# Copyright The Royal Society of Chemistry, 1998 # CCDC Number 186/1160 data_str549 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Os3H(CO)8(BINAP-H).0.5CH2Cl2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C55.50 H33 Cl O11 Os3 P2' _chemical_formula_weight 1543.81 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.610(4) _cell_length_b 10.957(2) _cell_length_c 16.186(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.97(2) _cell_angle_gamma 90.00 _cell_volume 2618.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 6.5 _cell_measurement_theta_max 11.5 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.958 _exptl_crystal_density_method ? _exptl_crystal_F_000 1458 _exptl_absorpt_coefficient_mu 7.434 _exptl_absorpt_correction_type 'empirical, psi-scans' _exptl_absorpt_correction_T_min 0.501 _exptl_absorpt_correction_T_max 0.986 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nicolet R3v/m' _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 4958 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0675 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4773 _reflns_number_observed 3857 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SHELXTL-PLUS' _computing_cell_refinement 'SHELXTL-PLUS' _computing_data_reduction 'SHELXTL-PLUS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXL-93 (Sheldrick, 1993)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0578P)^2^+54.7208P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 4769 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_obs 0.0595 _refine_ls_wR_factor_all 0.1611 _refine_ls_wR_factor_obs 0.1355 _refine_ls_goodness_of_fit_all 1.068 _refine_ls_goodness_of_fit_obs 1.025 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.025 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Os1 Os -0.30049(7) -0.1488 -0.16343(6) 0.0377(3) Uani 1 d . . Os2 Os -0.36796(8) -0.2095(2) -0.02154(7) 0.0471(3) Uani 1 d . . Os3 Os -0.34307(7) -0.40070(15) -0.13374(7) 0.0419(3) Uani 1 d . . P1 P -0.2397(4) -0.1671(6) -0.2817(4) 0.035(2) Uani 1 d . . P2 P -0.0235(5) -0.1139(7) -0.4146(4) 0.040(2) Uani 1 d . . C101 C -0.2780(16) -0.2940(26) -0.3551(14) 0.033(6) Uani 1 d . . C102 C -0.3730(20) -0.3230(35) -0.3876(20) 0.060(9) Uani 1 d . . H10A H -0.4144(20) -0.2792(35) -0.3658(20) 0.080 Uiso 1 d R . C103 C -0.4092(24) -0.4153(35) -0.4489(20) 0.070(11) Uani 1 d . . H10B H -0.4728(24) -0.4331(35) -0.4693(20) 0.080 Uiso 1 d R . C104 C -0.3480(32) -0.4789(34) -0.4763(22) 0.076(12) Uani 1 d . . H10C H -0.3709(32) -0.5434(34) -0.5177(22) 0.080 Uiso 1 d R . C105 C -0.2536(24) -0.4492(28) -0.4502(24) 0.062(9) Uani 1 d . . H10D H -0.2133(24) -0.4916(28) -0.4742(24) 0.080 Uiso 1 d R . C106 C -0.2218(14) -0.3624(29) -0.3874(15) 0.042(7) Uani 1 d . . H10E H -0.1578(14) -0.3466(29) -0.3653(15) 0.080 Uiso 1 d R . C111 C -0.2690(20) -0.0417(26) -0.3610(20) 0.044(7) Uani 1 d . . C112 C -0.2817(19) -0.0635(29) -0.4475(18) 0.047(7) Uani 1 d . . H11A H -0.2675(19) -0.1432(29) -0.4641(18) 0.080 Uiso 1 d R . C113 C -0.3093(25) 0.0308(33) -0.5099(17) 0.066(10) Uani 1 d . . H11B H -0.3223(25) 0.0131(33) -0.5708(17) 0.080 Uiso 1 d R . C114 C -0.3265(25) 0.1453(33) -0.4821(24) 0.070(11) Uani 1 d . . H11C H -0.3445(25) 0.2091(33) -0.5249(24) 0.080 Uiso 1 d R . C115 C -0.3119(26) 0.1701(32) -0.3979(20) 0.068(10) Uani 1 d . . H11D H -0.3190(26) 0.2516(32) -0.3795(20) 0.080 Uiso 1 d R . C116 C -0.2893(20) 0.0775(25) -0.3415(19) 0.046(7) Uani 1 d . . H11E H -0.2828(20) 0.0929(25) -0.2813(19) 0.080 Uiso 1 d R . C121 C 0.0990(24) -0.0914(31) -0.3840(21) 0.064(11) Uani 1 d . . C122 C 0.1385(22) 0.0275(31) -0.3620(21) 0.059(8) Uani 1 d . . H12A H 0.1011(22) 0.0974(31) -0.3634(21) 0.080 Uiso 1 d R . C123 C 0.2291(22) 0.0480(35) -0.3361(20) 0.059(8) Uiso 1 d . . H12B H 0.2569(22) 0.1272(35) -0.3257(20) 0.080 Uiso 1 d R . C124 C 0.2861(19) -0.0669(47) -0.3236(20) 0.076(13) Uani 1 d . . H12C H 0.3508(19) -0.0591(47) -0.3056(20) 0.080 Uiso 1 d R . C125 C 0.2510(20) -0.1802(34) -0.3393(21) 0.064(10) Uani 1 d . . H12D H 0.2879(20) -0.2523(34) -0.3273(21) 0.080 Uiso 1 d R . C126 C 0.1591(27) -0.1841(33) -0.3698(19) 0.072(11) Uani 1 d . . H12E H 0.1325(27) -0.2635(33) -0.3848(19) 