calc R H33C H 0.7759 0.3276 0.0503 0.048 Uiso 1 1 calc R C34 C 0.9911(4) 0.3839(3) 0.1447(2) 0.0320(10) Uani 1 1 d . H34A H 0.9165 0.3078 0.1573 0.048 Uiso 1 1 calc R H34B H 1.0661 0.4266 0.1889 0.048 Uiso 1 1 calc R H34C H 1.0223 0.3560 0.0954 0.048 Uiso 1 1 calc R C35 C 0.7447(4) 0.4004(3) 0.2479(2) 0.0216(9) Uani 1 1 d . H35 H 0.7872 0.3445 0.2520 0.026 Uiso 1 1 calc R C36 C 0.6187(4) 0.3164(3) 0.1820(2) 0.0343(11) Uani 1 1 d . H36A H 0.5479 0.2475 0.2024 0.051 Uiso 1 1 calc R H36B H 0.6450 0.2772 0.1345 0.051 Uiso 1 1 calc R H36C H 0.5840 0.3718 0.1678 0.051 Uiso 1 1 calc R C37 C 0.6962(4) 0.4261(3) 0.3298(2) 0.0302(10) Uani 1 1 d . H37A H 0.6247 0.4496 0.3233 0.045 Uiso 1 1 calc R H37B H 0.7725 0.4977 0.3680 0.045 Uiso 1 1 calc R H37C H 0.6605 0.3474 0.3498 0.045 Uiso 1 1 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os 0.01396(8) 0.01239(7) 0.01271(8) 0.00348(6) 0.00215(6) 0.00550(6) Sn 0.01377(14) 0.01591(12) 0.01387(14) 0.00412(10) 0.00250(11) 0.00587(11) Cl 0.0194(5) 0.0236(5) 0.0174(5) 0.0059(4) 0.0011(4) 0.0089(4) P1 0.0174(5) 0.0145(4) 0.0159(5) 0.0049(4) 0.0032(4) 0.0074(4) P2 0.0175(5) 0.0138(4) 0.0151(5) 0.0045(4) 0.0014(4) 0.0065(4) N 0.0161(16) 0.0133(14) 0.0170(17) 0.0065(13) 0.0064(13) 0.0089(13) C1 0.015(2) 0.0146(17) 0.025(2) 0.0122(16) 0.0061(16) 0.0110(16) C2 0.020(2) 0.0156(17) 0.020(2) 0.0093(16) 0.0089(16) 0.0108(17) C3 0.028(2) 0.0142(17) 0.0134(19) 0.0051(15) 0.0004(17) 0.0133(17) C4 0.013(2) 0.0229(19) 0.029(2) 0.0152(17) 0.0083(17) 0.0113(17) C5 0.014(2) 0.0141(17) 0.032(2) 0.0083(17) 0.0009(17) 0.0044(16) C6 0.018(2) 0.0169(18) 0.022(2) 0.0041(16) 0.0025(17) 0.0075(17) C7 0.018(2) 0.0208(18) 0.016(2) 0.0080(16) 0.0069(16) 0.0120(17) C8 0.017(2) 0.0198(18) 0.022(2) 0.0071(16) 0.0033(17) 0.0097(17) C9 0.019(2) 0.027(2) 0.021(2) 0.0046(17) 0.0036(17) 0.0120(18) C10 0.021(2) 0.023(2) 0.027(2) 0.0031(18) -0.0033(18) 0.0067(18) C11 0.015(2) 0.023(2) 0.042(3) 0.0127(19) 0.0025(19) 0.0060(18) C12 0.024(2) 0.031(2) 0.029(2) 0.0119(19) 0.0079(19) 0.0120(19) C13 0.020(2) 0.0211(19) 0.021(2) 0.0019(17) 0.0042(17) 0.0046(17) C14 0.020(2) 0.0198(18) 0.0135(19) 0.0059(15) 0.0035(16) 0.0104(17) C15 0.020(2) 0.026(2) 0.017(2) 0.0077(17) 0.0040(16) 0.0124(18) C16 0.027(2) 0.023(2) 0.023(2) 0.0021(17) -0.0021(18) 0.0089(19) C17 0.044(3) 0.030(2) 0.028(2) 0.0039(19) 0.005(2) 0.026(2) C18 0.028(2) 0.040(2) 0.027(2) 0.006(2) 0.0039(19) 0.025(2) C19 0.020(2) 0.027(2) 0.017(2) 0.0018(17) 0.0025(17) 0.0076(18) C20 0.025(2) 0.0143(17) 0.018(2) 0.0061(15) 0.0047(17) 0.0106(17) C21 0.033(2) 0.0160(18) 0.023(2) 0.0052(16) -0.0020(18) 0.0126(18) C22 0.023(2) 0.0174(18) 0.031(2) 0.0072(17) 0.0049(18) 0.0097(17) C23 0.023(2) 0.0188(18) 0.0116(19) 0.0072(15) 0.0011(16) 0.0072(17) C24 0.031(2) 0.0226(19) 0.013(2) 0.0019(16) -0.0011(17) 0.0088(18) C25 0.033(2) 0.026(2) 0.018(2) 0.0056(17) -0.0049(18) 0.0124(19) C26 0.019(2) 0.0236(19) 0.023(2) 0.0084(17) 0.0042(17) 0.0117(17) C27 0.026(2) 0.031(2) 0.044(3) 0.012(2) 0.005(2) 0.018(2) C28 0.017(2) 0.030(2) 0.028(2) 0.0086(18) 0.0041(18) 0.0087(18) C29 0.019(2) 