# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2217 data_global _publ_section_title ; Use of the monocationic fragment [Ru(h5-C5H5)(MeCN)3]+ as an ionic coupling reagent in the synthesis of mixed-metal phosphino clusters by R. Buntem, J.F. Gallagher, J. Lewis, P.R. Raithby, M.-A. Rennie and G.P. Shields ; _publ_requested_journal 'J.Chem.Soc.,Dalton Trans.' loop_ _publ_author_name 'Buntem, Rachada' 'Gallagher, John F.' 'Lewis, Jack' 'Raithby, Paul R.' 'Rennie, Moira-Ann' 'Shields, Gregory P.' data_ldb10 _audit_creation_method SHELXL _chemical_name_systematic ; (mu2-hydrido)(tri(phenyl)phosphine)bis(mu2-carbonyl)(octacarbonyl) tri-osmium(cyclopentadienyl)ruthenium ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H21 O10 Os3 P Ru' _chemical_formula_weight 1280.14 _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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.213(5) _cell_length_b 15.832(8) _cell_length_c 11.821(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.31(2) _cell_angle_gamma 90.00 _cell_volume 1654.8(14) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.569 _exptl_crystal_density_method ? _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 12.034 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.288 _exptl_absorpt_correction_T_max 0.391 _exptl_special_details ; The bridging hydride atom was located using the program HYDEX A. G. Orpen, J. Chem. Soc., Dalton Trans., 2509, 1980. ; _diffrn_ambient_temperature 153(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 'Stoe-Siemens four-circle diffractometer' _diffrn_measurement_method 'omega/theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 minutes' _diffrn_standards_decay_% ? _diffrn_reflns_number 6108 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5651 _reflns_number_observed 5633 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0725P)^2^+9.0013P] 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 noref _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 0.005(8) _refine_ls_number_reflns 5651 _refine_ls_number_parameters 433 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_obs 0.0332 _refine_ls_wR_factor_all 0.0890 _refine_ls_wR_factor_obs 0.0889 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.044 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.044 _refine_ls_shift/esd_max 0.002 _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 0.21633(5) 0.27063(2) -0.44783(3) 0.01631(11) Uani 1 d . . Os2 Os 0.03763(4) 0.15839(3) -0.36517(3) 0.01669(11) Uani 1 d . . Os3 Os 0.36376(4) 0.18132(2) -0.24578(3) 0.01040(10) Uani 1 d . . Ru1 Ru 0.26347(9) 0.09960(5) -0.46233(7) 0.0135(2) Uani 1 d . . P1 P 0.4457(3) 0.1285(2) -0.0505(2) 0.0105(5) Uani 1 d . . O11 O 0.5071(12) 0.3199(6) -0.4993(9) 0.038(2) Uani 1 d . . C11 C 0.3990(14) 0.3022(7) -0.4799(10) 0.023(2) Uani 1 d . . O12 O 0.0070(11) 0.2896(6) -0.6951(7) 0.037(2) Uani 1 d . . C12 C 0.0841(14) 0.2832(7) -0.5985(11) 0.025(3) Uani 1 d . . O13 O 0.1673(14) 0.4499(6) -0.3736(8) 0.046(3) Uani 1 d . . C13 C 0.1837(16) 0.3826(9) -0.4030(11) 0.031(3) Uani 1 d . . O21 O -0.0545(12) 0.3264(7) -0.2786(10) 0.043(2) Uani 1 d . . C21 C -0.0165(14) 0.2666(10) -0.3150(12) 0.033(3) Uani 1 d . . O22 O -0.2077(11) 0.1638(9) -0.5974(8) 0.052(3) Uani 1 d . . C22 C -0.1153(12) 0.1608(9) -0.5089(10) 0.026(3) Uani 1 d . . O23 O -0.1507(12) 0.0435(8) -0.2512(10) 0.048(3) Uani 1 d . . C23 C -0.0760(14) 0.0874(9) -0.2907(10) 0.031(3) Uani 1 d . . O24 O 0.0768(11) -0.0366(6) -0.4039(8) 0.033(2) Uani 1 d . . C24 C 0.1164(13) 0.0326(7) -0.4104(8) 0.019(2) Uani 1 d . . O31 O 0.3384(11) 0.3582(5) -0.1512(7) 0.028(2) Uani 1 d . . C31 C 0.3428(13) 0.2943(7) -0.1902(10) 0.021(2) Uani 1 d . . O32 O 0.6757(10) 0.2219(7) -0.2666(9) 0.039(2) Uani 1 d . . C32 C 0.5595(13) 0.2087(8) -0.2569(9) 0.022(2) Uani 1 d . . O33 O 0.4678(10) -0.0034(5) -0.2710(7) 0.027(2) Uani 1 d . . C33 C 0.3982(12) 0.0598(7) -0.3027(9) 0.019(2) Uani 1 d . . C41 C 0.4241(16) 0.0299(10) -0.5379(12) 0.039(3) Uani 1 d . . H41A H 0.5125(16) 0.0036(10) -0.4896(12) 0.047 Uiso 1 calc R . C42 C 0.4149(20) 0.1130(11) -0.5808(14) 0.050(4) Uani 1 d . . H42A H 0.4944(20) 0.1534(11) -0.5653(14) 0.060 Uiso 1 calc R . C43 C 0.2676(21) 0.1248(9) -0.6501(11) 0.044(4) Uani 1 d . . H43A H 0.2294(21) 0.1742(9) -0.6939(11) 0.053 Uiso 1 calc R . C44 C 0.1832(15) 0.0501(11) -0.6446(11) 0.040(4) Uani 1 d . . H44A H 0.0783(15) 0.0415(11) -0.6804(11) 0.049 Uiso 1 calc R . C45 C 0.2837(19) -0.0069(7) -0.5774(12) 0.036(3) Uani 1 d . . H45A H 0.2599(19) -0.0631(7) -0.5608(12) 0.043 Uiso 1 calc R . C111 C 0.3579(11) 0.0348(7) -0.0082(9) 0.014(2) Uani 1 d . . C112 C 0.2545(12) -0.0138(7) -0.0919(10) 0.019(2) Uani 1 d . . H11A H 0.2293(12) 0.0013(7) -0.1729(10) 0.023 Uiso 1 calc R . C113 C 0.1869(13) -0.0859(7) -0.0558(10) 0.022(2) Uani 1 d . . H11B H 0.1176(13) -0.1198(7) -0.1122(10) 0.027 Uiso 1 calc R . C114 C 0.2226(14) -0.1055(7) 0.0595(10) 0.023(2) Uani 1 d . . H11C H 0.1751(14) -0.1526(7) 0.0839(10) 0.027 Uiso 1 calc R . C115 C 0.3276(14) -0.0584(7) 0.1445(11) 0.024(2) Uani 1 d . . H11D H 0.3547(14) -0.0741(7) 0.2253(11) 0.029 Uiso 1 calc R . C116 C 0.3904(12) 0.0114(7) 0.1074(10) 0.019(2) Uani 1 d . . H11E H 0.4595(12) 0.0448(7) 0.1647(10) 0.023 Uiso 1 calc R . C121 C 0.4161(12) 0.2056(6) 0.0574(8) 0.013(2) Uani 1 d . . C122 C 0.5311(12) 0.2353(8) 0.1536(10) 0.022(2) Uani 1 d . . H12A H 0.6310(12) 0.2137(8) 0.1696(10) 0.026 Uiso 1 calc R . C123 C 0.4958(15) 0.2970(8) 0.2251(10) 0.030(3) Uani 1 d . . H12B H 0.5732(15) 0.3173(8) 0.2907(10) 0.036 Uiso 1 calc R . C124 C 0.3543(14) 0.3293(7) 0.2040(11) 0.026(3) Uani 1 d . . H12C H 0.3341(14) 0.3729(7) 0.2525(11) 0.031 Uiso 1 calc R . C125 C 0.2402(13) 0.2982(8) 0.1115(11) 0.023(2) Uani 1 d . . H12D H 0.1403(13) 0.3193(8) 0.0981(11) 0.028 Uiso 1 calc R . C126 C 0.2696(11) 0.2365(7) 0.0380(8) 0.016(2) Uani 1 d . . H12E H 0.1902(11) 0.2154(7) -0.0254(8) 0.019 Uiso 1 calc R . C131 C 0.6453(11) 0.1048(7) -0.0061(8) 0.013(2) Uani 1 d . . C132 C 0.7005(11) 0.0228(7) 0.0105(8) 0.014(2) Uani 1 d . . H13A H 0.6316(11) -0.0231(7) -0.0004(8) 0.016 Uiso 1 calc R . C133 C 0.8525(14) 0.0070(8) 0.0422(11) 0.027(3) Uani 1 d . . H13B H 0.8878(14) -0.0496(8) 0.0553(11) 0.033 Uiso 1 calc R . C134 C 0.9568(12) 0.0735(8) 0.0557(9) 0.024(2) Uani 1 d . . H13C H 1.0625(12) 0.0626(8) 0.0768(9) 0.029 Uiso 1 calc R . C135 C 0.9020(13) 0.1547(8) 0.0375(9) 0.022(2) Uani 1 d . . H13D H 0.9713(13) 0.2004(8) 0.0467(9) 0.026 Uiso 1 calc R . C136 C 0.7480(11) 0.1714(7) 0.0060(10) 0.020(2) Uani 1 d . . H13E H 0.7125(11) 0.2279(7) -0.0072(10) 0.023 Uiso 1 calc R . H23 H 0.1850 0.1515 -0.2204 0.050 Uiso 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 0.0218(2) 0.0122(2) 0.0142(2) 0.00310(15) 0.0039(2) 0.0035(2) Os2 0.0106(2) 0.0221(2) 0.0165(2) 0.00047(15) 0.00237(14) 0.00072(15) Os3 0.0104(2) 0.0100(2) 0.0107(2) 0.00000(13) 0.00277(13) 0.00020(13) Ru1 0.0168(4) 0.0122(4) 0.0117(4) -0.0018(3) 0.0044(3) -0.0010(3) P1 0.0093(12) 0.0087(11) 0.0128(11) 0.0009(9) 0.0018(9) -0.0002(9) O11 0.044(6) 0.036(5) 0.034(5) 0.003(4) 0.011(4) -0.011(4) C11 0.034(7) 0.011(5) 0.025(5) 0.000(4) 0.012(5) -0.012(5) O12 0.046(5) 0.038(5) 0.020(4) 0.000(4) -0.002(4) 0.019(4) C12 0.031(6) 0.014(5) 0.034(6) -0.004(5) 0.014(5) 0.012(5) O13 0.078(8) 0.021(5) 0.029(5) 0.001(4) 0.001(5) 0.020(5) C13 0.045(8) 0.028(7) 0.021(6) 0.000(5) 0.008(5) 0.007(6) O21 0.034(5) 0.039(6) 0.060(7) -0.012(5) 0.020(5) 0.004(5) C21 0.018(6) 0.040(8) 0.044(7) 0.002(6) 0.015(5) 0.000(6) O22 0.033(5) 0.080(9) 0.029(5) 0.019(5) -0.012(4) 0.002(6) C22 0.015(5) 0.036(7) 0.034(6) -0.004(5) 0.017(5) -0.001(5) O23 0.043(6) 0.053(7) 0.061(7) 0.005(5) 0.036(5) -0.019(5) C23 0.029(6) 0.044(8) 0.014(5) -0.007(5) -0.004(5) 0.010(6) O24 0.046(6) 0.023(5) 0.029(5) -0.005(4) 0.008(4) -0.013(4) C24 0.030(6) 0.016(6) 0.008(5) -0.001(4) 0.002(4) 0.004(5) O31 0.046(5) 0.015(4) 0.023(4) -0.008(3) 0.008(4) -0.003(4) C31 0.019(5) 0.019(6) 0.026(6) 0.008(5) 0.010(4) -0.003(4) O32 0.021(5) 0.055(6) 0.046(5) 0.010(5) 0.021(4) -0.003(4) C32 0.018(6) 0.027(6) 0.019(5) 0.004(4) 0.003(4) 0.005(5) O33 0.040(5) 0.013(4) 0.024(4) 0.003(3) 0.003(4) 0.014(4) C33 0.020(5) 0.021(6) 0.017(5) 0.002(4) 0.005(4) 0.001(5) C41 0.037(7) 0.051(9) 0.031(7) -0.004(6) 0.011(6) 0.024(7) C42 0.065(10) 0.053(9) 0.055(9) -0.034(8) 0.054(9) -0.020(8) C43 0.086(12) 0.035(7) 0.022(6) 0.008(5) 0.034(7) 0.031(8) C44 0.028(7) 0.068(11) 0.024(6) -0.024(7) 0.007(5) 0.000(7) C45 0.077(10) 0.011(6) 0.030(6) -0.011(5) 0.034(7) -0.001(6) C111 0.012(5) 0.018(5) 0.012(5) 0.001(4) 0.004(4) 0.002(4) C112 0.019(5) 0.018(5) 0.019(5) 0.006(4) 0.003(4) -0.009(4) C113 0.018(5) 0.020(6) 0.029(6) -0.003(5) 0.005(5) -0.004(4) C114 0.035(7) 0.016(5) 0.027(6) 0.000(4) 0.027(5) -0.003(5) C115 0.035(7) 0.011(5) 0.030(6) 0.003(4) 0.016(5) 0.008(5) C116 0.015(5) 0.018(5) 0.024(6) -0.005(4) 0.005(4) -0.008(4) C121 0.024(5) 0.009(5) 0.008(4) -0.003(4) 0.005(4) 0.000(4) C122 0.010(5) 0.032(7) 0.020(5) 0.001(4) -0.001(4) 0.001(4) C123 0.041(7) 0.027(6) 0.022(5) -0.009(5) 0.008(5) -0.008(5) C124 0.032(7) 0.020(6) 0.030(6) -0.012(5) 0.018(5) -0.005(5) C125 0.017(5) 0.022(6) 0.035(6) -0.003(5) 0.016(5) 0.005(5) C126 0.015(5) 0.022(6) 0.010(4) -0.004(4) 0.001(4) -0.011(4) C131 0.014(5) 0.016(5) 0.010(4) -0.001(4) 0.004(4) -0.003(4) C132 0.012(5) 0.015(5) 0.015(5) 0.001(4) 0.005(4) 0.000(4) C133 0.028(6) 0.024(6) 0.029(6) 0.008(5) 0.007(5) 0.008(5) C134 0.013(5) 0.036(7) 0.017(5) -0.001(5) -0.005(4) 0.003(5) C135 0.026(6) 0.019(5) 0.022(5) -0.007(4) 0.010(4) -0.006(5) C136 0.007(5) 0.020(6) 0.033(5) -0.005(5) 0.008(4) -0.006(4) _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 C12 1.865(12) . ? Os1 C11 1.893(12) . ? Os1 C13 1.899(13) . ? Os1 Ru1 2.755(2) . ? Os1 Os3 2.7796(12) . ? Os1 Os2 2.7797(10) . ? Os2 C22 1.879(12) . ? Os2 C23 1.912(15) . ? Os2 C21 1.923(15) . ? Os2 C24 2.235(11) . ? Os2 Ru1 2.8031(14) . ? Os2 Os3 2.961(2) . ? Os3 C32 1.895(12) . ? Os3 C31 1.934(12) . ? Os3 C33 2.091(12) . ? Os3 P1 2.371(3) . ? Os3 Ru1 2.7842(14) . ? Ru1 C24 1.950(11) . ? Ru1 C33 2.045(11) . ? Ru1 C45 2.208(11) . ? Ru1 C44 2.216(12) . ? Ru1 C41 2.224(13) . ? Ru1 C42 2.247(13) . ? Ru1 C43 2.266(12) . ? P1 C131 1.805(10) . ? P1 C111 1.825(11) . ? P1 C121 1.840(10) . ? O11 C11 1.12(2) . ? O12 C12 1.168(15) . ? O13 C13 1.14(2) . ? O21 C21 1.14(2) . ? O22 C22 1.149(15) . ? O23 C23 1.16(2) . ? O24 C24 1.16(2) . ? O31 C31 1.117(15) . ? O32 C32 1.13(2) . ? O33 C33 1.192(14) . ? C41 C45 1.38(2) . ? C41 C42 1.40(2) . ? C42 C43 1.39(2) . ? C43 C44 1.43(2) . ? C44 C45 1.38(2) . ? C111 C116 1.37(2) . ? C111 C112 1.396(15) . ? C112 C113 1.423(15) . ? C113 C114 1.34(2) . ? C114 C115 1.40(2) . ? C115 C116 1.37(2) . ? C121 C126 1.39(2) . ? C121 C122 1.399(14) . ? C122 C123 1.39(2) . ? C123 C124 1.36(2) . ? C124 C125 1.38(2) . ? C125 C126 1.38(2) . ? C131 C132 1.388(15) . ? C131 C136 1.397(14) . ? C132 C133 1.37(2) . ? C133 C134 1.40(2) . ? C134 C135 1.38(2) . ? C135 C136 1.39(2) . ? 