0.080 Uiso 1 d R . C131 C -0.0594(17) -0.0710(23) -0.5310(14) 0.033(6) Uani 1 d . . C132 C -0.1300(23) -0.1390(41) -0.5861(18) 0.069(9) Uani 1 d . . H13A H -0.1588(23) -0.1988(41) -0.5607(18) 0.080 Uiso 1 d R . C133 C -0.1608(32) -0.1210(45) -0.6771(22) 0.095(15) Uani 1 d . . H13B H -0.2108(32) -0.1672(45) -0.7142(22) 0.080 Uiso 1 d R . C134 C -0.1141(34) -0.0353(37) -0.7095(29) 0.091(14) Uani 1 d . . H13C H -0.1328(34) -0.0205(37) -0.7713(29) 0.080 Uiso 1 d R . C135 C -0.0419(22) 0.0241(35) -0.6559(21) 0.060(9) Uani 1 d . . H13D H -0.0144(22) 0.0878(35) -0.6794(21) 0.080 Uiso 1 d R . C136 C -0.0131(22) 0.0016(30) -0.5687(16) 0.055(9) Uani 1 d . . H13E H 0.0444(22) 0.0345(30) -0.5342(16) 0.080 Uiso 1 d R . C201 C -0.1151(16) -0.2003(26) -0.2392(14) 0.032(5) Uani 1 d . . C202 C -0.0958(15) -0.3145(20) -0.1954(13) 0.025(5) Uani 1 d . . H20A H -0.1441(15) -0.3693(20) -0.1962(13) 0.080 Uiso 1 d R . C203 C -0.0121(16) -0.3460(25) -0.1529(15) 0.035(5) Uiso 1 d . . H20B H 0.0012(16) -0.4230(25) -0.1231(15) 0.080 Uiso 1 d R . C204 C 0.0615(16) -0.2639(26) -0.1475(14) 0.037(6) Uani 1 d . . C205 C 0.1546(17) -0.3051(23) -0.1034(15) 0.039(6) Uani 1 d . . H20C H 0.1661(17) -0.3861(23) -0.0798(15) 0.080 Uiso 1 d R . C206 C 0.2209(18) -0.2209(35) -0.0945(19) 0.056(9) Uani 1 d . . H20D H 0.2823(18) -0.2439(35) -0.0635(19) 0.080 Uiso 1 d R . C207 C 0.2021(18) -0.1043(32) -0.1331(16) 0.047(7) Uani 1 d . . H20E H 0.2505(18) -0.0472(32) -0.1264(16) 0.080 Uiso 1 d R . C208 C 0.1197(17) -0.0742(25) -0.1763(16) 0.038(6) Uani 1 d . . H20F H 0.1095(17) 0.0055(25) -0.2022(16) 0.080 Uiso 1 d R . C209 C 0.0448(14) -0.1498(24) -0.1867(13) 0.027(4) Uiso 1 d . . C210 C -0.0446(14) -0.1172(20) -0.2346(15) 0.028(5) Uani 1 d . . C211 C -0.0581(18) 0.0158(23) -0.3648(16) 0.037(6) Uani 1 d . . C212 C -0.0692(21) 0.1373(28) -0.4015(18) 0.051(7) Uani 1 d . . H21A H -0.0668(21) 0.1494(28) -0.4594(18) 0.080 Uiso 1 d R . C213 C -0.0869(19) 0.2330(25) -0.3579(17) 0.040(6) Uani 1 d . . H21B H -0.1038(19) 0.3093(25) -0.3880(17) 0.080 Uiso 1 d R . C214 C -0.0818(18) 0.2249(26) -0.2710(19) 0.041(6) Uani 1 d . . C215 C -0.0928(27) 0.3315(33) -0.2238(21) 0.068(10) Uani 1 d . . H21C H -0.1048(27) 0.4094(33) -0.2524(21) 0.080 Uiso 1 d R . C216 C -0.0891(20) 0.3209(37) -0.1378(22) 0.069(12) Uani 1 d . . H21D H -0.0976(20) 0.3910(37) -0.1058(22) 0.080 Uiso 1 d R . C217 C -0.0756(22) 0.2057(27) -0.0974(21) 0.052(7) Uani 1 d . . H21E H -0.0675(22) 0.2022(27) -0.0360(21) 0.080 Uiso 1 d R . C218 C -0.0675(17) 0.0988(37) -0.1415(18) 0.051(8) Uani 1 d . . H21F H -0.0599(17) 0.0206(37) -0.1132(18) 0.080 Uiso 1 d R . C219 C -0.0714(16) 0.1090(25) -0.2318(13) 0.031(5) Uani 1 d . . C220 C -0.0624(15) 0.0070(24) -0.2796(12) 0.028(5) Uani 1 d . . C11 C -0.1836(18) -0.1606(31) -0.0790(17) 0.045(7) Uiso 1 d . . O11 O -0.1064(13) -0.1608(24) -0.0317(13) 0.058(6) Uani 1 d . . C12 C -0.4204(19) -0.1324(33) -0.2486(17) 0.048(7) Uiso 1 d . . O12 O -0.4860(14) -0.1048(27) -0.2999(16) 0.077(8) Uani 1 d . . C13 C -0.2942(19) 0.0144(28) -0.1343(17) 0.043(6) Uiso 1 d . . O13 O -0.2987(21) 0.1206(22) -0.1197(18) 0.090(9) Uani 1 d . . C21 C -0.2456(21) -0.2355(30) 0.0564(19) 0.051(8) Uiso 1 d . . O21 O -0.1774(17) -0.2534(25) 0.1106(14) 0.071(7) Uani 1 d . . C22 C -0.4858(21) -0.1858(32) -0.1064(19) 0.055(8) Uiso 1 d . . O22 O -0.5597(13) -0.1636(39) -0.1456(15) 0.098(12) Uani 1 d . . C23 C -0.3713(25) -0.0519(37) 0.0343(23) 0.067(9) Uiso 1 d . . O23 O -0.3765(21) 0.0383(28) 0.0633(23) 0.111(12) Uani 1 d . . C24 C -0.4168(28) -0.3068(41) 0.0439(26) 0.076(11) Uiso 1 d . . O24 O -0.4447(27) -0.3726(33) 0.0862(19) 0.123(14) Uani 1 d . . C31 C -0.2149(19) -0.4147(30) -0.0562(17) 0.044(7) Uiso 1 d . . O31 O -0.1403(13) -0.4298(22) -0.0164(13) 0.057(6) Uani 1 d . . C32 C -0.4654(20) -0.3658(29) -0.2199(19) 0.049(7) Uiso 1 d . . O32 O -0.5303(15) -0.3585(25) -0.2699(16) 0.081(8) Uani 1 d . . C33 C -0.3864(22) -0.5243(33) -0.0752(20) 0.057(8) Uiso 1 d . . O33 O -0.4130(19) -0.5974(26) -0.0383(17) 0.083(8) Uani 1 d . . C34 C -0.3152(22) -0.5054(33) -0.2189(21) 0.057(8) Uiso 1 d . . O34 O -0.2967(17) -0.5717(23) -0.2620(15) 0.071(7) Uani 1 d . . Cl1S Cl -0.5971 -0.6625 -0.2483 0.116(6) Uiso 0.50 d P . Cl2S Cl -0.5329 -0.7899 -0.3515 0.116(6) Uiso 0.25 d P . Cl3S Cl -0.5167 -0.6816 -0.3827 0.116(6) Uiso 0.25 d P . C1S C -0.5170 -0.7680 -0.2522 0.049(21) Uiso 0.25 d P . C2S C -0.4892 -0.8071 -0.2778 0.049(21) Uiso 0.25 d P . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0355(5) 0.0418(6) 0.0395(5) 0.0001(5) 0.0172(4) 0.0023(5) Os2 0.0492(6) 0.0543(7) 0.0456(6) -0.0021(6) 0.0261(5) 0.0022(6) Os3 0.0415(6) 0.0440(6) 0.0434(6) 0.0004(5) 0.0182(5) -0.0011(5) P1 0.030(3) 0.038(4) 0.038(3) 0.005(3) 0.011(2) -0.006(3) P2 0.048(4) 0.038(4) 0.040(3) -0.003(3) 0.023(3) 0.001(3) C101 0.026(12) 0.051(17) 0.020(11) -0.010(11) 0.004(9) -0.008(12) C102 0.048(17) 0.081(25) 0.067(18) 0.009(18) 0.040(15) 0.022(18) C103 0.072(21) 0.076(26) 0.065(19) -0.035(19) 0.027(17) -0.051(21) C104 0.143(39) 0.046(21) 0.058(19) -0.008(16) 0.057(24) -0.001(23) C105 0.079(23) 0.032(15) 0.103(25) -0.030(17) 0.068(21) -0.021(16) C106 0.012(10) 0.077(22) 0.036(12) 0.005(13) 0.010(9) -0.003(12) C111 0.049(16) 0.036(16) 0.069(18) -0.004(14) 0.050(15) 0.001(13) C112 0.047(16) 0.049(18) 0.045(15) -0.015(13) 0.017(13) -0.011(14) C113 0.098(26) 0.058(21) 0.023(13) 0.016(14) -0.007(14) -0.001(20) C114 0.074(23) 0.052(21) 0.074(23) 0.012(17) 0.009(18) 0.050(18) C115 0.101(27) 0.049(20) 0.053(18) 0.006(16) 0.025(18) 0.044(20) C116 0.054(17) 0.034(17) 0.052(16) -0.008(12) 0.018(13) 0.012(13) C121 0.088(24) 0.061(21) 0.068(19) 0.027(17) 0.058(19) 0.062(20) C122 0.059(19) 0.042(19) 0.072(20) 0.007(16) 0.017(16) 0.002(16) C124 0.020(14) 0.156(44) 0.049(17) -0.001(22) 0.008(12) -0.017(20) C125 0.034(16) 0.074(28) 0.074(21) 0.022(18) 0.005(15) 0.024(17) C126 0.111(30) 0.059(24) 0.049(17) -0.010(15) 0.030(19) 0.042(21) C131 0.051(14) 0.032(13) 0.029(11) -0.004(10) 0.032(11) -0.012(12) C132 0.077(22) 0.084(25) 0.039(14) -0.023(19) 0.008(14) -0.012(23) C133 0.121(34) 0.099(36) 0.044(17) 0.007(21) -0.003(20) -0.043(30) C134 0.129(39) 0.050(23) 0.081(26) 0.017(21) 0.017(27) 0.015(25) C135 0.057(19) 0.066(23) 0.064(19) 0.021(18) 0.030(16) 0.016(18) C136 0.072(20) 0.064(21) 0.027(12) -0.004(13) 0.013(13) -0.043(17) C201 0.036(13) 0.036(13) 0.027(11) -0.006(11) 0.013(9) -0.003(12) C202 0.027(11) 0.020(11) 0.027(10) 0.007(9) 0.010(9) 0.001(9) C204 0.040(14) 0.054(16) 0.019(10) 0.006(10) 0.014(9) -0.018(12) C205 0.039(14) 0.026(13) 0.036(13) 0.010(11) -0.008(11) 0.012(11) C206 0.022(12) 0.079(25) 0.060(17) -0.027(18) 0.005(12) 0.003(15) C207 0.032(14) 0.073(22) 0.038(13) 0.003(14) 0.015(11) 0.000(14) C208 0.038(13) 0.033(14) 0.038(13) -0.020(11) 0.007(11) -0.005(11) C210 0.020(10) 0.021(12) 0.041(12) 0.009(10) 0.006(9) -0.001(9) C211 0.049(15) 0.022(13) 0.041(13) 0.003(10) 0.019(12) 0.017(11) C212 0.060(18) 0.046(18) 0.044(15) 0.008(13) 0.015(14) 0.003(14) C213 0.052(17) 0.027(13) 0.040(14) 0.000(11) 0.015(12) 0.013(12) C214 0.027(13) 0.033(14) 0.061(17) 0.011(13) 0.013(12) -0.006(11) C215 0.111(30) 0.045(22) 0.061(19) 0.009(16) 0.044(20) 0.006(19) C216 0.047(17) 0.093(33) 0.076(21) -0.040(21) 0.033(16) 0.011(18) C217 0.072(21) 0.031(15) 0.066(19) -0.005(14) 0.042(16) -0.001(15) C218 0.032(13) 0.076(21) 0.051(15) -0.032(17) 0.024(12) -0.010(16) C219 0.047(14) 0.028(12) 0.022(10) -0.002(11) 0.017(10) 0.006(12) C220 0.031(12) 0.045(15) 0.007(8) -0.001(9) 0.005(8) 0.002(11) O11 0.044(11) 0.064(15) 0.062(12) 0.019(12) 0.011(9) -0.009(11) O12 0.038(11) 0.100(23) 0.087(16) 0.024(15) 0.015(11) 0.032(13) O13 0.133(24) 0.036(14) 0.098(19) -0.009(13) 0.035(17) 0.022(15) O21 0.077(17) 0.080(19) 0.045(12) -0.006(12) 0.006(11) -0.014(14) O22 0.031(11) 0.182(37) 0.081(15) 0.015(21) 0.018(10) 0.043(18) O23 0.105(22) 0.071(19) 0.185(31) -0.067(22) 0.086(22) 0.015(17) O24 0.196(36) 0.110(29) 0.098(20) 0.019(20) 0.094(24) -0.042(27) O31 0.036(10) 0.067(17) 0.066(12) -0.005(11) 0.013(9) 0.004(10) O32 0.052(13) 0.077(19) 0.086(16) -0.016(14) -0.014(12) 0.016(13) O33 0.105(20) 0.078(18) 0.080(16) 0.039(14) 0.047(16) -0.001(16) O34 0.085(17) 0.063(16) 0.073(14) -0.027(13) 0.035(13) 0.012(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C13 1.84(3) . ? Os1 C11 1.90(3) . ? Os1 C12 1.94(3) . ? Os1 P1 2.405(6) . yes Os1 