0.0151(17) 0.028(2) 0.0045(16) -0.0019(17) 0.0085(16) C30 0.021(2) 0.029(2) 0.038(3) 0.0133(19) 0.0031(19) 0.0140(19) C31 0.027(2) 0.034(2) 0.027(2) 0.0086(19) 0.0002(19) 0.013(2) C32 0.032(2) 0.0216(19) 0.025(2) 0.0082(17) 0.0088(19) 0.0180(19) C33 0.050(3) 0.025(2) 0.022(2) 0.0060(18) 0.010(2) 0.019(2) C34 0.051(3) 0.030(2) 0.028(2) 0.0086(19) 0.014(2) 0.029(2) C35 0.022(2) 0.0168(18) 0.022(2) 0.0066(16) 0.0009(17) 0.0047(17) C36 0.025(2) 0.029(2) 0.039(3) 0.012(2) -0.001(2) 0.0039(19) C37 0.026(2) 0.028(2) 0.038(3) 0.0128(19) 0.009(2) 0.0121(19) 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' N N 0.0061 0.0033 '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' Sn Sn -0.6537 1.4246 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C3 Os N 74.68(12) C3 Os P2 85.39(9) N Os P2 97.28(7) C3 Os P1 89.07(9) N Os P1 92.50(7) P2 Os P1 167.07(3) C3 Os Sn 165.74(9) N Os Sn 91.89(7) P2 Os Sn 91.70(2) P1 Os Sn 96.43(2) C3 Os H01 76.3(13) N Os H01 151.0(13) P2 Os H01 81.3(12) P1 Os H01 86.1(12) Sn Os H01 117.1(13) C3 Os H02 133.1(16) N Os H02 152.2(16) P2 Os H02 86.5(15) P1 Os H02 88.8(15) Sn Os H02 60.4(16) H01 Os H02 56.8(17) C8 Sn C14 98.13(13) C8 Sn Cl 97.77(9) C14 Sn Cl 92.71(9) C8 Sn Os 120.80(9) C14 Sn Os 126.71(9) Cl Sn Os 114.09(2) C32 P1 C35 102.61(16) C32 P1 C29 104.20(17) C35 P1 C29 102.40(15) C32 P1 Os 110.84(11) C35 P1 Os 120.28(12) C29 P1 Os 114.70(11) C26 P2 C20 101.65(16) C26 P2 C23 106.57(16) C20 P2 C23 99.27(15) C26 P2 Os 113.90(11) C20 P2 Os 121.12(12) C23 P2 Os 112.44(11) C7 N C1 116.7(3) C7 N Os 128.1(2) C1 N Os 115.2(2) N C1 C4 121.1(3) N C1 C2 114.1(3) C4 C1 C2 124.8(3) C3 C2 C1 116.7(3) C3 C2 H2 126.8(19) C1 C2 H2 116.5(19) C2 C3 Os 119.4(3) C2 C3 H3 117(2) Os C3 H3 124(2) C5 C4 C1 120.7(3) C5 C4 H4 119.6 C1 C4 H4 119.6 C4 C5 C6 118.3(3) C4 C5 H5 120.8 C6 C5 H5 120.8 C7 C6 C5 119.0(3) C7 C6 H6 120.5 C5 C6 H6 120.5 N C7 C6 123.9(3) N C7 H7 118.0 C6 C7 H7 118.0 C9 C8 C13 117.4(3) C9 C8 Sn 122.5(3) C13 C8 Sn 119.7(3) C10 C9 C8 121.5(3) C10 C9 H9 119.2 C8 C9 H9 119.2 C9 C10 C11 120.5(3) C9 C10 H10 119.8 C11 C10 H10 119.8 C10 C11 C12 119.1(4) C10 C11 H11 120.4 C12 C11 H11 120.4 C11 C12 C13 120.3(4) C11 C12 H12 119.9 C13 C12 H12 119.8 C12 C13 C8 121.1(3) C12 C13 H13 119.4 C8 C13 H13 119.4 C15 C14 C19 117.0(3) C15 C14 Sn 123.0(3) C19 C14 Sn 119.9(3) C16 C15 C14 121.0(3) C16 C15 H15 119.5 C14 C15 H15 119.5 C17 C16 C15 120.6(4) C17 C16 H16 119.7 C15 C16 H16 119.7 C16 C17 C18 120.1(4) C16 C17 H17 119.9 C18 C17 H17 119.9 C17 C18 C19 119.6(4) C17 C18 H18 120.2 C19 C18 H18 120.2 C18 C19 C14 121.6(3) C18 C19 H19 119.2 C14 C19 H19 119.2 C21 C20 C22 110.5(3) C21 C20 P2 111.6(2) C22 C20 P2 113.5(2) C21 C20 H20 106.9 C22 C20 H20 106.9 P2 C20 H20 106.9 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 C20 C22 H22A 109.5 C20 C22 H22B 109.5 H22A C22 H22B 109.5 C20 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C24 C23 C25 108.8(3) C24 C23 P2 117.2(2) C25 C23 P2 115.7(2) C24 C23 H23 104.5 C25 C23 H23 104.5 P2 C23 H23 104.5 C23 C24 H24A 109.5 C23 C24 H24B 109.5 H24A C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C23 