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 C12 Os1 C11 99.2(5) . . ? C12 Os1 C13 93.1(5) . . ? C11 Os1 C13 91.7(5) . . ? C12 Os1 Ru1 96.8(3) . . ? C11 Os1 Ru1 94.7(3) . . ? C13 Os1 Ru1 167.2(4) . . ? C12 Os1 Os3 154.9(4) . . ? C11 Os1 Os3 93.4(4) . . ? C13 Os1 Os3 108.2(4) . . ? Ru1 Os1 Os3 60.40(3) . . ? C12 Os1 Os2 96.4(4) . . ? C11 Os1 Os2 152.5(4) . . ? C13 Os1 Os2 110.1(4) . . ? Ru1 Os1 Os2 60.85(3) . . ? Os3 Os1 Os2 64.37(3) . . ? C22 Os2 C23 93.4(5) . . ? C22 Os2 C21 93.8(6) . . ? C23 Os2 C21 99.1(5) . . ? C22 Os2 C24 90.8(5) . . ? C23 Os2 C24 81.0(5) . . ? C21 Os2 C24 175.4(5) . . ? C22 Os2 Os1 92.1(4) . . ? C23 Os2 Os1 173.3(3) . . ? C21 Os2 Os1 76.7(4) . . ? C24 Os2 Os1 102.8(3) . . ? C22 Os2 Ru1 95.2(3) . . ? C23 Os2 Ru1 124.0(4) . . ? C21 Os2 Ru1 135.1(4) . . ? C24 Os2 Ru1 43.8(3) . . ? Os1 Os2 Ru1 59.15(4) . . ? C22 Os2 Os3 146.2(3) . . ? C23 Os2 Os3 117.8(3) . . ? C21 Os2 Os3 93.5(4) . . ? C24 Os2 Os3 82.5(3) . . ? Os1 Os2 Os3 57.81(3) . . ? Ru1 Os2 Os3 57.68(4) . . ? C32 Os3 C31 90.0(5) . . ? C32 Os3 C33 87.4(5) . . ? C31 Os3 C33 177.1(5) . . ? C32 Os3 P1 95.7(3) . . ? C31 Os3 P1 91.8(3) . . ? C33 Os3 P1 87.3(3) . . ? C32 Os3 Os1 93.9(3) . . ? C31 Os3 Os1 75.5(3) . . ? C33 Os3 Os1 105.9(3) . . ? P1 Os3 Os1 164.01(6) . . ? C32 Os3 Ru1 96.8(3) . . ? C31 Os3 Ru1 134.7(3) . . ? C33 Os3 Ru1 47.0(3) . . ? P1 Os3 Ru1 131.60(7) . . ? Os1 Os3 Ru1 59.37(4) . . ? C32 Os3 Os2 148.5(3) . . ? C31 Os3 Os2 95.2(3) . . ? C33 Os3 Os2 87.7(3) . . ? P1 Os3 Os2 115.07(6) . . ? Os1 Os3 Os2 57.81(2) . . ? Ru1 Os3 Os2 58.30(3) . . ? C24 Ru1 C33 80.6(4) . . ? C24 Ru1 C45 88.0(5) . . ? C33 Ru1 C45 101.5(5) . . ? C24 Ru1 C44 92.4(5) . . ? C33 Ru1 C44 137.6(5) . . ? C45 Ru1 C44 36.2(6) . . ? C24 Ru1 C41 117.1(5) . . ? C33 Ru1 C41 85.3(5) . . ? C45 Ru1 C41 36.2(6) . . ? C44 Ru1 C41 60.8(5) . . ? C24 Ru1 C42 148.8(5) . . ? C33 Ru1 C42 106.4(6) . . ? C45 Ru1 C42 60.9(5) . . ? C44 Ru1 C42 61.5(6) . . ? C41 Ru1 C42 36.6(6) . . ? C24 Ru1 C43 127.5(6) . . ? C33 Ru1 C43 141.7(5) . . ? C45 Ru1 C43 60.2(5) . . ? C44 Ru1 C43 37.1(6) . . ? C41 Ru1 C43 59.8(5) . . ? C42 Ru1 C43 35.8(6) . . ? C24 Ru1 Os1 112.3(3) . . ? C33 Ru1 Os1 108.1(3) . . ? C45 Ru1 Os1 146.2(3) . . ? C44 Ru1 Os1 113.1(5) . . ? C41 Ru1 Os1 130.3(4) . . ? C42 Ru1 Os1 94.7(4) . . ? C43 Ru1 Os1 86.2(3) . . ? C24 Ru1 Os3 92.5(3) . . ? C33 Ru1 Os3 48.4(3) . . ? C45 Ru1 Os3 149.1(4) . . ? C44 Ru1 Os3 172.9(5) . . ? C41 Ru1 Os3 120.9(4) . . ? C42 Ru1 Os3 115.2(4) . . ? C43 Ru1 Os3 136.6(4) . . ? Os1 Ru1 Os3 60.23(2) . . ? C24 Ru1 Os2 52.4(3) . . ? C33 Ru1 Os2 93.0(3) . . ? C45 Ru1 Os2 135.0(4) . . ? C44 Ru1 Os2 115.6(3) . . ? C41 Ru1 Os2 169.5(4) . . ? C42 Ru1 Os2 152.4(5) . . ? C43 Ru1 Os2 124.2(4) . . ? Os1 Ru1 Os2 60.00(2) . . ? Os3 Ru1 Os2 64.01(4) . . ? C131 P1 C111 104.2(5) . . ? C131 P1 C121 105.9(5) . . ? C111 P1 C121 100.7(5) . . ? C131 P1 Os3 112.1(3) . . ? C111 P1 Os3 120.6(3) . . ? C121 P1 Os3 111.9(3) . . ? O11 C11 Os1 179.2(11) . . ? O12 C12 Os1 176.6(10) . . ? O13 C13 Os1 178.2(12) . . ? O21 C21 Os2 173.6(12) . . ? O22 C22 Os2 178.6(12) . . ? O23 C23 Os2 176.3(11) . . ? O24 C24 Ru1 142.3(9) . . ? O24 C24 Os2 133.9(9) . . ? Ru1 C24 Os2 83.8(4) . . ? O31 C31 Os3 175.1(10) . . ? O32 C32 Os3 177.0(11) . . ? O33 C33 Ru1 133.0(9) . . ? O33 C33 Os3 142.1(8) . . ? Ru1 C33 Os3 84.6(4) . . ? C45 C41 C42 108.7(13) . . ? C45 C41 Ru1 71.3(7) . . ? C42 C41 Ru1 72.6(7) . . ? C43 C42 C41 106.8(14) . . ? C43 C42 Ru1 72.9(8) . . ? C41 C42 Ru1 70.8(8) . . ? C42 C43 C44 108.5(13) . . ? C42 C43 Ru1 71.3(8) . . ? C44 C43 Ru1 69.5(7) . . ? C45 C44 C43 106.5(13) . . ? C45 C44 Ru1 71.6(7) . . ? C43 C44 Ru1 73.4(7) . . ? C41 C45 C44 109.5(12) . . ? C41 C45 Ru1 72.6(7) . . ? C44 C45 Ru1 72.2(7) . . ? C116 C111 C112 118.3(10) . . ? C116 C111 P1 120.3(8) . . ? C112 C111 P1 121.3(8) . . ? C111 C112 C113 119.9(10) . . ? C114 C113 C112 119.1(10) . . ? C113 C114 C115 121.9(10) . . ? C116 C115 C114 117.9(11) . . ? C111 C116 C115 122.9(10) . . ? C126 C121 C122 119.5(9) . . ? C126 C121 P1 116.4(7) . . ? C122 C121 P1 124.1(8) . . ? C123 C122 C121 118.5(10) . . ? C124 C123 C122 122.0(11) . . ? C123 C124 C125 119.4(10) . . ? C124 C125 C126 120.7(10) . . ? C125 C126 C121 119.8(9) . . ? C132 C131 C136 118.8(9) . . ? C132 C131 P1 122.6(8) . . ? C136 C131 P1 118.6(8) . . ? C133 C132 C131 121.1(10) . . ? C132 C133 C134 120.6(11) . . ? C135 C134 C133 118.3(10) . . ? C134 C135 C136 121.5(11) . . ? C135 C136 C131 119.7(11) . . ? _refine_diff_density_max 1.818 _refine_diff_density_min -1.543 _refine_diff_density_rms 0.211 data_ldb07 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H21 O11 Os3 P Ru' _chemical_formula_weight 1308.15 _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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.878(4) _cell_length_b 22.669(17) _cell_length_c 9.415(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.06(4) _cell_angle_gamma 90.00 _cell_volume 1730.