Os2 2.898(2) . yes Os1 Os3 2.915(2) . yes Os2 C24 1.83(4) . ? Os2 C22 1.92(3) . ? Os2 C21 1.94(3) . ? Os2 C23 1.96(4) . ? Os2 Os3 2.880(2) . yes Os3 C33 1.90(3) . ? Os3 C34 1.95(3) . ? Os3 C31 1.99(3) . ? Os3 C32 2.00(3) . ? P1 C101 1.80(3) . yes P1 C111 1.83(3) . yes P1 C201 1.88(2) . yes P2 C211 1.80(2) . yes P2 C121 1.83(4) . yes P2 C131 1.84(2) . yes C101 C106 1.38(4) . ? C101 C102 1.44(4) . ? C102 C103 1.40(5) . ? C103 C104 1.37(5) . ? C104 C105 1.43(5) . ? C105 C106 1.36(4) . ? C111 C112 1.37(4) . ? C111 C116 1.40(4) . ? C112 C113 1.41(4) . ? C113 C114 1.39(5) . ? C114 C115 1.33(5) . ? C115 C116 1.33(4) . ? C121 C126 1.35(4) . ? C121 C122 1.43(5) . ? C122 C123 1.36(4) . ? C123 C124 1.52(6) . ? C124 C125 1.35(6) . ? C125 C126 1.36(5) . ? C131 C136 1.35(3) . ? C131 C132 1.39(4) . ? C132 C133 1.41(4) . ? C133 C134 1.39(6) . ? C134 C135 1.35(5) . ? C135 C136 1.36(4) . ? C201 C210 1.41(3) . ? C201 C202 1.42(3) . ? C202 C203 1.31(3) . ? C203 C204 1.44(3) . ? C204 C209 1.39(4) . ? C204 C205 1.47(3) . ? C205 C206 1.36(4) . ? C206 C207 1.41(5) . ? C207 C208 1.29(4) . ? C208 C209 1.40(3) . ? C209 C210 1.40(3) . ? C210 C220 1.53(3) . ? C211 C220 1.41(3) . ? C211 C212 1.44(4) . ? C212 C213 1.34(4) . ? C213 C214 1.39(4) . ? C214 C219 1.41(4) . ? C214 C215 1.44(5) . ? C215 C216 1.38(4) . ? C216 C217 1.41(5) . ? C217 C218 1.40(4) . ? C218 C219 1.45(3) . ? C219 C220 1.39(3) . ? C11 O11 1.20(3) . ? C12 O12 1.13(3) . ? C13 O13 1.19(4) . ? C21 O21 1.16(3) . ? C22 O22 1.15(3) . ? C23 O23 1.11(5) . ? C24 O24 1.17(5) . ? C31 O31 1.15(3) . ? C32 O32 1.07(3) . ? C33 O33 1.15(4) . ? C34 O34 1.11(4) . ? Cl1S C1S 1.7185(3) . ? Cl2S C2S 1.1802(4) . ? Cl2S Cl3S 1.3453(2) . ? Cl2S C1S 1.5630(4) . ? Cl3S C2S 2.1170(4) . ? C1S C2S 0.8129(1) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Os1 C11 85.6(13) . . ? C13 Os1 C12 92.9(14) . . ? C11 Os1 C12 178.5(16) . . ? C13 Os1 P1 106.4(9) . . ? C11 Os1 P1 91.8(8) . . ? C12 Os1 P1 88.9(8) . . ? C13 Os1 Os2 91.3(8) . . ? C11 Os1 Os2 85.7(8) . . ? C12 Os1 Os2 94.0(8) . . ? P1 Os1 Os2 161.9(2) . . ? C13 Os1 Os3 150.7(8) . . ? C11 Os1 Os3 92.0(10) . . ? C12 Os1 Os3 89.2(10) . . ? P1 Os1 Os3 102.8(2) . . yes Os2 Os1 Os3 59.40(4) . . yes C24 Os2 C22 90.6(16) . . ? C24 Os2 C21 92.6(16) . . ? C22 Os2 C21 175.5(13) . . ? C24 Os2 C23 99.7(17) . . ? C22 Os2 C23 92.7(15) . . ? C21 Os2 C23 89.9(14) . . ? C24 Os2 Os3 96.2(13) . . ? C22 Os2 Os3 86.6(10) . . ? C21 Os2 Os3 89.8(9) . . ? C23 Os2 Os3 164.1(11) . . ? C24 Os2 Os1 156.5(13) . . ? C22 Os2 Os1 85.0(9) . . ? C21 Os2 Os1 90.8(9) . . ? C23 Os2 Os1 103.5(11) . . ? Os3 Os2 Os1 60.60(4) . . yes C33 Os3 C34 97.5(14) . . ? C33 Os3 C31 94.5(13) . . ? C34 Os3 C31 89.5(12) . . ? C33 Os3 C32 94.0(13) . . ? C34 Os3 C32 90.1(13) . . ? C31 Os3 C32 171.5(13) . . ? C33 Os3 Os2 93.5(10) . . ? C34 Os3 Os2 168.9(10) . . ? C31 Os3 Os2 88.4(8) . . ? C32 Os3 Os2 90.4(9) . . ? C33 Os3 Os1 153.5(10) . . ? C34 Os3 Os1 109.0(10) . . ? C31 Os3 Os1 86.6(9) . . ? C32 Os3 Os1 85.5(9) . . ? Os2 Os3 Os1 60.00(4) . . ? C101 P1 C111 99.4(12) . . yes C101 P1 C201 100.0(12) . . yes C111 P1 C201 113.3(12) . . yes C101 P1 Os1 117.2(8) . . yes C111 P1 Os1 114.9(8) . . yes C201 P1 Os1 110.8(7) . . ? C211 P2 C121 102.2(14) . . yes C211 P2 C131 102.7(11) . . yes C121 P2 C131 100.7(12) . . yes C106 C101 C102 116.7(24) . . ? C106 C101 P1 123.6(19) . . ? C102 C101 P1 119.6(21) . . ? C103 C102 C101 123.3(28) . . ? C104 C103 C102 115.7(32) . . ? C103 C104 C105 123.2(31) . . ? C106 C105 C104 118.0(26) . . ? C105 C106 C101 122.6(23) . . ? C112 C111 C116 115.0(29) . . ? C112 C111 P1 120.4(23) . . ? C116 C111 P1 124.3(22) . . ? C111 C112 C113 120.9(29) . . ? C114 C113 C112 118.5(27) . . ? C115 C114 C113 121.8(30) . . ? C116 C115 C114 117.7(31) . . ? C115 C116 C111 125.6(28) . . ? C126 C121 C122 114.9(34) . . ? C126 C121 P2 123.5(32) . . ? C122 C121 P2 121.1(21) . . ? C123 C122 C121 123.2(32) . . ? C122 C123 C124 114.2(33) . . ? C125 C124 C123 123.7(25) . . ? C124 C125 C126 114.5(30) . . ? C121 C126 C125 129.1(38) . . ? C136 C131 C132 117.2(24) . . ? C136 C131 P2 125.7(20) . . ? C132 C131 P2 115.7(21) . . ? C131 C132 C133 121.8(36) . . ? C134 C133 C132 116.5(38) . . ? C135 C134 