# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1258 data_(2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C45 H44 Cl N O Os P2 Sn, (C H2 Cl2)' _chemical_formula_sum 'C46 H46 Cl3 N O Os P2 Sn' _chemical_formula_weight 1106.02 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 9.6249(1) _cell_length_b 12.5510(2) _cell_length_c 19.6568(3) _cell_angle_alpha 96.708(1) _cell_angle_beta 97.968(1) _cell_angle_gamma 107.02(1) _cell_volume 2217.36(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.06 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 3.714 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.3564 _exptl_absorpt_correction_T_max 0.4021 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens SMART CCD' _diffrn_measurement_method multi-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21704 _diffrn_reflns_av_R_equivalents 0.0144 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 27.45 _reflns_number_total 9612 _reflns_number_gt 9304 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+12.6327P] 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 9612 _refine_ls_number_parameters 494 _refine_ls_number_restraints 109 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.037 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os Os 0.218407(18) 0.222626(14) 0.246410(9) 0.02251(6) Uani 1 d . . . Sn Sn 0.50945(4) 0.30258(4) 0.29475(2) 0.04810(12) Uani 1 d . . . Cl1 Cl 0.6023(2) 0.29276(19) 0.41406(11) 0.0718(5) Uani 1 d . . . P1 P 0.16500(14) 0.08684(10) 0.32217(6) 0.0291(2) Uani 1 d . . . P2 P 0.23487(15) 0.34819(10) 0.16390(6) 0.0310(3) Uani 1 d . . . O1 O 0.2826(4) 0.0541(3) 0.1447(2) 0.0400(8) Uani 1 d . . . N1 N 0.1841(5) 0.3524(3) 0.3259(2) 0.0318(9) Uani 1 d . . . C1 C -0.0276(5) 0.1690(4) 0.2098(3) 0.0302(10) Uani 1 d . . . H1A H -0.0568 0.1044 0.1726 0.045 Uiso 1 calc R . . H1B H -0.0547 0.2309 0.1926 0.045 Uiso 1 calc R . . H1C H -0.0773 0.1486 0.2483 0.045 Uiso 1 calc R . . C2 C 0.2561(5) 0.1197(4) 0.1843(2) 0.0268(9) Uani 1 d . . . C3 C 0.6423(5) 0.4857(3) 0.3069(2) 0.0206(8) Uiso 1 d . . . H3A H 0.7440 0.4961 0.3274 0.031 Uiso 1 calc R . . H3B H 0.6015 0.5308 0.3370 0.031 Uiso 1 calc R . . H3C H 0.6387 0.5093 0.2616 0.031 Uiso 1 calc R . . C4 C 0.6597(8) 0.2265(8) 0.2508(5) 0.079(3) Uani 1 d . . . H4A H 0.7374 0.2845 0.2374 0.119 Uiso 1 calc R . . H4B H 0.6059 0.1705 0.2102 0.119 Uiso 1 calc R . . H4C H 0.7030 0.1904 0.2853 0.119 Uiso 1 calc R . . C5 C 0.0572(8) 0.3723(8) 0.3258(4) 0.071(2) Uani 1 d . . . H5A H -0.0226 0.3302 0.2903 0.085 Uiso 1 calc R . . C6 C 0.0330(10) 0.4518(9) 0.3748(5) 0.092(3) Uani 1 d . . . H6A H -0.0610 0.4611 0.3714 0.111 Uiso 1 calc R . . C7 C 0.1401(9) 0.5138(6) 0.4258(4) 0.0614(19) Uani 1 d . . . H7A H 0.1255 0.5678 0.4589 0.074 Uiso 1 calc R . . C8 C 0.2738(11) 0.4955(9) 0.4280(6) 0.102(4) Uani 1 d . . . H8A H 0.3544 0.5384 0.4628 0.122 Uiso 1 calc R . . C9 C 0.2904(9) 0.4137(8) 0.3789(5) 0.088(3) Uani 1 d . . . H9A H 0.3823 0.4006 0.3832 0.106 Uiso 1 calc R . . C11 C 0.3021(6) 0.0177(4) 0.3519(3) 0.0357(11) Uani 1 d . . . C12 C 0.2920(9) -0.0377(6) 0.4091(4) 0.0593(18) Uani 1 d . . . H12A H 0.2151 -0.0392 0.4341 0.071 Uiso 1 calc R . . C13 C 0.3955(11) -0.0910(8) 0.4295(4) 0.076(2) Uani 1 d . . . H13A H 0.3884 -0.1275 0.4687 0.091 Uiso 1 calc R . . C14 C 0.5063(9) -0.0910(6) 0.3937(4) 0.065(2) Uani 1 d . . . H14A H 0.5771 -0.1254 0.4087 0.078 Uiso 1 calc R . . C15 C 0.5145(8) -0.0412(6) 0.3361(4) 0.0559(17) Uani 1 d . . . H15A H 0.5895 -0.0434 0.3106 0.067 Uiso 1 calc R . . C16 C 0.4127(7) 0.0134(5) 0.3143(3) 0.0456(13) Uani 