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour 'Dark Red/Purple' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.511 _exptl_crystal_density_method ? _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 11.514 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.401 _exptl_absorpt_correction_T_max 0.526 _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(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 'Stoe-Siemens four-circle diffractometer' _diffrn_measurement_method 'omega/theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 minutes' _diffrn_standards_decay_% ? _diffrn_reflns_number 5552 _diffrn_reflns_av_R_equivalents 0.1280 _diffrn_reflns_av_sigmaI/netI 0.1260 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 23.99 _reflns_number_total 2788 _reflns_number_observed 2670 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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^)+(0.0191P)^2^+8.7521P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 2787 _refine_ls_number_parameters 227 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_obs 0.0462 _refine_ls_wR_factor_all 0.1080 _refine_ls_wR_factor_obs 0.1055 _refine_ls_goodness_of_fit_all 1.175 _refine_ls_goodness_of_fit_obs 1.178 _refine_ls_restrained_S_all 1.169 _refine_ls_restrained_S_obs 1.168 _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 0.53051(11) 0.29882(3) 0.84187(13) 0.0346(3) Uani 1 d . . Os2 Os 0.60499(9) 0.42297(3) 0.90352(11) 0.0294(3) Uani 1 d . . Os3 Os 0.54450(10) 0.36028(4) 0.59840(12) 0.0336(3) Uani 1 d . . Ru4 Ru 0.2272(2) 0.31729(8) 0.5600(3) 0.0402(5) Uani 1 d . . P1 P 0.6480(6) 0.5250(2) 0.8824(8) 0.0298(13) Uani 1 d . . C1 C 0.1853(45) 0.2743(17) 0.3275(55) 0.089(11) Uiso 1 d . . H1 H 0.2521(45) 0.2808(17) 0.2744(55) 0.107 Uiso 1 calc R . C2 C 0.2052(40) 0.2278(16) 0.4297(50) 0.077(9) Uiso 1 d . . H2 H 0.2843(40) 0.1982(16) 0.4540(50) 0.093 Uiso 1 calc R . C3 C 0.0821(45) 0.2336(18) 0.4912(60) 0.093(11) Uiso 1 d . . H3 H 0.0703(45) 0.2112(18) 0.5688(60) 0.112 Uiso 1 calc R . C4 C -0.0223(42) 0.2836(17) 0.4019(52) 0.085(11) Uiso 1 d . . H4 H -0.1214(42) 0.2961(17) 0.4032(52) 0.102 Uiso 1 calc R . C5 C 0.0591(33) 0.3083(14) 0.3150(47) 0.067(8) Uiso 1 d . . H5 H 0.0289(33) 0.3430(14) 0.2578(47) 0.081 Uiso 1 calc R . C101 C 0.8171(22) 0.5612(7) 1.0453(28) 0.032(5) Uiso 1 d D . C102 C 0.9395(22) 0.5301(10) 1.1611(27) 0.045(6) Uiso 1 d D . H102 H 0.9351(22) 0.4892(10) 1.1610(27) 0.054 Uiso 1 calc R . C103 C 1.0691(27) 0.5587(9) 1.2777(34) 0.050(6) Uiso 1 d D . H103 H 1.1498(27) 0.5364(9) 1.3539(34) 0.060 Uiso 1 calc R . C104 C 1.0816(29) 0.6195(9) 1.2838(35) 0.053(6) Uiso 1 d D . H104 H 1.1677(29) 0.6387(9) 1.3629(35) 0.064 Uiso 1 calc R . C105 C 0.9595(24) 0.6501(11) 1.1663(29) 0.052(6) Uiso 1 d D . H105 H 0.9655(24) 0.6911(11) 1.1651(29) 0.062 Uiso 1 calc R . C106 C 0.8289(27) 0.6222(8) 1.0505(34) 0.048(6) Uiso 1 d D . H106 H 0.7478(27) 0.6446(8) 0.9750(34) 0.058 Uiso 1 calc R . C111 C 0.6898(20) 0.5403(10) 0.7094(28) 0.039(5) Uiso 1 d D . C112 C 0.8428(29) 0.5538(12) 0.7115(37) 0.061(7) Uiso 1 d D . H112 H 0.9297(29) 0.5620(12) 0.8063(37) 0.073 Uiso 1 calc R . C113 C 0.8705(33) 0.5554(13) 0.5802(29) 0.065(8) Uiso 1 d D . H113 H 0.9777(33) 0.5564(13) 0.5861(29) 0.078 Uiso 1 calc R . C114 C 0.7387(23) 0.5555(12) 0.4389(37) 0.060(7) Uiso 1 d D . H114 H 0.7539(23) 0.5614(12) 0.3479(37) 0.072 Uiso 1 calc R . C115 C 0.5837(27) 0.5468(11) 0.4335(33) 0.053(7) Uiso 1 d D . H115 H 0.4941(27) 0.5449(11) 0.3375(33) 0.063 Uiso 1 calc R . C116 C 0.5582(27) 0.5409(11) 0.5665(23) 0.048(6) Uiso 1 d D . H116 H 0.4514(27) 0.5372(11) 0.5605(23) 0.057 Uiso 1 calc R . C121 C 0.4798(27) 0.5729(10) 0.8703(29) 0.044(6) Uiso 1 d D . C122 C 0.4242(24) 0.6204(9) 0.7707(34) 0.042(6) Uiso 1 d D . H122 H 0.4791(24) 0.6293(9) 0.7077(34) 0.050 Uiso 1 calc R . C123 C 0.2929(27) 0.6553(10) 0.7584(35) 0.051(6) Uiso 1 d D . H123 H 0.2521(27) 0.6840(10) 0.6816(35) 0.061 Uiso 1 calc R . C124 C 0.2238(32) 0.6464(11) 0.8637(31) 0.057(7) Uiso 1 d D . H124 H 0.1434(32) 0.6724(11) 0.8654(31) 0.069 Uiso 1 calc R . C125 C 0.2711(25) 0.6000(9) 0.9663(33) 0.046(6) Uiso 1 d D . H125 H 0.2183(25) 0.5921(9) 1.0317(33) 0.056 Uiso 1 calc R . C126 C 0.4003(24) 0.5655(9) 0.9684(30) 0.040(5) Uiso 1 d D . H126 H 0.4364(24) 0.5351(9) 1.0410(30) 0.048 Uiso 1 calc R . C11 C 0.4742(37) 0.2185(14) 0.7889(49) 0.067(8) Uiso 1 d . . C12 C 0.5084(28) 0.2934(12) 1.0391(36) 0.046(6) Uiso 1 d . . C13 C 0.7551(33) 0.2819(13) 0.9204(43) 0.058(7) Uiso 1 d . . C21 C 0.8356(27) 0.4058(10) 0.9275(34) 0.040(6) Uiso 1 d . . C22 C 0.3778(24) 0.4296(10) 0.8667(32) 0.037(5) Uiso 1 d . . C23 C 0.6744(29) 0.4206(13) 1.1272(38) 0.049(6) Uiso 1 d . . C31 C 0.5758(29) 0.2845(11) 0.5282(38) 0.048(6) Uiso 1 d . . C32 C 0.4376(29) 0.3991(11) 0.3959(36) 0.046(6) Uiso 1 d . . C33 C 0.7590(25) 0.3875(10) 0.6110(30) 0.035(5) Uiso 1 d . . C41 C 0.2208(26) 0.3131(10) 0.7503(35) 0.044(6) Uiso 1 d . . C42 C 0.2019(30) 0.3979(12) 0.5485(42) 0.048(6) Uiso 1 d . . O11 O 0.4450(25) 0.1695(9) 0.7682(36) 0.072(6) Uiso 1 d . . O12 O 0.4931(29) 0.2936(13) 1.1466(39) 0.095(8) Uiso 1 d . . O13 O 0.8992(22) 0.2691(8) 0.9609(27) 0.062(5) Uiso 1 d . . O21 O 0.9660(18) 0.3997(6) 0.9664(22) 0.041(4) Uiso 1 d . . O22 O 0.2496(20) 0.4382(7) 0.8841(25) 0.051(4) Uiso 1 d . . O23 O 0.7076(23) 0.4171(10) 1.2504(30) 0.065(5) Uiso 1 d . . O31 O 0.6091(25) 0.2388(10) 0.4900(32) 0.074(6) Uiso 1 d . . O32 O 0.3658(24) 0.4180(10) 0.2784(33) 0.074(6) Uiso 1 d . . O33 O 0.8761(21) 0.4013(8) 0.6207(27) 0.057(5) Uiso 1 d . . O41 O 0.1558(21) 0.3056(9) 0.8527(28) 0.062(5) Uiso 1 d . . O42 O 0.1582(24) 0.4474(9) 0.5435(31) 0.067(6) Uiso 1 d . . H23 H 0.5242 0.4306 0.6891 0.080 Uiso 1 calc . . 