C133 121.0(37) . . ? C134 C135 C136 120.5(34) . . ? C131 C136 C135 122.2(28) . . ? C210 C201 C202 120.4(21) . . ? C210 C201 P1 126.3(20) . . ? C202 C201 P1 112.3(17) . . ? C203 C202 C201 120.5(22) . . ? C202 C203 C204 120.5(24) . . ? C209 C204 C203 120.5(23) . . ? C209 C204 C205 120.7(21) . . ? C203 C204 C205 118.8(23) . . ? C206 C205 C204 116.3(24) . . ? C205 C206 C207 121.7(24) . . ? C208 C207 C206 119.9(28) . . ? C207 C208 C209 124.2(28) . . ? C204 C209 C208 116.9(21) . . ? C204 C209 C210 119.2(21) . . ? C208 C209 C210 123.9(24) . . ? C209 C210 C201 118.9(21) . . ? C209 C210 C220 119.1(20) . . ? C201 C210 C220 122.1(20) . . ? C220 C211 C212 115.4(23) . . ? C220 C211 P2 120.1(19) . . ? C212 C211 P2 123.8(19) . . ? C213 C212 C211 121.5(24) . . ? C212 C213 C214 122.0(27) . . ? C213 C214 C219 118.5(26) . . ? C213 C214 C215 120.7(26) . . ? C219 C214 C215 120.7(25) . . ? C216 C215 C214 119.7(32) . . ? C215 C216 C217 119.8(30) . . ? C216 C217 C218 122.6(28) . . ? C217 C218 C219 118.0(33) . . ? C220 C219 C214 119.5(20) . . ? C220 C219 C218 121.3(26) . . ? C214 C219 C218 119.2(26) . . ? C219 C220 C211 122.4(23) . . ? C219 C220 C210 119.1(18) . . ? C211 C220 C210 118.1(21) . . ? O11 C11 Os1 172.9(24) . . ? O12 C12 Os1 169.2(32) . . ? O13 C13 Os1 173.9(29) . . ? O21 C21 Os2 171.8(27) . . ? O22 C22 Os2 168.6(28) . . ? O23 C23 Os2 177.2(38) . . ? O24 C24 Os2 176.9(40) . . ? O31 C31 Os3 174.2(26) . . ? O32 C32 Os3 172.5(29) . . ? O33 C33 Os3 178.4(30) . . ? O34 C34 Os3 174.3(30) . . ? C2S Cl2S Cl3S 113.754(9) . . ? C2S Cl2S C1S 30.615(10) . . ? Cl3S Cl2S C1S 105.322(10) . . ? Cl2S Cl3S C2S 30.680(7) . . ? C2S C1S Cl2S 47.679(13) . . ? C2S C1S Cl1S 152.667(8) . . ? Cl2S C1S Cl1S 105.51(2) . . ? C1S C2S Cl2S 101.71(2) . . ? C1S C2S Cl3S 93.69(2) . . ? Cl2S C2S Cl3S 35.566(8) . . ? _refine_diff_density_max 1.369 _refine_diff_density_min -1.383 _refine_diff_density_rms 0.251 #===END data_str599 _audit_creation_method SHELXL _chemical_name_systematic ; (orthometallated BINAP)hydridooctacarbonyltriosmium ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural Os3H(BINAP-H)(CO)8 _chemical_formula_analytical ? _chemical_formula_sum 'C52 H32 O8 Os3 P2' _chemical_formula_weight 1417.32 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.661(4) _cell_length_b 21.265(16) _cell_length_c 24.214(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5489(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16 _cell_measurement_theta_max 27 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method ? _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 7.032 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.728 _exptl_absorpt_correction_T_max 0.930 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nicolet 3v/m' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5266 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5266 _reflns_number_observed 4231 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SHELXTL-PLUS' _computing_cell_refinement 'SHELXTL-PLUS' _computing_data_reduction 'SHELXTL-PLUS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0866P)^2^+478.4703P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_ls_number_reflns 5259 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1131 _refine_ls_R_factor_obs 0.0891 _refine_ls_wR_factor_all 0.2727 _refine_ls_wR_factor_obs 0.2411 _refine_ls_goodness_of_fit_all 1.075 _refine_ls_goodness_of_fit_obs 1.115 _refine_ls_restrained_S_all 1.128 _refine_ls_restrained_S_obs 1.115 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Os1 Os -0.70137(15) -0.69026(7) -0.05697(6) 0.0370(4) Uani 1 d . . Os2 Os -0.86286(13) -0.67962(7) -0.15210(6) 0.0333(4) Uani 1 d . . Os3 Os -0.57981(14) -0.70258(7) -0.15887(7) 0.0389(4) Uani 1 d . . P1 P -0.8039(9) -0.5740(4) -0.1290(4) 0.035(2) Uani 1 d . . P2 P -0.9613(10) -0.6492(5) -0.2362(4) 0.034(2) Uani 1 d . . C101 C -0.5611(31) -0.6249(15) -0.1050(13) 0.022(7) Uiso 1 d . . C102 C -0.4328(39) -0.6074(18) -0.0829(16) 0.039(9) Uiso 1 d . . H10A H -0.3621(39) -0.6294(18) -0.0981(16) 0.080 Uiso 1 d R . C103 C -0.4106(57) -0.5635(24) -0.0432(21) 0.066(14) Uiso 1 d . . H10B H -0.3264(57) -0.5539(24) -0.0319(21) 0.080 