1 d . . . H16A H 0.4193 0.0472 0.2741 0.055 Uiso 1 calc R . . C21 C 0.0061(6) -0.0415(4) 0.2874(3) 0.0345(11) Uani 1 d . . . C22 C -0.0242(7) -0.0857(5) 0.2170(3) 0.0489(15) Uani 1 d . . . H22A H 0.0341 -0.0477 0.1872 0.059 Uiso 1 calc R . . C23 C -0.1391(8) -0.1851(5) 0.1895(4) 0.0547(16) Uani 1 d . . . H23A H -0.1575 -0.2139 0.1417 0.066 Uiso 1 calc R . . C24 C -0.2254(7) -0.2407(5) 0.2323(4) 0.0543(16) Uani 1 d . . . H24A H -0.3047 -0.3066 0.2138 0.065 Uiso 1 calc R . . C25 C -0.1954(8) -0.1997(7) 0.3024(4) 0.070(2) Uani 1 d . . . H25A H -0.2534 -0.2387 0.3319 0.084 Uiso 1 calc R . . C26 C -0.0799(8) -0.1009(6) 0.3301(4) 0.0568(18) Uani 1 d . . . H26A H -0.0600 -0.0742 0.3783 0.068 Uiso 1 calc R . . C31 C 0.1219(8) 0.1443(5) 0.4038(3) 0.0453(14) Uani 1 d U . . C32 C -0.0178(11) 0.1495(8) 0.4085(4) 0.072(2) Uani 1 d U . . H32A H -0.0965 0.1161 0.3708 0.087 Uiso 1 calc R . . C33 C -0.0417(14) 0.2056(10) 0.4705(5) 0.096(4) Uani 1 d U . . H33A H -0.1371 0.2083 0.4739 0.115 Uiso 1 calc R . . C34 C 0.0690(16) 0.2546(8) 0.5243(4) 0.094(4) Uani 1 d U . . H34A H 0.0509 0.2912 0.5650 0.113 Uiso 1 calc R . . C35 C 0.2087(15) 0.2520(8) 0.5203(4) 0.094(3) Uani 1 d U . . H35A H 0.2863 0.2876 0.5582 0.113 Uiso 1 calc R . . C36 C 0.2364(11) 0.1969(7) 0.4606(4) 0.073(2) Uani 1 d U . . H36A H 0.3326 0.1950 0.4584 0.087 Uiso 1 calc R . . C41 C 0.1923(8) 0.4767(4) 0.1948(3) 0.0478(15) Uani 1 d U . . C42 C 0.0476(10) 0.4822(6) 0.1817(4) 0.0626(19) Uani 1 d U . . H42A H -0.0282 0.4219 0.1531 0.075 Uiso 1 calc R . . C43 C 0.0167(14) 0.5768(7) 0.2110(5) 0.086(3) Uani 1 d U . . H43A H -0.0806 0.5796 0.2020 0.103 Uiso 1 calc R . . C44 C 0.1210(16) 0.6635(8) 0.2514(5) 0.099(4) Uani 1 d U . . H44A H 0.0974 0.7272 0.2698 0.119 Uiso 1 calc R . . C45 C 0.2598(15) 0.6607(8) 0.2661(5) 0.104(4) Uani 1 d U . . H45A H 0.3327 0.7225 0.2950 0.125 Uiso 1 calc R . . C46 C 0.2984(12) 0.5656(6) 0.2387(4) 0.086(3) Uani 1 d U . . H46A H 0.3955 0.5634 0.2504 0.103 Uiso 1 calc R . . C51 C 0.4087(7) 0.3978(5) 0.1305(3) 0.0466(15) Uani 1 d U . . C52 C 0.4579(9) 0.5059(7) 0.1120(4) 0.075(3) Uani 1 d U . . H52A H 0.4055 0.5575 0.1188 0.091 Uiso 1 calc R . . C53 C 0.5854(11) 0.5347(10) 0.0834(5) 0.099(4) Uani 1 d U . . H53A H 0.6184 0.6066 0.0707 0.119 Uiso 1 calc R . . C54 C 0.6650(10) 0.4605(11) 0.0730(4) 0.097(4) Uani 1 d U . . H54A H 0.7513 0.4819 0.0538 0.117 Uiso 1 calc R . . C55 C 0.6170(10) 0.3557(10) 0.0909(5) 0.090(3) Uani 1 d U . . H55A H 0.6703 0.3045 0.0844 0.108 Uiso 1 calc R . . C56 C 0.4871(8) 0.3249(7) 0.1192(4) 0.064(2) Uani 1 d U . . H56A H 0.4535 0.2521 0.1306 0.076 Uiso 1 calc R . . C61 C 0.1087(6) 0.2946(4) 0.0789(2) 0.0331(10) Uani 1 d . . . C62 C 0.0417(9) 0.1797(6) 0.0549(3) 0.0603(19) Uani 1 d . . . H62A H 0.0572 0.1276 0.0834 0.072 Uiso 1 calc R . . C63 C -0.0479(10) 0.1402(6) -0.0107(4) 0.070(2) Uani 1 d . . . H63A H -0.0910 0.0621 -0.0264 0.085 Uiso 1 calc R . . C64 C -0.0731(7) 0.2154(6) -0.0522(3) 0.0492(14) Uani 1 d . . . H64A H -0.1342 0.1890 -0.0963 0.059 Uiso 1 calc R . . C65 C -0.0096(9) 0.3281(6) -0.0296(3) 0.0586(18) Uani 1 d . . . H65A H -0.0268 0.3798 -0.0581 0.070 Uiso 1 calc R . . C66 C 0.0804(8) 0.3675(5) 0.0355(3) 0.0524(16) Uani 1 d . . . H66A H 0.1233 0.4458 0.0503 0.063 Uiso 1 calc R . . C70 C -0.4257(17) -0.0536(12) 0.1078(7) 0.178(9) Uani 1 d D . . H70A H -0.4847 -0.0042 0.0962 0.213 Uiso 1 calc R . . H70B H -0.3422 -0.0101 0.1447 0.213 Uiso 1 calc R . . Cl2 Cl -0.5354(4) -0.1702(4) 0.1388(3) 0.1515(16) Uani 1 d D . . Cl3 Cl -0.3599(7) -0.0938(6) 0.0357(3) 0.203(3) Uani 1 d 