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 0.0464(5) 0.0238(4) 0.0326(7) 0.0022(5) 0.0150(5) 0.0001(4) Os2 0.0326(4) 0.0275(4) 0.0300(6) 0.0005(4) 0.0147(4) -0.0010(3) Os3 0.0379(4) 0.0363(4) 0.0304(6) -0.0009(5) 0.0177(4) -0.0003(3) Ru4 0.0348(9) 0.0398(10) 0.0414(14) -0.0019(11) 0.0109(9) -0.0067(7) P1 0.035(3) 0.031(3) 0.022(3) 0.005(3) 0.011(3) 0.002(2) _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 1.86(3) . ? Os1 C11 1.90(3) . ? Os1 C12 1.95(3) . ? Os1 C41 2.54(2) . ? Os1 Os3 2.728(2) . ? Os1 Os2 2.895(2) . ? Os1 Ru4 2.940(3) . ? Os2 C22 1.91(2) . ? Os2 C23 1.94(3) . ? Os2 C21 2.00(2) . ? Os2 P1 2.366(6) . ? Os2 Os3 3.050(2) . ? Os3 C31 1.90(3) . ? Os3 C32 1.96(3) . ? Os3 C33 1.96(2) . ? Os3 Ru4 2.861(2) . ? Ru4 C41 1.82(3) . ? Ru4 C42 1.84(3) . ? Ru4 C5 2.19(4) . ? Ru4 C3 2.24(4) . ? Ru4 C4 2.24(4) . ? Ru4 C1 2.28(5) . ? Ru4 C2 2.34(4) . ? P1 C121 1.81(2) . ? P1 C101 1.84(2) . ? P1 C111 1.85(3) . ? C1 C5 1.32(5) . ? C1 C2 1.39(5) . ? C2 C3 1.44(6) . ? C3 C4 1.49(5) . ? C4 C5 1.41(6) . ? C101 C102 1.38(2) . ? C101 C106 1.39(2) . ? C102 C103 1.38(2) . ? C103 C104 1.38(2) . ? C104 C105 1.38(2) . ? C105 C106 1.38(2) . ? C111 C116 1.38(2) . ? C111 C112 1.38(2) . ? C112 C113 1.36(2) . ? C113 C114 1.37(2) . ? C114 C115 1.37(2) . ? C115 C116 1.37(2) . ? C121 C122 1.38(2) . ? C121 C126 1.38(2) . ? C122 C123 1.38(2) . ? C123 C124 1.38(2) . ? C124 C125 1.37(2) . ? C125 C126 1.38(2) . ? C11 O11 1.14(4) . ? C12 O12 1.07(4) . ? C13 O13 1.21(3) . ? C21 O21 1.07(2) . ? C22 O22 1.23(3) . ? C23 O23 1.08(4) . ? C31 O31 1.17(3) . ? C32 O32 1.11(3) . ? C33 O33 1.05(2) . ? C41 O41 1.32(4) . ? C42 O42 1.18(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Os1 C11 91.8(13) . . ? C13 Os1 C12 96.7(14) . . ? C11 Os1 C12 94.1(15) . . ? C13 Os1 C41 174.2(11) . . ? C11 Os1 C41 84.3(11) . . ? C12 Os1 C41 79.4(10) . . ? C13 Os1 Os3 91.7(11) . . ? C11 Os1 Os3 111.5(13) . . ? C12 Os1 Os3 152.8(8) . . ? C41 Os1 Os3 93.6(7) . . ? C13 Os1 Os2 90.0(9) . . ? C11 Os1 Os2 176.6(12) . . ? C12 Os1 Os2 88.5(8) . . ? C41 Os1 Os2 94.1(5) . . ? Os3 Os1 Os2 65.61(4) . . ? C13 Os1 Ru4 145.7(12) . . ? C11 Os1 Ru4 81.6(11) . . ? C12 Os1 Ru4 117.2(7) . . ? C41 Os1 Ru4 37.9(7) . . ? Os3 Os1 Ru4 60.50(6) . . ? Os2 Os1 Ru4 95.33(5) . . ? C22 Os2 C23 92.5(11) . . ? C22 Os2 C21 172.5(10) . . ? C23 Os2 C21 90.8(11) . . ? C22 Os2 P1 95.9(7) . . ? C23 Os2 P1 97.3(9) . . ? C21 Os2 P1 90.4(6) . . ? C22 Os2 Os1 84.4(7) . . ? C23 Os2 Os1 97.9(9) . . ? C21 Os2 Os1 88.5(6) . . ? P1 Os2 Os1 164.8(2) . . ? C22 Os2 Os3 95.6(8) . . ? C23 Os2 Os3 150.0(9) . . ? C21 Os2 Os3 78.2(8) . . ? P1 Os2 Os3 110.4(2) . . ? Os1 Os2 Os3 54.56(4) . . ? C31 Os3 C32 98.6(12) . . ? C31 Os3 C33 91.7(10) . . ? C32 Os3 C33 89.5(10) . . ? C31 Os3 Os1 83.9(9) . . ? C32 Os3 Os1 151.3(7) . . ? C33 Os3 Os1 119.1(7) . . ? C31 Os3 Ru4 85.6(7) . . ? C32 Os3 Ru4 88.2(7) . . ? C33 Os3 Ru4 176.1(7) . . ? Os1 Os3 Ru4 63.42(7) . . ? C31 Os3 Os2 138.9(10) . . ? C32 Os3 Os2 122.5(8) . . ? C33 Os3 Os2 90.2(7) . . ? Os1 Os3 Os2 59.83(5) . . ? Ru4 Os3 Os2 93.67(7) . . ? C41 Ru4 C42 93.3(14) . . ? C41 Ru4 C5 138.8(11) . . ? C42 Ru4 C5 91.0(13) . . ? C41 Ru4 C3 89.8(15) . . ? C42 Ru4 C3 141.7(13) . . ? C5 Ru4 C3 63.3(16) . . ? C41 Ru4 C4 102.6(14) . . ? C42 Ru4 C4 103.6(13) . . ? C5 Ru4 C4 37.1(14) . . ? C3 Ru4 C4 38.9(14) . . ? C41 Ru4 C1 149.8(13) . . ? C42 Ru4 C1 113.5(15) . . ? C5 Ru4 C1 34.4(12) . . ? C3 Ru4 C1 60.7(17) . . ? C4 Ru4 C1 59.1(15) . . ? C41 Ru4 C2 116.3(13) . . ? C42 Ru4 C2 148.2(16) . . ? C5 Ru4 C2 59.3(13) . . ? C3 Ru4 C2 36.5(15) . . ? C4 Ru4 C2 60.5(13) . . ? C1 Ru4 C2 35.0(13) . . ? C41 Ru4 Os3 108.5(7) . . ? C42 Ru4 Os3 76.0(8) . . ? C5 Ru4 Os3 112.2(8) . . ? C3 Ru4 Os3 138.3(10) . . ? C4 Ru4 Os3 148.9(12) . . ? C1 Ru4 Os3 91.9(10) . . ? C2 Ru4 Os3 103.2(8) . . ? C41 Ru4 Os1 59.2(7) . . ? C42 Ru4 Os1 103.8(10) . . ? C5 Ru4 Os1 156.8(8) . . ? C3 Ru4 Os1 110.4(11) . . ? C4 Ru4 Os1 147.7(11) . . ? C1 Ru4 Os1 122.4(9) . . ? C2 Ru4 Os1 101.5(9) . . ? Os3 Ru4 Os1 56.08(5) . . ? C121 P1 C101 99.0(10) . . ? C121 P1 C111 106.8(9) . . ? C101 P1 C111 105.2(9) . . ? C121 P1 Os2 115.7(7) . . ? C101 P1 Os2 118.0(6) . . ? C111 P1 Os2 110.8(7) . . ? C5 C1 C2 111.5(39) . . ? C5 C1 Ru4 68.8(26) . . ? C2 C1 Ru4 74.6(25) . . ? C1 C2 C3 107.9(33) . . ? C1 C2 Ru4 70.4(22) . . ? C3 C2 Ru4 67.9(23) . . ? C2 C3 C4 104.0(40) . . ? C2 C3 Ru4 75.6(22) . . ? C4 C3 Ru4 70.7(21) . . ? C5 C4 C3 106.3(34) . . ? C5 C4 Ru4 69.4(20) . . ? C3 C4 Ru4 70.5(19) . . ? C1 C5 C4 109.5(35) . . ? C1 C5 Ru4 76.8(25) . . ? C4 C5 Ru4 73.5(25) . . ? C102 C101 C106 117.2(20) . . ? C102 C101 P1 122.9(13) . . ? C106 C101 P1 119.8(16) . . ? C101 C102 C103 121.4(20) . . ? C104 C103 C102 