Uiso 1 d R . C104 C -0.5257(45) -0.5275(22) -0.0172(19) 0.051(11) Uiso 1 d . . H10C H -0.5157(45) -0.5024(22) 0.0154(19) 0.080 Uiso 1 d R . C105 C -0.6370(47) -0.5340(21) -0.0404(18) 0.050(11) Uiso 1 d . . H10D H -0.7056(47) -0.5082(21) -0.0282(18) 0.080 Uiso 1 d R . C106 C -0.6593(33) -0.5821(16) -0.0867(14) 0.029(8) Uiso 1 d . . C111 C -0.9020(45) -0.5206(21) -0.0911(18) 0.048(10) Uiso 1 d . . C112 C -0.8622(46) -0.4532(20) -0.0908(18) 0.049(10) Uiso 1 d . . H11A H -0.7914(46) -0.4411(20) -0.1129(18) 0.080 Uiso 1 d R . C113 C -0.9266(62) -0.4044(29) -0.0565(25) 0.081(16) Uiso 1 d . . H11B H -0.8997(62) -0.3614(29) -0.0545(25) 0.080 Uiso 1 d R . C114 C -1.0238(66) -0.4272(32) -0.0308(28) 0.089(19) Uiso 1 d . . H11C H -1.0692(66) -0.3968(32) -0.0094(28) 0.080 Uiso 1 d R . C115 C -1.0673(73) -0.4848(32) -0.0293(29) 0.095(20) Uiso 1 d . . H11D H -1.1418(73) -0.4952(32) -0.0090(29) 0.080 Uiso 1 d R . C116 C -1.0017(50) -0.5304(25) -0.0582(22) 0.062(13) Uiso 1 d . . H11E H -1.0297(50) -0.5731(25) -0.0548(22) 0.080 Uiso 1 d R . C121 C -0.8657(41) -0.6418(18) -0.2986(16) 0.040(9) Uiso 1 d . . C122 C -0.7627(47) -0.6779(24) -0.3052(21) 0.061(13) Uiso 1 d . . H12A H -0.7409(47) -0.7060(24) -0.2757(21) 0.080 Uiso 1 d R . C123 C -0.6918(61) -0.6766(29) -0.3509(25) 0.086(17) Uiso 1 d . . H12B H -0.6221(61) -0.7047(29) -0.3554(25) 0.080 Uiso 1 d R . C124 C -0.7164(75) -0.6289(33) -0.3947(29) 0.097(21) Uiso 1 d . . H12C H -0.6651(75) -0.6252(33) -0.4271(29) 0.080 Uiso 1 d R . C125 C -0.8260(49) -0.5907(24) -0.3887(21) 0.060(13) Uiso 1 d . . H12D H -0.8537(49) -0.5622(24) -0.4170(21) 0.080 Uiso 1 d R . C126 C -0.8876(44) -0.5956(21) -0.3385(19) 0.054(11) Uiso 1 d . . H12E H -0.9502(44) -0.5647(21) -0.3298(19) 0.080 Uiso 1 d R . C131 C -1.0839(38) -0.7043(18) -0.2617(15) 0.039(8) Uiso 1 d . . C132 C -1.1455(37) -0.7474(18) -0.2280(16) 0.038(9) Uiso 1 d . . H13A H -1.1271(37) -0.7468(18) -0.1892(16) 0.080 Uiso 1 d R . C133 C -1.2355(47) -0.7888(25) -0.2489(21) 0.062(13) Uiso 1 d . . H13B H -1.2623(47) -0.8238(25) -0.2269(21) 0.080 Uiso 1 d R . C134 C -1.2855(53) -0.7786(25) -0.3028(21) 0.065(13) Uiso 1 d . . H13C H -1.3563(53) -0.8024(25) -0.3157(21) 0.080 Uiso 1 d R . C135 C -1.2299(53) -0.7340(26) -0.3371(24) 0.072(15) Uiso 1 d . . H13D H -1.2595(53) -0.7274(26) -0.3741(24) 0.080 Uiso 1 d R . C136 C -1.1314(42) -0.6988(20) -0.3164(17) 0.047(10) Uiso 1 d . . H13E H -1.0914(42) -0.6692(20) -0.3406(17) 0.080 Uiso 1 d R . C201 C -0.7605(39) -0.5274(19) -0.1903(17) 0.040(9) Uiso 1 d . . C202 C -0.6341(44) -0.5109(19) -0.1991(18) 0.045(10) Uiso 1 d . . H20A H -0.5748(44) -0.5206(19) -0.1705(18) 0.080 Uiso 1 d R . C203 C -0.5898(41) -0.4804(18) -0.2481(16) 0.038(9) Uiso 1 d . . H20B H -0.5024(41) -0.4724(18) -0.2546(16) 0.080 Uiso 1 d R . C204 C -0.6817(44) -0.4610(21) -0.2869(19) 0.050(11) Uiso 1 d . . C205 C -0.6428(51) -0.4310(23) -0.3409(21) 0.063(12) Uiso 1 d . . H20C H -0.5556(51) -0.4231(23) -0.3482(21) 0.080 Uiso 1 d R . C206 C -0.7270(60) -0.4113(29) -0.3779(26) 0.077(16) Uiso 1 d . . H20D H -0.6993(60) -0.3954(29) -0.4130(26) 0.080 Uiso 1 d R . C207 C -0.8561(53) -0.4163(25) -0.3668(22) 0.065(13) Uiso 1 d . . H20E H -0.9172(53) -0.3995(25) -0.3919(22) 0.080 Uiso 1 d R . C208 C -0.8931(53) -0.4456(23) -0.3179(21) 0.063(13) Uiso 1 d . . H20F H -0.9810(53) -0.4478(23) -0.3096(21) 0.080 Uiso 1 d R . C209 C -0.8065(45) -0.4727(21) -0.2769(18) 0.049(10) Uiso 1 d . . C210 C -0.8477(31) -0.5015(15) -0.2273(13) 0.025(7) Uiso 1 d . . C211 C -1.0421(32) -0.5725(16) -0.2233(14) 0.027(7) Uiso 1 d . . C212 C -1.1767(39) -0.5788(20) -0.2106(17) 0.042(9) Uiso 1 d . . H21A H -1.2165(39) -0.6191(20) -0.2140(17) 0.080 Uiso 1 d R . C213 C -1.2439(39) -0.5293(19) -0.1920(16) 0.038(9) Uiso 1 d . . H21B H -1.3311(39) -0.5354(19) -0.1836(16) 0.080 Uiso 1 d R . C214 C -1.1997(47) -0.4705(21) -0.1871(19) 0.050(11) Uiso 1 d . . C215 C -1.2658(50) -0.4164(23) -0.1715(19) 0.059(12) Uiso 1 d . . H21C H -1.3524(50) -0.4212(23) -0.1615(19) 0.080 Uiso 1 d R . C216 C -1.2124(48) -0.3575(23) -0.1683(19) 0.058(12) Uiso 1 d . . H21D H -1.2626(48) -0.3217(23) -0.1584(19) 0.080 Uiso 1 d R . C217 C -1.0894(45) -0.3502(22) -0.1799(18) 