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 0.02135(9) 0.02110(9) 0.02337(9) 0.00417(6) 0.00219(6) 0.00476(6) Sn 0.02429(18) 0.0525(2) 0.0561(2) -0.01483(19) -0.00429(16) 0.00929(16) Cl1 0.0667(11) 0.0747(12) 0.0638(11) 0.0015(9) -0.0134(9) 0.0222(10) P1 0.0350(6) 0.0261(6) 0.0280(6) 0.0078(5) 0.0077(5) 0.0100(5) P2 0.0402(7) 0.0226(5) 0.0253(6) 0.0052(4) 0.0016(5) 0.0039(5) O1 0.041(2) 0.042(2) 0.0367(19) 0.0016(16) 0.0084(16) 0.0141(17) N1 0.037(2) 0.028(2) 0.031(2) 0.0057(16) 0.0056(17) 0.0115(17) C1 0.030(2) 0.023(2) 0.035(2) -0.0007(18) 0.0016(19) 0.0081(18) C2 0.028(2) 0.026(2) 0.026(2) 0.0012(17) 0.0058(17) 0.0073(18) C4 0.036(4) 0.095(6) 0.102(7) -0.014(5) 0.016(4) 0.022(4) C5 0.048(4) 0.095(6) 0.062(4) -0.031(4) -0.006(3) 0.035(4) C6 0.071(5) 0.131(9) 0.078(6) -0.042(6) -0.003(4) 0.065(6) C7 0.090(5) 0.055(4) 0.051(4) -0.004(3) 0.019(4) 0.042(4) C8 0.075(6) 0.089(7) 0.116(8) -0.063(6) 0.004(5) 0.024(5) C9 0.048(4) 0.090(6) 0.107(7) -0.054(5) -0.004(4) 0.026(4) C11 0.043(3) 0.027(2) 0.033(3) 0.0068(19) -0.005(2) 0.009(2) C12 0.064(4) 0.069(5) 0.052(4) 0.030(3) 0.004(3) 0.026(4) C13 0.092(6) 0.081(6) 0.063(5) 0.040(4) -0.008(4) 0.040(5) C14 0.066(5) 0.061(4) 0.068(5) 0.009(4) -0.018(4) 0.035(4) C15 0.058(4) 0.053(4) 0.059(4) -0.001(3) -0.006(3) 0.032(3) C16 0.052(3) 0.046(3) 0.043(3) 0.004(3) 0.001(3) 0.028(3) C21 0.031(2) 0.029(2) 0.048(3) 0.015(2) 0.011(2) 0.011(2) C22 0.050(3) 0.030(3) 0.057(4) 0.000(2) 0.024(3) -0.004(2) C23 0.057(4) 0.036(3) 0.061(4) -0.003(3) 0.018(3) 0.001(3) C24 0.040(3) 0.036(3) 0.079(5) 0.017(3) 0.008(3) -0.002(2) C25 0.054(4) 0.069(5) 0.072(5) 0.036(4) 0.013(4) -0.013(4) C26 0.052(4) 0.062(4) 0.047(3) 0.027(3) 0.005(3) -0.003(3) C31 0.076(4) 0.037(3) 0.037(3) 0.017(2) 0.026(3) 0.027(3) C32 0.104(6) 0.106(6) 0.049(4) 0.036(4) 0.033(4) 0.078(5) C33 0.153(9) 0.134(8) 0.073(6) 0.056(6) 0.063(6) 0.118(8) C34 0.198(12) 0.079(6) 0.048(4) 0.028(4) 0.055(6) 0.086(7) C35 0.154(10) 0.071(5) 0.051(4) -0.006(4) 0.047(6) 0.018(6) C36 0.095(6) 0.056(4) 0.048(4) -0.008(3) 0.028(4) -0.005(4) C41 0.088(5) 0.023(2) 0.030(3) 0.008(2) 0.003(3) 0.017(3) C42 0.089(5) 0.043(3) 0.070(5) 0.014(3) 0.030(4) 0.033(4) C43 0.140(9) 0.058(5) 0.082(6) 0.016(4) 0.038(6) 0.056(5) C44 0.188(12) 0.065(5) 0.061(5) 0.006(4) 0.003(6) 0.077(7) C45 0.171(11) 0.050(5) 0.069(5) -0.020(4) -0.030(6) 0.036(6) C46 0.131(8) 0.041(4) 0.065(5) -0.013(3) -0.040(5) 0.031(4) C51 0.045(3) 0.048(3) 0.027(2) 0.011(2) 0.000(2) -0.014(3) C52 0.057(4) 0.070(5) 0.072(5) 0.038(4) -0.010(4) -0.022(4) C53 0.066(5) 0.115(8) 0.079(6) 0.061(6) -0.005(5) -0.037(5) C54 0.052(5) 0.155(10) 0.051(4) 0.037(5) 0.013(4) -0.028(6) C55 0.060(5) 0.125(8) 0.069(5) 0.009(5) 0.036(4) -0.003(5) C56 0.058(4) 0.066(4) 0.058(4) 0.008(3) 0.031(3) -0.001(3) C61 0.036(3) 0.035(3) 0.025(2) 0.0060(19) 0.0024(19) 0.008(2) C62 0.089(5) 0.041(3) 0.042(3) -0.001(3) -0.019(3) 0.024(3) C63 0.099(6) 0.048(4) 0.048(4) -0.008(3) -0.027(4) 0.022(4) C64 0.051(3) 0.062(4) 0.030(3) 0.005(3) -0.003(2) 0.016(3) C65 0.071(5) 0.060(4) 0.042(3) 0.020(3) -0.007(3) 0.020(3) C66 0.065(4) 0.037(3) 0.044(3) 0.012(3) -0.009(3) 0.005(3) C70 0.170(16) 0.145(14) 0.193(17) -0.088(13) -0.033(13) 0.088(13) Cl2 0.098(2) 0.162(4) 0.213(5) 0.070(3) 0.012(3) 0.063(2) Cl3 0.199(5) 0.272(7) 0.138(4) -0.010(4) 0.060(4) 0.078(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os C2 1.823(4) . ? Os C1 2.249(5) . ? Os N1 2.251(4) . ? Os P2 2.3794(12) . ? Os P1 2.3830(12) . ? Os Sn 2.6741(4) . ? Sn C4 2.171(7) . ? Sn C3 2.245(4) . ? Sn Cl1 2.422(2) . ? P1 C31 1.832(6) . ? P1 C11 1.847(5) . ? P1 C21 