121.7(24) . . ? C105 C104 C103 116.4(24) . . ? C106 C105 C104 122.4(22) . . ? C105 C106 C101 120.8(22) . . ? C116 C111 C112 116.7(22) . . ? C116 C111 P1 117.9(15) . . ? C112 C111 P1 125.3(18) . . ? C113 C112 C111 122.3(26) . . ? C112 C113 C114 119.1(27) . . ? C113 C114 C115 118.9(28) . . ? C116 C115 C114 121.3(26) . . ? C115 C116 C111 120.3(22) . . ? C122 C121 C126 114.2(22) . . ? C122 C121 P1 124.6(15) . . ? C126 C121 P1 121.1(15) . . ? C123 C122 C121 124.2(23) . . ? C122 C123 C124 117.8(24) . . ? C125 C124 C123 121.4(24) . . ? C124 C125 C126 117.2(23) . . ? C125 C126 C121 124.7(23) . . ? O11 C11 Os1 175.1(41) . . ? O12 C12 Os1 176.0(29) . . ? O13 C13 Os1 175.1(30) . . ? O21 C21 Os2 167.3(25) . . ? O22 C22 Os2 162.8(23) . . ? O23 C23 Os2 176.4(29) . . ? O31 C31 Os3 174.3(21) . . ? O32 C32 Os3 174.0(23) . . ? O33 C33 Os3 178.3(24) . . ? O41 C41 Ru4 157.6(20) . . ? O41 C41 Os1 118.0(19) . . ? Ru4 C41 Os1 82.9(9) . . ? O42 C42 Ru4 167.4(24) . . ? _refine_diff_density_max 2.987 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.236 data_ldb06 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H19 O14 Os3 P Ru2' _chemical_formula_weight 1335.10 _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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.049(6) _cell_length_b 9.548(2) _cell_length_c 19.163(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.62(3) _cell_angle_gamma 90.00 _cell_volume 3109.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.852 _exptl_crystal_density_method ? _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 13.281 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.251 _exptl_absorpt_correction_T_max 0.932 _exptl_special_details ; ? ; _diffrn_ambient_temperature 290(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 'Stoe-Siemens four-circle diffractometer' _diffrn_measurement_method 'Omega/theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 minutes' _diffrn_standards_decay_% ? _diffrn_reflns_number 5740 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 24.98 _reflns_number_total 5453 _reflns_number_observed 4507 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXTL-PLUS (Siemens, 1991)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-PLUS (Siemens, 1991)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 14 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^)+(0.0661P)^2^+21.3374P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5439 _refine_ls_number_parameters 444 _refine_ls_number_restraints 212 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_obs 0.0430 _refine_ls_wR_factor_all 0.1163 _refine_ls_wR_factor_obs 0.1017 _refine_ls_goodness_of_fit_all 1.095 _refine_ls_goodness_of_fit_obs 1.082 _refine_ls_restrained_S_all 1.095 _refine_ls_restrained_S_obs 1.057 _refine_ls_shift/esd_max 0.004 _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 0.71691(2) 0.37036(5) 0.43538(2) 0.03364(13) Uani 1 d . . Os2 Os 0.76820(2) 0.37212(5) 0.29170(2) 0.03433(13) Uani 1 d . . Os3 Os 0.82856(3) 0.18633(5) 0.39487(3) 0.03909(14) Uani 1 d . . Ru4 Ru 0.86944(5) 0.47938(10) 0.41040(5) 0.0397(2) Uani 1 d . . Ru5 Ru 0.74296(7) 0.62952(11) 0.22169(6) 0.0485(3) Uani 1 d . . P1 P 0.5973(2) 0.2695(4) 0.4208(2) 0.0457(8) Uani 1 d . . O101 O 0.5695(7) 0.1800(15) 0.4832(7) 0.094(4) Uani 1 d D . O102 O 0.5922(6) 0.1602(12) 0.3600(7) 0.078(3) Uani 1 d . . O103 O 0.5215(5) 0.3630(11) 0.4062(6) 0.067(3) Uani 1 d . . C101 C 0.5434(19) 0.2533(38) 0.5403(14) 0.097(11) Uiso 0.72(5) d PDU 1 H10A H 0.5281(19) 0.1880(38) 0.5747(14) 0.116 Uiso 0.72(5) calc PR 1 H10B H 0.4990(19) 0.3105(38) 0.5247(14) 0.116 Uiso 0.72(5) calc PR 1 H10C H 0.5850(19) 0.3118(38) 0.5605(14) 0.116 Uiso 0.72(5) calc PR 1 C111 C 0.5216(37) 0.1574(96) 0.5361(31) 0.091(24) Uiso 0.28(5) d PDU 2 H11A H 0.5357(37) 0.0706(96) 0.5591(31) 0.110 Uiso 0.28(5) calc PR 2 H11B H 0.4678(37) 0.1530(96) 0.5170(31) 0.110 Uiso 0.28(5) calc PR 2 H11C H 0.5276(37) 0.2328(96) 0.5693(31) 0.110 Uiso 0.28(5) calc PR 2 C102 C 0.5248(11) 0.0778(24) 0.3397(14) 0.122(9) Uani 1 d . . H10D H 0.5395(20) -0.0192(27) 0.3388(78) 0.146 Uiso 1 calc R . H10E H 0.5034(52) 0.1060(108) 0.2940(35) 0.146 Uiso 1 calc R . H10F H 0.4859(37) 0.0909(124) 0.3727(45) 0.146 Uiso 1 calc R . C103 C 0.5113(10) 0.4448(21) 0.3450(10) 0.103(7) Uani 1 d . . H10G H 0.4880(28) 0.5330(33) 0.3558(13) 0.124 Uiso 1 calc R . H10H H 0.4774(24) 0.3965(35) 0.3106(16) 0.124 Uiso 1 calc R . H10I H 0.5615(10) 0.4607(41) 0.3270(14) 0.124 Uiso 1 calc R . C1 C 0.8384(10) 0.7416(40) 0.1679(15) 0.071(10) Uani 0.47(4) d PRDU 1 H1 H 0.8866(10) 0.7661(40) 0.1907(15) 0.085 Uiso 0.47(4) calc PR 1 C2 C 0.7698(26) 0.8259(37) 0.1623(29) 0.083(11) Uani 0.47(4) d PDU 1 H2 H 0.7657(26) 0.9168(37) 0.1790(29) 0.100 Uiso 0.47(4) calc PR 1 C3 C 0.7086(17) 0.7468(53) 0.1264(26) 0.077(11) Uani 0.47(4) d PDU 1 H3 H 0.6563(17) 0.7742(53) 0.1186(26) 0.093 Uiso 0.47(4) calc PR 1 C4 C 0.7408(31) 0.6193(45) 0.1046(24) 0.075(11) Uani 0.47(4) d PDU 1 H4 H 0.7145(31) 0.5514(45) 0.0769(24) 0.091 Uiso 0.47(4) calc PR 1 C5 C 0.8208(27) 0.6132(34) 0.1328(28) 0.068(10) Uani 0.47(4) d PDU 1 H5 H 0.8552(27) 0.5386(34) 0.1288(28) 0.081 Uiso 0.47(4) calc PR 1 C1A C 0.8200(22) 0.7875(36) 0.1703(17) 0.067(9) Uani 0.53(4) d PDU 2 H1A H 