0.050(11) Uiso 1 d . . H21E H -1.0527(45) -0.3092(22) -0.1754(18) 0.080 Uiso 1 d R . C218 C -1.0132(47) -0.3985(21) -0.1986(19) 0.052(11) Uiso 1 d . . H21F H -0.9277(47) -0.3904(21) -0.2089(19) 0.080 Uiso 1 d R . C219 C -1.0637(44) -0.4607(20) -0.2012(18) 0.047(10) Uiso 1 d . . C220 C -0.9868(40) -0.5121(19) -0.2166(17) 0.040(9) Uiso 1 d . . C11 C -0.7174(39) -0.7723(19) -0.0557(17) 0.039(9) Uiso 1 d . . O11 O -0.7229(35) -0.8348(17) -0.0564(15) 0.067(9) Uiso 1 d . . C12 C -0.5834(30) -0.6954(14) 0.0013(12) 0.023(6) Uiso 1 d . . O12 O -0.5201(32) -0.6908(20) 0.0410(11) 0.074(12) Uani 1 d . . C13 C -0.8499(40) -0.6719(19) -0.0058(17) 0.041(9) Uiso 1 d . . O13 O -0.9362(30) -0.6667(19) 0.0149(12) 0.066(10) Uani 1 d . . C21 C -0.8790(33) -0.7647(16) -0.1586(15) 0.031(7) Uiso 1 d . . O21 O -0.8825(31) -0.8234(12) -0.1679(16) 0.066(10) Uani 1 d . . C22 C -1.0210(48) -0.6820(25) -0.1144(20) 0.058(12) Uiso 1 d . . O22 O -1.1113(25) -0.6788(14) -0.0916(10) 0.041(6) Uani 1 d . . C31 C -0.6063(52) -0.7803(25) -0.1941(22) 0.064(14) Uiso 1 d . . O31 O -0.6142(25) -0.8319(13) -0.2130(15) 0.058(9) Uani 1 d . . C32 C -0.4996(55) -0.6718(27) -0.2228(23) 0.070(15) Uiso 1 d . . O32 O -0.4507(32) -0.6436(19) -0.2586(14) 0.069(10) Uani 1 d . . C33 C -0.4278(52) -0.7384(24) -0.1251(21) 0.059(12) Uiso 1 d . . O33 O -0.3373(33) -0.7603(15) -0.1092(18) 0.075(12) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0339(7) 0.0373(8) 0.0398(8) 0.0048(7) -0.0036(7) -0.0028(7) Os2 0.0283(7) 0.0298(7) 0.0418(8) 0.0034(6) -0.0034(7) -0.0033(6) Os3 0.0294(7) 0.0409(8) 0.0463(9) 0.0032(7) 0.0001(7) 0.0014(7) P1 0.023(4) 0.029(5) 0.054(6) -0.001(4) 0.005(5) -0.009(4) P2 0.036(5) 0.035(5) 0.031(5) 0.008(4) 0.003(4) 0.001(4) O12 0.074(22) 0.123(31) 0.026(14) 0.001(18) -0.029(15) 0.055(24) O13 0.048(19) 0.115(31) 0.035(16) 0.003(18) -0.001(15) -0.009(20) O21 0.068(21) 0.020(13) 0.111(28) -0.019(16) 0.000(20) -0.012(14) O22 0.040(15) 0.055(16) 0.028(12) 0.012(12) 0.012(11) -0.004(14) O31 0.025(14) 0.038(16) 0.112(27) -0.033(17) -0.023(16) -0.004(12) O32 0.059(22) 0.094(27) 0.054(20) 0.002(19) 0.026(18) -0.009(20) O33 0.057(23) 0.042(18) 0.126(34) 0.008(19) -0.021(22) -0.016(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C11 1.75(4) . ? Os1 C12 1.89(3) . ? Os1 C13 2.05(4) . ? Os1 C101 2.35(3) . yes Os1 C106 2.45(3) . yes Os1 Os3 2.799(2) . yes Os1 Os2 2.885(2) . yes Os2 C21 1.82(3) . ? Os2 C22 1.92(5) . ? Os2 P2 2.380(10) . yes Os2 P1 2.399(9) . yes Os2 Os3 3.061(2) . yes Os3 C31 1.88(5) . ? Os3 C32 1.88(6) . ? Os3 C33 1.97(6) . ? Os3 C101 2.11(3) . yes P1 C111 1.80(5) . yes P1 C106 1.86(4) . yes P1 C201 1.84(4) . yes P2 C121 1.83(4) . yes P2 C131 1.86(4) . yes P2 C211 1.87(3) . yes C101 C106 1.46(5) . ? C101 C102 1.52(5) . ? C102 C103 1.36(6) . ? C103 C104 1.58(7) . ? C104 C105 1.32(6) . ? C105 C106 1.54(6) . ? C111 C116 1.34(7) . ? C111 C112 1.49(6) . ? C112 C113 1.50(7) . ? C113 C114 1.30(8) . ? C114 C115 1.31(9) . ? C115 C116 1.39(8) . ? C121 C122 1.35(6) . ? C121 C126 1.40(6) . ? C122 C123 1.34(8) . ? C123 C124 1.49(8) . ? C124 C125 1.43(8) . ? C125 C126 1.39(6) . ? C131 C132 1.39(5) . ? C131 C136 1.42(5) . ? C132 C133 1.40(6) . ? C133 C134 1.43(7) . ? C134 C135 1.39(7) . ? C135 C136 1.38(7) . ? C201 C210 1.40(5) . ? C201 C202 1.41(6) . ? C202 C203 1.43(6) . ? C203 C204 1.42(6) . ? C204 C209 1.38(6) . ? C204 C205 1.51(7) . ? C205 C206 1.34(7) . ? C206 C207 1.41(8) . ? C207 C208 1.40(7) . ? C208 C209 1.47(7) . ? C209 C210 1.42(5) . ? C210 C220 1.52(5) . ? C211 C220 1.42(5) . ? C211 C212 1.47(5) . ? C212 C213 1.35(6) . ? C213 C214 1.34(6) . ? C214 C215 1.40(6) . ? C214 C219 1.50(6) . ? C215 C216 1.38(7) . ? C216 C217 1.35(7) . ? C217 C218 1.39(6) . ? C218 C219 1.43(6) . ? C219 C220 1.42(6) . ? C11 O11 1.33(5) . ? C12 O12 1.18(4) . ? C13 O13 1.05(5) . ? C21 O21 1.27(4) . ? C22 O22 1.11(5) . ? C31 O31 1.19(6) . ? C32 O32 1.18(6) . ? C33 O33 1.14(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Os1 C12 89.7(16) . . ? C11 Os1 C13 95.9(18) . . ? C12 Os1 C13 94.2(15) . . ? C11 Os1 C101 131.2(16) . . ? C12 Os1 C101 88.9(12) . . ? C13 Os1 C101 132.8(14) . . ? C11 Os1 C106 163.1(16) . . ? C12 Os1 C106 98.7(12) . . ? C13 Os1 C106 