1.847(5) . ? P2 C41 1.835(6) . ? P2 C51 1.846(6) . ? P2 C61 1.847(5) . ? O1 C2 1.173(6) . ? N1 C5 1.316(8) . ? N1 C9 1.335(9) . ? C5 C6 1.397(10) . ? C6 C7 1.316(11) . ? C7 C8 1.367(12) . ? C8 C9 1.384(10) . ? C11 C16 1.388(9) . ? C11 C12 1.389(8) . ? C12 C13 1.395(10) . ? C13 C14 1.358(12) . ? C14 C15 1.356(11) . ? C15 C16 1.400(8) . ? C21 C22 1.386(8) . ? C21 C26 1.387(8) . ? C22 C23 1.393(8) . ? C23 C24 1.370(9) . ? C24 C25 1.371(11) . ? C25 C26 1.392(10) . ? C31 C32 1.381(10) . ? C31 C36 1.399(11) . ? C32 C33 1.417(11) . ? C33 C34 1.335(16) . ? C34 C35 1.366(16) . ? C35 C36 1.390(10) . ? C41 C46 1.377(10) . ? C41 C42 1.404(11) . ? C42 C43 1.388(10) . ? C43 C44 1.327(15) . ? C44 C45 1.339(17) . ? C45 C46 1.421(13) . ? C51 C56 1.363(11) . ? C51 C52 1.409(9) . ? C52 C53 1.389(13) . ? C53 C54 1.384(17) . ? C54 C55 1.366(15) . ? C55 C56 1.408(10) . ? C61 C66 1.380(8) . ? C61 C62 1.390(8) . ? C62 C63 1.394(9) . ? C63 C64 1.369(10) . ? C64 C65 1.359(10) . ? C65 C66 1.387(9) . ? C70 Cl3 1.712(11) . ? C70 Cl2 1.763(13) . ? 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 C2 Os C1 97.05(19) . . ? C2 Os N1 177.05(18) . . ? C1 Os N1 85.87(16) . . ? C2 Os P2 90.21(15) . . ? C1 Os P2 86.30(13) . . ? N1 Os P2 90.34(11) . . ? C2 Os P1 89.97(15) . . ? C1 Os P1 85.51(13) . . ? N1 Os P1 89.90(11) . . ? P2 Os P1 171.77(5) . . ? C2 Os Sn 87.36(15) . . ? C1 Os Sn 175.30(12) . . ? N1 Os Sn 89.73(11) . . ? P2 Os Sn 92.08(3) . . ? P1 Os Sn 96.15(3) . . ? C4 Sn C3 99.5(3) . . ? C4 Sn Cl1 94.7(3) . . ? C3 Sn Cl1 92.17(12) . . ? C4 Sn Os 120.9(2) . . ? C3 Sn Os 123.47(11) . . ? Cl1 Sn Os 119.17(6) . . ? C31 P1 C11 103.1(3) . . ? C31 P1 C21 104.3(3) . . ? C11 P1 C21 98.4(2) . . ? C31 P1 Os 112.47(18) . . ? C11 P1 Os 120.51(18) . . ? C21 P1 Os 115.86(17) . . ? C41 P2 C51 105.3(3) . . ? C41 P2 C61 102.6(3) . . ? C51 P2 C61 97.7(2) . . ? C41 P2 Os 112.84(18) . . ? C51 P2 Os 119.1(2) . . ? C61 P2 Os 116.95(17) . . ? C5 N1 C9 114.0(6) . . ? C5 N1 Os 123.5(4) . . ? C9 N1 Os 122.6(4) . . ? O1 C2 Os 179.0(4) . . ? N1 C5 C6 124.5(7) . . ? C7 C6 C5 120.9(7) . . ? C6 C7 C8 116.6(7) . . ? C7 C8 C9 120.0(8) . . ? N1 C9 C8 124.0(8) . . ? C16 C11 C12 118.2(6) . . ? C16 C11 P1 120.2(4) . . ? C12 C11 P1 121.4(5) . . ? C11 C12 C13 120.2(7) . . ? C14 C13 C12 120.9(7) . . ? C15 C14 C13 119.7(6) . . ? C14 C15 C16 120.9(7) . . ? C11 C16 C15 120.0(6) . . ? C22 C21 C26 117.8(5) . . ? C22 C21 P1 119.8(4) . . ? C26 C21 P1 122.2(5) . . ? C21 C22 C23 121.3(6) . . ? C24 C23 C22 119.9(7) . . ? C23 C24 C25 119.7(6) . . ? C24 C25 C26 120.6(6) . . ? C21 C26 C25 120.6(7) . . ? C32 C31 C36 118.4(7) . . ? C32 C31 P1 121.7(6) . . ? C36 C31 P1 119.5(6) . . ? C31 C32 C33 119.5(9) . . ? C34 C33 C32 121.1(9) . . ? C33 C34 C35 120.4(8) . . ? C34 C35 C36 120.3(10) . . ? C35 C36 C31 120.3(10) . . ? C46 C41 C42 117.9(7) . . ? C46 C41 P2 120.4(6) . . ? C42 C41 P2 121.3(5) . . ? C43 C42 C41 119.8(8) . . ? C44 C43 C42 121.6(11) . . ? C43 C44 C45 120.4(9) . . ? C44 C45 C46 120.9(9) . . ? C41 C46 C45 119.4(10) . . ? C56 C51 C52 118.8(7) . . ? C56 C51 P2 118.9(5) . . ? C52 C51 P2 122.1(7) . . ? C53 C52 C51 118.8(10) . . ? C54 C53 C52 121.8(9) . . ? C55 C54 C53 119.3(8) . . ? C54 C55 C56 119.5(11) . . ? C51 C56 C55 121.8(8) . . ? C66 C61 C62 117.0(5) . . ? C66 C61 P2 121.1(4) . . ? C62 C61 P2 121.9(4) . . ? C61 C62 C63 121.3(6) . . ? C64 C63 C62 119.9(7) . . ? C65 C64 C63 119.8(6) . . ? C64 C65 C66 120.4(6) . . ? C61 C66 C65 121.7(6) . . ? Cl3 C70 Cl2 112.3(8) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 3.285 _refine_diff_density_min -3.515 _refine_diff_density_rms 0.130 # = END data_(3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C42 H42 O3 Os P2 Sn, (C H2 Cl2)' _chemical_formula_sum 'C43 H44 Cl2 O3 Os P2 Sn' _chemical_formula_weight 1050.51 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' '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' 'Cl' 'Cl' 0.1484 0.1585 '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 9.8497(1) _cell_length_b 11.9753(2) _cell_length_c 18.5656(3) _cell_angle_alpha 95.559(1) _cell_angle_beta 101.214(1) _cell_angle_gamma 103.598(1) _cell_volume 2064.36(5) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 6181 _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 27.40 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 3.924 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.2395 _exptl_absorpt_correction_T_max 0.8279 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens SMART CCD' _diffrn_measurement_method multi-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19303 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.40 _reflns_number_total 8834 _reflns_number_gt 7401 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+8.5675P] 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 8834 _refine_ls_number_parameters 500 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.148 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os Os 0.01646(2) 0.967257(18) 0.220818(12) 0.02102(6) Uani 1 d . . . Sn Sn -0.19736(4) 0.87358(3) 0.28383(2) 0.02988(10) Uani 1 d . . . P1 P 0.07225(14) 0.78937(11) 0.19187(8) 0.0211(3) Uani 1 d . . . P2 P -0.01318(15) 1.15688(11) 0.24449(8) 0.0226(3) Uani 1 d . . . O1 O -0.1381(5) 0.9479(4) 0.0618(2) 0.0421(11) Uani 1 d . . . O2 O 0.1325(4) 0.9816(3) 0.3356(2) 0.0296(9) Uani 1 d . . . O3 O -0.0473(5) 0.8995(4) 0.3883(2) 0.0435(11) Uani 1 d . . . C1 C -0.0780(6) 0.9555(5) 0.1234(3) 0.0285(13) Uani 1 d . . . C2 C 0.2336(6) 1.0504(5) 0.2118(3) 0.0264(12) Uani 1 d . . . H2A H 0.2325 1.0652 0.1613 0.040 Uiso 1 calc R . . H2B H 0.2954 0.9997 0.2248 0.040 Uiso 1 calc R . . H2C H 0.2695 1.1234 0.2455 0.040 Uiso 1 calc R . . C3 C 0.0847(7) 0.9491(5) 0.3902(3) 0.0332(13) Uani 1 d . . . C4 C 0.1872(8) 0.9714(6) 0.4648(3) 0.0493(18) Uani 1 d . . . H4A H 0.2829 1.0089 0.4599 0.074 Uiso 1 calc R . . H4B H 0.1874 0.8982 0.4830 0.074 Uiso 1 calc R . . H4C H 0.1574 1.0213 0.4995 0.074 Uiso 1 calc R . . C5 C -0.3023(7) 0.6926(6) 0.2873(4) 0.0459(17) Uani 1 d . . . H5A H -0.3560 0.6891 0.3260 0.069 Uiso 1 calc R . . H5B H -0.2305 0.6496 0.2976 0.069 Uiso 1 calc R . . H5C H -0.3671 0.6588 0.2397 0.069 Uiso 1 calc R . . C6 C -0.3454(7) 0.9535(6) 0.3283(4) 0.0448(16) Uani 1 d . . . H6A H -0.3812 0.9095 0.3650 0.067 Uiso 1 calc R . . H6B H -0.4250 0.9541 0.2884 0.067 Uiso 1 calc R . . H6C H -0.2963 1.0326 0.3514 0.067 Uiso 1 calc R . . C11 C 0.1350(6) 0.7234(4) 0.2727(3) 0.0258(12) Uani 1 d . . . C12 C 0.0519(7) 0.6215(5) 0.2903(3) 0.0336(14) Uani 1 d . . . H12A H -0.0378 0.5834 0.2591 0.040 Uiso 1 calc R . . C13 C 0.1019(9) 0.5769(6) 0.3538(4) 0.0454(17) Uani 1 d . . . H13A H 0.0447 0.5094 0.3654 0.054 Uiso 1 calc R . . C14 C 0.2329(8) 0.6297(6) 0.3996(4) 0.0455(18) Uani 1 d . . . H14A H 0.2665 0.5974 0.4415 0.055 Uiso 1 calc R . . C15 C 0.3160(7) 0.7313(6) 0.3836(4) 0.0424(16) Uani 1 d . . . H15A H 0.4060 0.7680 0.4149 0.051 Uiso 1 calc R . . C16 C 0.2665(6) 0.7787(5) 0.3217(3) 0.0343(14) Uani 1 d . . . H16A H 0.3218 0.8490 0.3125 0.041 Uiso 1 calc R . . C21 C 0.2133(6) 0.7970(4) 0.1382(3) 0.0251(12) Uani 1 d . . . C22 C 0.3398(6) 0.7626(5) 0.1601(3) 0.0294(12) Uani 1 d . . . H22A H 0.3554 