C25 H25A 109.5 C23 C25 H25B 109.5 H25A C25 H25B 109.5 C23 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C28 C26 C27 109.0(3) C28 C26 P2 112.3(2) C27 C26 P2 119.4(2) C28 C26 H26 104.9 C27 C26 H26 104.9 P2 C26 H26 104.9 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 C26 C28 H28A 109.5 C26 C28 H28B 109.5 H28A C28 H28B 109.5 C26 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C30 C29 C31 108.3(3) C30 C29 P1 112.8(2) C31 C29 P1 119.1(2) C30 C29 H29 105.2 C31 C29 H29 105.2 P1 C29 H29 105.2 C29 C30 H30A 109.5 C29 C30 H30B 109.5 H30A C30 H30B 109.5 C29 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C29 C31 H31A 109.5 C29 C31 H31B 109.5 H31A C31 H31B 109.5 C29 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C34 C32 C33 108.1(3) C34 C32 P1 116.7(3) C33 C32 P1 115.2(3) C34 C32 H32 105.2 C33 C32 H32 105.2 P1 C32 H32 105.2 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 C32 C34 H34A 109.5 C32 C34 H34B 109.5 H34A C34 H34B 109.5 C32 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 C37 C35 C36 109.1(3) C37 C35 P1 114.5(2) C36 C35 P1 114.1(2) C37 C35 H35 106.1 C36 C35 H35 106.1 P1 C35 H35 106.1 C35 C36 H36A 109.5 C35 C36 H36B 109.5 H36A C36 H36B 109.5 C35 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C35 C37 H37A 109.5 C35 C37 H37B 109.5 H37A C37 H37B 109.5 C35 C37 H37C 109.5 H37A C37 H37C 109.5 H37B C37 H37C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Os C3 2.068(4) Os N 2.195(3) Os P2 2.3822(9) Os P1 2.3942(9) Os Sn 2.6987(4) Os H01 1.40(3) Os H02 1.35(4) Sn C8 2.162(3) Sn C14 2.171(3) Sn Cl 2.4542(9) P1 C32 1.857(4) P1 C35 1.858(3) P1 C29 1.863(3) P2 C26 1.863(4) P2 C20 1.867(3) P2 C23 1.868(3) N C7 1.348(4) N C1 1.365(4) C1 C4 1.393(4) C1 C2 1.431(5) C2 C3 1.336(5) C2 H2 0.96(3) C3 H3 0.88(3) C4 C5 1.365(4) C4 H4 0.9300 C5 C6 1.379(4) C5 H5 0.9300 C6 C7 1.374(4) C6 H6 0.9300 C7 H7 0.9300 C8 C9 1.389(4) C8 C13 1.394(4) C9 C10 1.376(4) C9 H9 0.9300 C10 C11 1.381(5) C10 H10 0.9300 C11 C12 1.382(5) C11 H11 0.9300 C12 C13 1.385(4) C12 H12 0.9300 C13 H13 0.9300 C14 C15 1.401(4) C14 C19 1.399(5) C15 C16 1.380(4) C15 H15 0.9300 C16 C17 1.372(5) C16 H16 0.9300 C17 C18 1.375(5) C17 H17 0.9300 C18 C19 1.388(5) C18 H18 0.9300 C19 H19 0.9300 C20 C21 1.529(4) C20 C22 1.527(4) C20 H20 0.9800 C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C22 H22A 0.9600 C22 H22B 0.9600 C22 H22C 0.9600 C23 C24 1.525(4) C23 C25 1.537(4) C23 H23 0.9800 C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 C26 C28 1.525(4) C26 C27 1.530(4) C26 H26 0.9800 C27 H27A 0.9600 C27 H27B 0.9600 C27 H27C 0.9600 C28 H28A 0.9600 C28 H28B 0.9600 C28 H28C 0.9600 C29 C30 1.529(4) C29 C31 1.541(4) C29 H29 0.9800 C30 H30A 0.9600 C30 H30B 0.9600 C30 H30C 0.9600 C31 H31A 0.9600 C31 H31B 0.9600 C31 H31C 0.9600 C32 C34 1.526(4) C32 C33 1.543(5) C32 H32 0.9800 C33 H33A 0.9600 C33 H33B 0.9600 C33 H33C 0.9600 C34 H34A 0.9600 C34 H34B 0.9600 C34 H34C 0.9600 C35 C37 1.516(5) C35 C36 1.529(4) C35 H35 0.9800 C36 H36A 0.9600 C36 H36B 0.9600 C36 H36C 0.9600 C37 H37A 0.9600 C37 H37B 0.9600 C37 H37C 0.9600