0.8520(22) 0.8490(36) 0.1973(17) 0.081 Uiso 0.53(4) calc PR 2 C2A C 0.7398(23) 0.8084(31) 0.1470(27) 0.071(9) Uani 0.53(4) d PDU 2 H2A H 0.7103(23) 0.8879(31) 0.1549(27) 0.085 Uiso 0.53(4) calc PR 2 C3A C 0.7121(18) 0.6880(47) 0.1095(19) 0.072(10) Uani 0.53(4) d PDU 2 H3A H 0.6612(18) 0.6741(47) 0.0895(19) 0.086 Uiso 0.53(4) calc PR 2 C4A C 0.7756(29) 0.5923(34) 0.1077(23) 0.077(10) Uani 0.53(4) d PDU 2 H4A H 0.7739(29) 0.5048(34) 0.0864(23) 0.093 Uiso 0.53(4) calc PR 2 C5A C 0.8423(18) 0.6544(45) 0.1445(22) 0.068(10) Uani 0.53(4) d PDU 2 H5A H 0.8922(18) 0.6149(45) 0.1507(22) 0.082 Uiso 0.53(4) calc PR 2 C1' C 0.8040(8) 0.6766(13) 0.3769(7) 0.050(3) Uani 1 d . . H1' H 0.7542(8) 0.6960(13) 0.3909(7) 0.059 Uiso 1 calc R . C2' C 0.8770(9) 0.7133(14) 0.4166(9) 0.065(4) Uani 1 d . . H2' H 0.8819(9) 0.7597(14) 0.4594(9) 0.078 Uiso 1 calc R . C3' C 0.9397(9) 0.6652(15) 0.3781(10) 0.073(5) Uani 1 d . . H3' H 0.9932(9) 0.6744(15) 0.3909(10) 0.088 Uiso 1 calc R . C4' C 0.9054(8) 0.6019(15) 0.3177(8) 0.060(4) Uani 1 d . . H4' H 0.9338(8) 0.5608(15) 0.2836(8) 0.072 Uiso 1 calc R . C5' C 0.8185(7) 0.6076(12) 0.3141(7) 0.043(3) Uani 1 d . . C11 C 0.7344(7) 0.2933(16) 0.5256(6) 0.053(3) Uani 1 d . . C12 C 0.6686(7) 0.5391(14) 0.4618(7) 0.048(3) Uani 1 d . . C21 C 0.8493(8) 0.3315(15) 0.2314(8) 0.055(3) Uani 1 d . . C22 C 0.7240(8) 0.1958(15) 0.2681(7) 0.054(3) Uani 1 d . . C31 C 0.8812(8) 0.1234(15) 0.4791(8) 0.054(3) Uani 1 d . . C32 C 0.8980(8) 0.0871(15) 0.3363(8) 0.060(4) Uani 1 d . . C33 C 0.7522(9) 0.0450(15) 0.4047(8) 0.059(4) Uani 1 d . . C41 C 0.8687(8) 0.4640(14) 0.5084(9) 0.055(3) Uani 1 d . . C42 C 0.9530(8) 0.3471(15) 0.4113(9) 0.063(4) Uani 1 d . . C51 C 0.6636(8) 0.7023(14) 0.2725(7) 0.052(3) Uani 1 d . . C52 C 0.6835(8) 0.4452(15) 0.2188(7) 0.053(3) Uani 1 d . . O11 O 0.7419(7) 0.2479(15) 0.5805(6) 0.084(4) Uani 1 d . . O12 O 0.6444(6) 0.6432(12) 0.4809(6) 0.078(3) Uani 1 d . . O21 O 0.8977(6) 0.3054(13) 0.1957(6) 0.079(3) Uani 1 d . . O22 O 0.6954(7) 0.0942(10) 0.2457(6) 0.074(3) Uani 1 d . . O31 O 0.9163(8) 0.0895(14) 0.5298(6) 0.091(4) Uani 1 d . . O32 O 0.9342(7) 0.0227(13) 0.3017(7) 0.094(4) Uani 1 d . . O33 O 0.7113(6) -0.0426(12) 0.4136(8) 0.088(4) Uani 1 d . . O41 O 0.8741(6) 0.4600(13) 0.5691(6) 0.077(3) Uani 1 d . . O42 O 1.0147(6) 0.3019(12) 0.4149(8) 0.086(4) Uani 1 d . . O51 O 0.6133(6) 0.7473(13) 0.3003(6) 0.081(3) Uani 1 d . . O52 O 0.6265(6) 0.4006(12) 0.1869(6) 0.067(3) Uani 1 d . . H12 H 0.6938 0.4437 0.3469 0.080 Uiso 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 0.0312(2) 0.0367(3) 0.0333(2) -0.0048(2) 0.0044(2) -0.0005(2) Os2 0.0375(2) 0.0321(2) 0.0341(2) -0.0037(2) 0.0070(2) 0.0032(2) Os3 0.0411(2) 0.0286(2) 0.0479(3) -0.0008(2) 0.0057(2) 0.0037(2) Ru4 0.0329(4) 0.0327(5) 0.0530(6) -0.0024(4) 0.0002(4) -0.0017(4) Ru5 0.0651(6) 0.0405(6) 0.0409(6) 0.0062(5) 0.0108(5) 0.0102(5) P1 0.0360(15) 0.047(2) 0.055(2) -0.003(2) 0.0096(13) -0.0062(13) O101 0.068(7) 0.108(10) 0.109(10) 0.047(9) 0.021(7) -0.012(7) O102 0.053(6) 0.077(7) 0.103(9) -0.048(7) 0.003(6) -0.006(5) O103 0.042(5) 0.075(7) 0.083(7) -0.006(6) 0.000(5) 0.014(5) C102 0.070(11) 0.110(17) 0.182(25) -0.059(17) -0.015(13) -0.023(12) C103 0.083(12) 0.098(15) 0.122(17) 0.055(14) -0.037(11) -0.023(11) C1 0.099(19) 0.048(22) 0.073(18) 0.001(17) 0.053(16) 0.009(18) C2 0.120(26) 0.048(19) 0.087(22) 0.009(17) 0.038(22) 0.022(20) C3 0.116(22) 0.049(24) 0.070(23) 0.027(19) 0.028(18) 0.013(19) C4 0.130(26) 0.058(21) 0.040(15) 0.004(17) 0.017(21) 0.020(20) C5 0.111(24) 0.025(16) 0.072(22) 0.011(16) 0.036(19) -0.002(18) C1A 0.104(20) 0.033(17) 0.069(16) 0.015(13) 0.032(16) 0.008(16) C2A 0.096(21) 0.029(15) 0.090(22) 0.010(15) 0.022(19) -0.008(15) C3A 0.123(21) 0.049(23) 0.045(16) 0.016(17) 0.017(16) 0.014(17) C4A 0.131(27) 0.061(18) 0.043(16) 0.001(14) 0.034(20) 0.018(20) C5A 0.088(18) 0.057(21) 0.066(17) -0.018(16) 0.045(15) -0.010(16) C1' 0.052(7) 0.035(7) 0.059(8) 0.009(6) -0.009(6) 0.004(5) C2' 0.069(9) 0.031(7) 0.091(11) -0.009(7) -0.016(8) -0.004(6) C3' 0.055(8) 0.045(8) 0.115(14) 0.036(9) -0.016(9) -0.017(7) C4' 0.051(7) 0.056(9) 0.075(10) 0.022(8) 0.014(7) -0.007(6) C5' 0.044(6) 0.031(6) 0.057(8) 0.007(6) 0.012(5) -0.009(5) C11 0.047(7) 0.077(10) 0.034(7) 0.010(7) -0.001(5) -0.004(6) C12 0.051(7) 0.047(8) 0.045(7) -0.016(6) 0.006(5) 0.008(6) C21 0.054(7) 0.050(8) 0.061(9) -0.005(7) 0.004(7) 0.005(6) C22 0.052(7) 0.058(9) 0.052(8) -0.010(7) 0.010(6) 0.004(6) C31 0.048(7) 0.060(9) 0.054(8) 0.010(7) 0.004(6) 0.002(6) C32 0.057(8) 0.048(8) 0.074(10) 0.003(8) 0.002(7) 0.008(7) C33 0.066(8) 0.040(8) 0.070(10) 0.007(7) 0.003(7) -0.001(7) C41 0.048(7) 0.039(7) 0.077(10) -0.011(7) -0.003(7) 0.004(6) C42 0.045(8) 0.055(9) 0.090(11) 0.001(8) 0.007(7) -0.001(6) C51 0.053(7) 0.049(8) 0.051(8) 0.000(7) -0.006(6) 0.000(6) C52 0.062(8) 0.060(9) 0.036(7) 0.001(6) 0.002(6) 0.019(7) O11 0.078(7) 0.125(11) 0.048(6) 0.021(7) 0.002(5) -0.009(7) O12 0.076(7) 0.077(8) 0.081(8) -0.040(6) 0.004(6) 0.017(6) O21 0.078(7) 0.095(9) 0.070(7) -0.005(6) 0.047(6) 0.016(6) O22 0.109(8) 0.039(5) 0.073(7) -0.028(5) 0.008(6) -0.014(6) O31 0.096(8) 0.106(10) 0.067(7) 0.031(7) -0.010(7) 0.003(7) O32 0.105(9) 0.074(8) 0.108(10) -0.010(7) 0.044(8) 0.040(7) O33 0.071(7) 0.050(7) 0.144(12) 0.013(7) 