98.1(14) . . ? C101 Os1 C106 35.2(11) . . ? C11 Os1 Os3 88.2(13) . . ? C12 Os1 Os3 110.1(9) . . ? C13 Os1 Os3 155.4(11) . . ? C101 Os1 Os3 47.5(8) . . yes C106 Os1 Os3 75.2(8) . . yes C11 Os1 Os2 92.0(13) . . ? C12 Os1 Os2 174.9(9) . . ? C13 Os1 Os2 90.4(11) . . ? C101 Os1 Os2 86.4(8) . . yes C106 Os1 Os2 78.5(8) . . yes Os3 Os1 Os2 65.15(6) . . yes C21 Os2 C22 86.1(19) . . ? C21 Os2 P2 98.9(12) . . ? C22 Os2 P2 91.5(15) . . ? C21 Os2 P1 166.8(11) . . ? C22 Os2 P1 98.3(16) . . ? P2 Os2 P1 93.5(4) . . yes C21 Os2 Os1 92.7(11) . . ? C22 Os2 Os1 98.2(14) . . ? P2 Os2 Os1 165.4(3) . . yes P1 Os2 Os1 74.4(3) . . yes C21 Os2 Os3 86.0(11) . . ? C22 Os2 Os3 152.6(15) . . ? P2 Os2 Os3 115.6(2) . . yes P1 Os2 Os3 84.5(2) . . yes Os1 Os2 Os3 56.08(5) . . yes C31 Os3 C32 90.1(24) . . ? C31 Os3 C33 88.4(22) . . ? C32 Os3 C33 95.9(23) . . ? C31 Os3 C101 168.6(18) . . ? C32 Os3 C101 101.1(19) . . ? C33 Os3 C101 88.2(17) . . ? C31 Os3 Os1 114.4(16) . . ? C32 Os3 Os1 154.3(17) . . ? C33 Os3 Os1 92.9(15) . . ? C101 Os3 Os1 55.0(8) . . yes C31 Os3 Os2 90.9(17) . . ? C32 Os3 Os2 115.8(17) . . ? C33 Os3 Os2 148.3(15) . . ? C101 Os3 Os2 86.3(9) . . yes Os1 Os3 Os2 58.77(5) . . yes C111 P1 C106 105.1(19) . . ? C111 P1 C201 102.6(20) . . ? C106 P1 C201 106.6(17) . . ? C111 P1 Os2 124.0(15) . . yes C106 P1 Os2 105.0(12) . . yes C201 P1 Os2 112.4(14) . . ? C121 P2 C131 99.9(18) . . ? C121 P2 C211 108.6(17) . . ? C131 P2 C211 106.4(17) . . ? C121 P2 Os2 119.0(14) . . ? C131 P2 Os2 115.0(12) . . ? C211 P2 Os2 107.3(11) . . ? C106 C101 C102 112.8(28) . . ? C106 C101 Os3 127.5(24) . . yes C102 C101 Os3 119.7(23) . . yes C106 C101 Os1 76.2(19) . . yes C102 C101 Os1 123.0(23) . . yes Os3 C101 Os1 77.5(10) . . yes C103 C102 C101 125.1(41) . . ? C102 C103 C104 118.6(48) . . ? C105 C104 C103 118.6(43) . . ? C104 C105 C106 121.3(43) . . ? C101 C106 C105 121.8(33) . . ? C101 C106 P1 119.1(25) . . ? C105 C106 P1 117.9(28) . . ? C101 C106 Os1 68.6(18) . . ? C105 C106 Os1 116.0(25) . . ? P1 C106 Os1 95.6(15) . . ? C116 C111 C112 111.8(43) . . ? C116 C111 P1 131.7(38) . . ? C112 C111 P1 116.3(34) . . ? C113 C112 C111 122.5(45) . . ? C114 C113 C112 111.9(59) . . ? C113 C114 C115 129.9(76) . . ? C114 C115 C116 117.5(71) . . ? C111 C116 C115 126.1(55) . . ? C122 C121 C126 117.0(43) . . ? C122 C121 P2 120.1(34) . . ? C126 C121 P2 122.6(34) . . ? C121 C122 C123 123.0(52) . . ? C122 C123 C124 120.2(61) . . ? C125 C124 C123 117.2(63) . . ? C126 C125 C124 115.7(52) . . ? C121 C126 C125 125.5(46) . . ? C132 C131 C136 115.6(37) . . ? C132 C131 P2 123.5(29) . . ? C136 C131 P2 120.4(30) . . ? C133 C132 C131 121.8(39) . . ? C132 C133 C134 119.5(47) . . ? C135 C134 C133 119.3(52) . . ? C136 C135 C134 118.5(52) . . ? C135 C136 C131 124.2(44) . . ? C210 C201 C202 116.0(37) . . ? C210 C201 P1 124.0(30) . . ? C202 C201 P1 119.8(32) . . ? C201 C202 C203 123.7(41) . . ? C204 C203 C202 116.9(40) . . ? C203 C204 C209 119.9(42) . . ? C203 C204 C205 120.4(42) . . ? C209 C204 C205 119.6(43) . . ? C206 C205 C204 121.9(51) . . ? C205 C206 C207 120.3(58) . . ? C208 C207 C206 118.2(55) . . ? C207 C208 C209 124.7(51) . . ? C210 C209 C204 121.8(41) . . ? C210 C209 C208 123.0(42) . . ? C204 C209 C208 114.7(43) . . ? C201 C210 C209 120.3(35) . . ? C201 C210 C220 118.6(33) . . ? C209 C210 C220 120.7(33) . . ? C220 C211 C212 117.5(34) . . ? C220 C211 P2 128.0(27) . . ? C212 C211 P2 113.8(27) . . ? C213 C212 C211 121.1(39) . . ? C214 C213 C212 124.7(42) . . ? C213 C214 C215 127.8(47) . . ? C213 C214 C219 116.6(42) . . ? C215 C214 C219 115.6(43) . . ? C216 C215 C214 123.7(49) . . ? C215 C216 C217 119.6(50) . . ? C218 C217 C216 123.5(48) . . ? C217 C218 C219 118.7(44) . . ? C218 C219 C220 120.5(41) . . ? C218 C219 C214 118.8(42) . . ? C220 C219 C214 120.7(40) . . ? C211 C220 C219 119.2(37) . . ? C211 C220 C210 121.2(34) . . ? C219 C220 C210 119.6(36) . . ? O11 C11 Os1 176.4(38) . . ? O12 C12 Os1 169.6(30) . . ? O13 C13 Os1 169.5(38) . . ? O21 C21 Os2 173.5(33) . . ? O22 C22 Os2 174.9(47) . . ? O31 C31 Os3 173.5(44) . . ? O32 C32 Os3 169.5(49) . . ? O33 C33 Os3 175.2(49) . . ? _refine_diff_density_max 3.929 _refine_diff_density_min -2.096 _refine_diff_density_rms 0.389