0.7308 0.2044 0.035 Uiso 1 calc R . . C23 C 0.4421(6) 0.7745(5) 0.1177(4) 0.0345(14) Uani 1 d . . . H23A H 0.5267 0.7517 0.1336 0.041 Uiso 1 calc R . . C24 C 0.4198(7) 0.8204(5) 0.0514(4) 0.0359(14) Uani 1 d . . . H24A H 0.4901 0.8299 0.0232 0.043 Uiso 1 calc R . . C25 C 0.2935(7) 0.8520(5) 0.0273(4) 0.0372(14) Uani 1 d . . . H25A H 0.2760 0.8801 -0.0182 0.045 Uiso 1 calc R . . C26 C 0.1934(6) 0.8416(5) 0.0712(3) 0.0308(13) Uani 1 d . . . H26A H 0.1094 0.8652 0.0553 0.037 Uiso 1 calc R . . C31 C -0.0665(6) 0.6677(5) 0.1319(3) 0.0250(11) Uani 1 d . . . C32 C -0.0298(6) 0.5672(5) 0.1059(3) 0.0315(13) Uani 1 d . . . H32A H 0.0658 0.5630 0.1186 0.038 Uiso 1 calc R . . C33 C -0.1337(7) 0.4740(5) 0.0617(4) 0.0364(14) Uani 1 d . . . H33A H -0.1083 0.4068 0.0447 0.044 Uiso 1 calc R . . C34 C -0.2747(7) 0.4799(5) 0.0425(3) 0.0358(14) Uani 1 d . . . H34A H -0.3449 0.4164 0.0128 0.043 Uiso 1 calc R . . C35 C -0.3126(6) 0.5777(5) 0.0666(3) 0.0332(13) Uani 1 d . . . H35A H -0.4085 0.5809 0.0533 0.040 Uiso 1 calc R . . C36 C -0.2090(6) 0.6726(5) 0.1109(3) 0.0271(12) Uani 1 d . . . H36A H -0.2353 0.7400 0.1265 0.033 Uiso 1 calc R . . C41 C 0.1048(5) 1.2673(4) 0.2051(3) 0.0234(11) Uani 1 d . . . C42 C 0.2015(6) 1.3675(5) 0.2468(4) 0.0330(13) Uani 1 d . . . H42A H 0.2082 1.3829 0.2982 0.040 Uiso 1 calc R . . C43 C 0.2882(7) 1.4452(5) 0.2129(4) 0.0416(16) Uani 1 d . . . H43A H 0.3544 1.5117 0.2418 0.050 Uiso 1 calc R . . C44 C 0.2783(7) 1.4258(6) 0.1378(4) 0.0420(16) Uani 1 d . . . H44A H 0.3367 1.4787 0.1152 0.050 Uiso 1 calc R . . C45 C 0.1796(7) 1.3256(5) 0.0952(4) 0.0390(15) Uani 1 d . . . H45A H 0.1710 1.3121 0.0436 0.047 Uiso 1 calc R . . C46 C 0.0960(7) 1.2480(5) 0.1283(3) 0.0359(14) Uani 1 d . . . H46A H 0.0318 1.1807 0.0993 0.043 Uiso 1 calc R . . C51 C 0.0247(6) 1.2195(4) 0.3430(3) 0.0274(12) Uani 1 d . . . C52 C -0.0792(7) 1.2527(5) 0.3758(3) 0.0349(14) Uani 1 d . . . H52A H -0.1720 1.2437 0.3471 0.042 Uiso 1 calc R . . C53 C -0.0451(8) 1.2990(6) 0.4507(4) 0.0470(17) Uani 1 d . . . H53A H -0.1157 1.3210 0.4722 0.056 Uiso 1 calc R . . C54 C 0.0893(8) 1.3132(6) 0.4938(4) 0.0491(18) Uani 1 d . . . H54A H 0.1114 1.3460 0.5442 0.059 Uiso 1 calc R . . C55 C 0.1915(8) 1.2791(6) 0.4626(4) 0.0454(17) Uani 1 d . . . H55A H 0.2836 1.2876 0.4919 0.055 Uiso 1 calc R . . C56 C 0.1596(7) 1.2320(5) 0.3879(4) 0.0383(15) Uani 1 d . . . H56A H 0.2303 1.2083 0.3675 0.046 Uiso 1 calc R . . C61 C -0.1869(6) 1.1854(4) 0.2057(3) 0.0239(11) Uani 1 d . . . C62 C -0.1956(6) 1.3010(5) 0.2093(4) 0.0337(14) Uani 1 d . . . H62A H -0.1130 1.3623 0.2286 0.040 Uiso 1 calc R . . C63 C -0.3271(7) 1.3245(6) 0.1841(4) 0.0414(16) Uani 1 d . . . H63A H -0.3331 1.4019 0.1873 0.050 Uiso 1 calc R . . C64 C -0.4491(7) 1.2354(6) 0.1545(4) 0.0383(15) Uani 1 d . . . H64A H -0.5377 1.2519 0.1380 0.046 Uiso 1 calc R . . C65 C -0.4392(6) 1.1215(6) 0.1494(4) 0.0379(15) Uani 1 d . . . H65A H -0.5213 1.0606 0.1283 0.045 Uiso 1 calc R . . C66 C -0.3097(6) 1.0966(5) 0.1750(3) 0.0292(12) Uani 1 d . . . H66A H -0.3047 1.0189 0.1715 0.035 Uiso 1 calc R . . C70 C 0.531(3) 0.2991(17) 0.3467(12) 0.095(11) Uani 0.50 d PD A 1 H70A H 0.5809 0.2768 0.3090 0.114 Uiso 0.50 calc PR A 1 H70B H 0.4317 0.2933 0.3221 0.114 Uiso 0.50 calc PR A 1 Cl1 Cl 0.535(2) 0.2071(14) 0.4138(7) 0.069(2) Uani 0.50 d PD A 1 Cl2 Cl 0.6127(17) 0.4368(9) 0.3888(7) 0.198(7) Uani 0.50 d PD A 1 C71 C 0.571(4) 0.363(2) 0.3581(17) 0.134(19) Uani 0.50 d PD B 2 H71A H 0.6721 0.3906 0.3561 0.161 Uiso 0.50 calc PR B 2 H71B H 0.5132 0.3531 0.3075 0.161 Uiso 0.50 calc PR B 2 Cl3 Cl 0.5268(6) 0.4661(5) 0.4134(4) 0.0757(15) Uani 0.50 d PD B 2 Cl4 Cl 0.545(2) 0.2270(17) 0.3895(9) 0.123(6) Uani 0.50 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os 0.02131(11) 0.01851(10) 0.02353(11) 0.00194(8) 0.00620(8) 0.00524(8) Sn 0.0291(2) 0.0282(2) 0.0330(2) 0.00503(17) 0.01244(18) 0.00409(17) P1 0.0210(7) 0.0189(6) 0.0236(7) 0.0018(5) 0.0053(6) 0.0054(5) P2 0.0229(7) 0.0186(7) 0.0266(8) 0.0027(6) 0.0075(6) 0.0046(5) O1 0.054(3) 0.044(3) 0.030(3) 0.003(2) 0.004(2) 0.021(2) O2 0.033(2) 0.028(2) 0.026(2) 0.0033(17) 0.0040(17) 0.0075(17) O3 0.043(3) 0.054(3) 0.031(2) 0.010(2) 0.011(2) 0.005(2) C1 0.033(3) 0.021(3) 0.034(3) -0.001(2) 0.011(3) 0.011(2) C2 0.031(3) 0.023(3) 0.026(3) 0.002(2) 0.010(2) 0.007(2) C3 0.037(3) 0.035(3) 0.028(3) 0.004(3) 0.006(3) 0.011(3) C4 0.059(5) 0.060(5) 0.025(3) 0.006(3) 0.002(3) 0.013(4) C5 0.047(4) 0.039(4) 0.052(4) 0.011(3) 0.018(3) 0.005(3) C6 0.036(4) 0.050(4) 0.049(4) 0.003(3) 0.019(3) 0.007(3) C11 0.031(3) 0.022(3) 0.027(3) 0.005(2) 0.009(2) 0.009(2) C12 0.044(4) 0.027(3) 0.032(3) 0.000(2) 0.014(3) 0.011(3) C13 0.077(5) 0.030(3) 0.040(4) 0.011(3) 0.028(4) 0.020(3) C14 0.072(5) 0.052(4) 0.026(3) 0.010(3) 0.016(3) 0.038(4) C15 0.038(4) 0.061(4) 0.030(4) 0.006(3) 0.002(3) 0.021(3) C16 0.035(3) 0.039(3) 0.034(3) 0.009(3) 0.011(3) 0.015(3) C21 0.026(3) 0.017(3) 0.030(3) 0.000(2) 0.007(2) 0.003(2) C22 0.025(3) 0.027(3) 0.035(3) 0.002(2) 0.007(2) 0.009(2) C23 0.024(3) 0.037(3) 0.043(4) -0.004(3) 0.009(3) 0.012(3) C24 0.037(3) 0.030(3) 0.039(4) -0.004(3) 0.018(3) 0.001(3) C25 0.039(4) 0.040(4) 0.034(4) 0.005(3) 0.013(3) 0.009(3) C26 0.026(3) 0.035(3) 0.035(3) 0.005(3) 0.011(3) 0.012(3) C31 0.023(3) 0.026(3) 0.024(3) 0.002(2) 0.004(2) 0.003(2) C32 0.034(3) 0.024(3) 0.039(4) 0.000(2) 0.007(3) 0.014(3) C33 0.040(4) 0.022(3) 0.043(4) -0.003(3) 0.008(3) 0.007(3) C34 0.038(3) 0.026(3) 0.033(3) 0.001(3) 0.003(3) -0.006(3) C35 0.023(3) 0.035(3) 0.034(3) -0.004(3) -0.001(2) 0.002(2) C36 0.026(3) 0.024(3) 0.031(3) 0.000(2) 0.007(2) 0.007(2) C41 0.022(3) 0.018(3) 0.031(3) 0.005(2) 0.009(2) 0.006(2) C42 0.034(3) 0.028(3) 0.038(4) 0.003(3) 0.014(3) 0.005(3) C43 0.037(4) 0.027(3) 0.058(5) 0.013(3) 0.012(3) 0.000(3) C44 0.036(4) 0.039(4) 0.061(5) 0.028(3) 0.024(3) 0.011(3) C45 0.049(4) 0.039(4) 0.035(4) 0.014(3) 0.015(3) 0.015(3) C46 0.039(3) 0.032(3) 0.037(4) 0.011(3) 0.009(3) 0.006(3) C51 0.037(3) 0.019(3) 0.025(3) 0.004(2) 0.008(2) 0.004(2) C52 0.042(4) 0.034(3) 0.029(3) 0.005(3) 0.016(3) 0.003(3) C53 0.061(5) 0.048(4) 0.041(4) 0.006(3) 0.031(4) 0.016(4) C54 0.064(5) 0.050(4) 0.027(4) 0.003(3) 0.009(3) 0.003(4) C55 0.046(4) 0.047(4) 0.035(4) -0.002(3) 0.000(3) 0.007(3) C56 0.039(4) 0.034(3) 0.040(4) -0.001(3) 0.007(3) 0.008(3) C61 0.028(3) 0.024(3) 0.022(3) 0.005(2) 0.010(2) 0.008(2) C62 0.032(3) 0.026(3) 0.044(4) 0.007(3) 0.010(3) 0.009(3) C63 0.047(4) 0.037(4) 0.054(4) 0.019(3) 0.019(3) 0.025(3) C64 0.029(3) 0.051(4) 0.041(4) 0.013(3) 0.011(3) 0.018(3) C65 0.024(3) 0.043(4) 0.045(4) 0.002(3) 0.008(3) 0.007(3) C66 0.032(3) 0.025(3) 0.035(3) 0.009(2) 0.012(3) 0.008(2) C70 0.039(10) 0.19(3) 0.063(15) 0.077(19) 0.007(10) 0.017(16) Cl1 0.060(4) 0.080(4) 0.067(5) 0.003(3) 0.003(4) 0.028(3) Cl2 0.248(14) 0.099(7) 0.181(13) 0.052(7) -0.051(10) -0.016(8) C71 0.16(4) 0.22(5) 0.09(2) 0.02(3) 0.06(3) 0.15(4) Cl3 0.065(3) 0.070(3) 0.082(4) 0.002(3) 0.018(3) 0.001(2) Cl4 0.064(5) 0.152(14) 0.143(15) -0.037(10) 0.008(10) 0.046(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 Os C1 1.841(6) . ? Os C2 2.183(5) . ? Os O2 2.183(4) . ? Os P1 2.3606(13) . ? Os P2 2.3671(13) . ? Os Sn 2.6766(4) . ? Sn O3 2.143(4) . ? Sn C6 2.167(6) . ? Sn C5 2.183(6) . ? P1 C11 1.832(6) . ? P1 C31 1.840(5) . ? P1 C21 1.852(6) . ? P2 C51 1.840(6) . ? P2 C61 1.846(5) . ? P2 C41 1.851(5) . ? O1 C1 1.166(7) . ? O2 C3 1.256(7) . ? O3 C3 1.287(7) . ? C3 C4 1.506(8) . ? C11 C16 1.402(8) . ? C11 C12 1.407(8) . ? C12 C13 1.391(9) . ? C13 C14 1.369(10) . ? C14 C15 1.391(10) . ? C15 C16 1.385(8) . ? C21 C26 1.398(8) . ? C21 C22 1.401(7) . ? C22 C23 1.385(8) . ? C23 C24 1.394(9) . ? C24 C25 1.389(9) . ? C25 C26 1.387(8) . ? C31 C36 1.399(7) . ? C31 C32 1.404(7) . ? C32 C33 1.388(8) . ? C33 C34 1.386(9) . ? C34 C35 1.371(8) . ? C35 C36 1.399(8) . ? C41 C42 1.394(8) . ? C41 C46 1.405(8) . ? C42 C43 1.394(8) . ? C43 C44 1.370(9) . ? C44 C45 1.407(9) . ? C45 C46 1.367(8) . ? C51 C56 1.391(8) . ? C51 C52 1.400(8) . ? C52 C53 1.392(9) . ? C53 C54 1.370(10) . ? C54 C55 1.376(10) . ? C55 C56 1.391(9) . ? C61 C66 1.389(8) . ? C61 C62 1.403(7) . ? C62 C63 1.392(8) . ? C63 C64 1.382(9) . ? C64 C65 1.385(9) . ? C65 C66 1.383(8) . ? C70 Cl2 1.690(18) . ? C70 Cl1 1.742(16) . ? C71 Cl3 1.719(16) . ? C71 Cl4 1.760(18) . ? 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 C2 99.3(2) . . ? C1 Os O2 178.9(2) . . ? C2 Os O2 79.66(18) . . ? C1 Os P1 89.65(16) . . ? C2 Os P1 86.17(14) . . ? O2 Os P1 89.91(10) . . ? C1 Os P2 89.65(16) . . ? C2 Os P2 86.75(14) . . ? O2 Os P2 90.65(10) . . ? P1 Os P2 172.68(5) . . ? C1 Os Sn 101.97(18) . . ? C2 Os Sn 158.77(15) . . ? O2 Os Sn 79.12(10) . . ? P1 Os Sn 94.25(4) . . ? P2 Os Sn 93.02(4) . . ? O3 Sn C6 94.6(2) . . ? O3 Sn C5 95.8(2) . . ? C6 Sn C5 98.2(3) . . ? O3 Sn Os 89.83(12) . . ? C6 Sn Os 129.70(18) . . ? C5 Sn Os 131.22(19) . . ? C11 P1 C31 102.8(2) . . ? C11 P1 C21 104.3(2) . . ? C31 P1 C21 98.6(2) . . ? C11 P1 Os 114.62(18) . . ? C31 P1 Os 119.28(18) . . ? C21 P1 Os 114.89(17) . . ? C51 P2 C61 103.2(2) . . ? C51 P2 C41 103.1(2) . . ? C61 P2 C41 99.0(2) . . ? C51 P2 Os 115.71(17) . . ? C61 P2 Os 119.41(18) . . ? C41 P2 Os 113.90(17) . . ? C3 O2 Os 128.6(4) . . ? C3 O3 Sn 117.2(4) . . ? O1 C1 Os 179.8(6) . . ? O2 C3 O3 125.2(5) . . ? O2 C3 C4 118.4(6) . . ? O3 C3 C4 116.3(6) . . ? C16 C11 C12 117.9(5) . . ? C16 C11 P1 119.7(4) . . ? C12 C11 P1 122.3(4) . . ? C13 C12 C11 120.2(6) . . ? C14 C13 C12 121.1(6) . . ? C13 C14 C15 119.6(6) . . ? C16 C15 C14 120.2(6) . . ? C15 C16 C11 121.0(6) . . ? C26 C21 C22 117.3(5) . . ? C26 C21 P1 117.8(4) . . ? C22 C21 P1 124.8(4) . . ? C23 C22 C21 121.2(6) . . ? C22 C23 C24 120.1(5) . . ? C25 C24 C23 119.9(6) . . ? C26 C25 C24 119.2(6) . . ? C25 C26 C21 122.2(5) . . ? C36 C31 C32 118.6(5) . . ? C36 C31 P1 121.6(4) . . ? C32 C31 P1 119.8(4) . . ? C33 C32 C31 120.5(5) . . ? C34 C33 C32 119.9(5) . . ? C35 C34 C33 120.5(5) . . ? C34 C35 C36 120.2(5) . . ? C35 C36 C31 120.2(5) . . ? C42 C41 C46 118.3(5) . . ? C42 C41 P2 124.2(4) . . ? C46 C41 P2 117.5(4) . . ? C41 C42 C43 120.4(6) . . ? C44 C43 C42 120.8(6) . . ? C43 C44 C45 119.1(6) . . ? C46 C45 C44 120.4(6) . . ? C45 C46 C41 120.9(6) . . ? C56 C51 C52 118.0(5) . . ? C56 C51 P2 119.6(5) . . ? C52 C51 P2 122.4(5) . . ? C53 C52 C51 120.0(6) . . ? C54 C53 C52 121.3(6) . . ? C53 C54 C55 119.2(6) . . ? C54 C55 C56 120.5(7) . . ? C55 C56 C51 120.9(6) . . ? C66 C61 C62 119.0(5) . . ? C66 C61 P2 122.4(4) . . ? C62 C61 P2 118.6(4) . . ? C63 C62 C61 119.7(6) . . ? C64 C63 C62 120.9(6) . . ? C63 C64 C65 119.3(6) . . ? C66 C65 C64 120.6(6) . . ? C65 C66 C61 120.6(5) . . ? Cl2 C70 Cl1 108.5(14) . . ? Cl3 C71 Cl4 113.3(15) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 1.248 _refine_diff_density_min -1.216 _refine_diff_density_rms 0.149