0.006(7) -0.015(6) O41 0.076(7) 0.094(9) 0.060(7) -0.007(6) -0.011(5) -0.015(6) O42 0.038(5) 0.071(8) 0.150(12) -0.024(8) 0.008(6) 0.009(5) O51 0.067(7) 0.089(8) 0.087(8) -0.020(7) 0.013(6) 0.029(6) O52 0.053(5) 0.079(7) 0.067(7) -0.011(6) -0.014(5) 0.014(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 Os1 C11 1.880(13) . ? Os1 C12 1.897(12) . ? Os1 P1 2.253(3) . ? Os1 Os3 2.7480(8) . ? Os1 Ru4 2.8768(13) . ? Os1 Os2 2.9552(11) . ? Os2 C22 1.885(15) . ? Os2 C21 1.911(14) . ? Os2 C52 2.050(13) . ? Os2 C5' 2.432(11) . ? Os2 Os3 2.7905(9) . ? Os2 Ru5 2.8164(12) . ? Os2 Ru4 2.9272(14) . ? Os3 C31 1.881(14) . ? Os3 C33 1.894(15) . ? Os3 C32 1.94(2) . ? Os3 Ru4 2.8931(12) . ? Ru4 C41 1.89(2) . ? Ru4 C42 1.903(15) . ? Ru4 C2' 2.239(13) . ? Ru4 C4' 2.253(13) . ? Ru4 C3' 2.255(13) . ? Ru4 C1' 2.256(12) . ? Ru4 C5' 2.325(13) . ? Ru5 C51 1.864(15) . ? Ru5 C52 2.03(2) . ? Ru5 C5' 2.114(13) . ? Ru5 C3 2.18(4) . ? Ru5 C2A 2.23(4) . ? Ru5 C3A 2.24(3) . ? Ru5 C4 2.24(5) . ? Ru5 C5 2.25(5) . ? Ru5 C2 2.26(5) . ? Ru5 C1 2.26(2) . ? Ru5 C1A 2.28(3) . ? Ru5 C4A 2.32(4) . ? P1 O102 1.561(10) . ? P1 O101 1.573(12) . ? P1 O103 1.578(10) . ? O101 C111 1.37(3) . ? O101 C101 1.40(3) . ? O102 C102 1.42(2) . ? O103 C103 1.41(2) . ? C1 C2 1.42(2) . ? C1 C5 1.42(2) . ? C2 C3 1.42(2) . ? C3 C4 1.41(2) . ? C4 C5 1.43(2) . ? C1A C2A 1.42(2) . ? C1A C5A 1.43(2) . ? C2A C3A 1.42(2) . ? C3A C4A 1.42(2) . ? C4A C5A 1.42(2) . ? C1' C5' 1.41(2) . ? C1' C2' 1.45(2) . ? C2' C3' 1.42(2) . ? C3' C4' 1.39(2) . ? C4' C5' 1.48(2) . ? C11 O11 1.14(2) . ? C12 O12 1.147(15) . ? C21 O21 1.14(2) . ? C22 O22 1.15(2) . ? C31 O31 1.15(2) . ? C32 O32 1.13(2) . ? C33 O33 1.11(2) . ? C41 O41 1.16(2) . ? C42 O42 1.13(2) . ? C51 O51 1.13(2) . ? C52 O52 1.18(2) . ? 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 97.3(6) . . ? C11 Os1 P1 91.2(4) . . ? C12 Os1 P1 89.3(4) . . ? C11 Os1 Os3 87.0(4) . . ? C12 Os1 Os3 160.8(4) . . ? P1 Os1 Os3 109.41(9) . . ? C11 Os1 Ru4 102.5(4) . . ? C12 Os1 Ru4 98.9(4) . . ? P1 Os1 Ru4 162.89(9) . . ? Os3 Os1 Ru4 61.86(3) . . ? C11 Os1 Os2 145.3(4) . . ? C12 Os1 Os2 114.3(4) . . ? P1 Os1 Os2 102.71(9) . . ? Os3 Os1 Os2 58.45(2) . . ? Ru4 Os1 Os2 60.24(3) . . ? C22 Os2 C21 88.2(6) . . ? C22 Os2 C52 83.9(6) . . ? C21 Os2 C52 99.3(6) . . ? C22 Os2 C5' 175.3(5) . . ? C21 Os2 C5' 91.9(5) . . ? C52 Os2 C5' 91.4(5) . . ? C22 Os2 Os3 73.7(4) . . ? C21 Os2 Os3 93.2(4) . . ? C52 Os2 Os3 154.0(4) . . ? C5' Os2 Os3 111.0(3) . . ? C22 Os2 Ru5 128.5(4) . . ? C21 Os2 Ru5 88.8(4) . . ? C52 Os2 Ru5 46.0(4) . . ? C5' Os2 Ru5 46.8(3) . . ? Os3 Os2 Ru5 157.78(3) . . ? C22 Os2 Ru4 134.3(4) . . ? C21 Os2 Ru4 97.5(4) . . ? C52 Os2 Ru4 138.6(4) . . ? C5' Os2 Ru4 50.4(3) . . ? Os3 Os2 Ru4 60.74(3) . . ? Ru5 Os2 Ru4 97.05(4) . . ? C22 Os2 Os1 94.3(4) . . ? C21 Os2 Os1 147.6(4) . . ? C52 Os2 Os1 113.1(4) . . ? C5' Os2 Os1 88.2(3) . . ? Os3 Os2 Os1 57.06(2) . . ? Ru5 Os2 Os1 113.80(3) . . ? Ru4 Os2 Os1 58.55(3) . . ? C31 Os3 C33 88.3(6) . . ? C31 Os3 C32 94.0(6) . . ? C33 Os3 C32 99.6(6) . . ? C31 Os3 Os1 104.8(4) . . ? C33 Os3 Os1 86.0(4) . . ? C32 Os3 Os1 160.6(4) . . ? C31 Os3 Os2 159.1(4) . . ? C33 Os3 Os2 107.8(4) . . ? C32 Os3 Os2 96.2(4) . . ? Os1 Os3 Os2 64.49(3) . . ? C31 Os3 Ru4 97.3(4) . . ? C33 Os3 Ru4 147.2(4) . . ? C32 Os3 Ru4 112.2(4) . . ? Os1 Os3 Ru4 61.26(3) . . ? Os2 Os3 Ru4 61.97(3) . . ? C41 Ru4 C42 90.2(7) . . ? C41 Ru4 C2' 91.7(6) . . ? C42 Ru4 C2' 128.4(6) . . ? C41 Ru4 C4' 148.3(6) . . ? C42 Ru4 C4' 95.8(6) . . ? C2' Ru4 C4' 60.4(6) . . ? C41 Ru4 C3' 112.4(7) . . ? C42 Ru4 C3' 96.4(6) . . ? C2' Ru4 C3' 36.9(6) . . ? C4' Ru4 C3' 36.0(6) . . ? C41 Ru4 C1' 107.8(5) . . ? C42 Ru4 C1' 155.4(6) . . ? C2' Ru4 C1' 37.6(5) . . ? C4' Ru4 C1' 60.1(5) . . ? C3' Ru4 C1' 61.7(5) . . ? C41 Ru4 C5' 143.1(5) . . ? C42 Ru4 C5' 126.1(6) . . ? C2' Ru4 C5' 62.1(5) . . ? C4' Ru4 C5' 37.7(4) . . ? C3' Ru4 C5' 62.6(5) . . ? C1' Ru4 C5' 35.9(5) . . ? C41 Ru4 Os1 74.2(4) . . ? C42 Ru4 Os1 116.4(4) . . ? C2' Ru4 Os1 113.6(4) . . ? C4' Ru4 Os1 128.8(4) . . ? C3' Ru4 Os1 146.9(4) . . ? C1' Ru4 Os1 85.2(3) . . ? C5' Ru4 Os1 92.2(3) . . ? C41 Ru4 Os3 90.3(4) . . ? C42 Ru4 Os3 62.2(4) . . ? C2' Ru4 Os3 169.2(4) . . ? C4' Ru4 Os3 120.0(4) . . ? C3' Ru4 Os3 149.5(5) . . ? C1' Ru4 Os3 132.0(3) . . ? C5' Ru4 Os3 110.9(3) . . ? Os1 Ru4 Os3 56.88(2) . . ? C41 Ru4 Os2 134.1(4) . . ? C42 Ru4 Os2 99.7(5) . . ? C2' Ru4 Os2 114.7(4) . . ? C4' Ru4 Os2 75.5(4) . . ? C3' Ru4 Os2 110.8(5) . . ? C1' Ru4 Os2 79.9(3) . . ? C5' Ru4 Os2 53.7(3) . . ? Os1 Ru4 Os2 61.21(3) . . ? Os3 Ru4 Os2 57.29(2) . . ? C51 Ru5 C52 87.5(5) . . ? C51 Ru5 C5' 91.0(5) . . ? C52 Ru5 C5' 101.9(5) . . ? C51 Ru5 C3 95.1(12) . . ? C52 Ru5 C3 108.8(13) . . ? C5' Ru5 C3 148.9(12) . . ? C51 Ru5 C2A 93.9(10) . . ? C52 Ru5 C2A 131.4(12) . . ? C5' Ru5 C2A 126.6(12) . . ? C51 Ru5 C3A 106.5(11) . . ? C52 Ru5 C3A 96.4(10) . . ? C5' Ru5 C3A 155.1(9) . . ? C2A Ru5 C3A 36.9(7) . . ? C51 Ru5 C4 125.8(15) . . ? C52 Ru5 C4 88.1(10) . . ? C5' Ru5 C4 142.5(15) . . ? C3 Ru5 C4 37.2(7) . . ? C51 Ru5 C5 156.9(10) . . ? C52 Ru5 C5 104.1(12) . . ? C5' Ru5 C5 105.7(14) . . ? C3 Ru5 C5 62.4(11) . . ? C4 Ru5 C5 37.1(7) . . ? C51 Ru5 C2 98.0(10) . . ? C52 Ru5 C2 145.8(12) . . ? C5' Ru5 C2 111.7(12) . . ? C3 Ru5 C2 37.3(7) . . ? C4 Ru5 C2 61.3(12) . . ? C5 Ru5 C2 61.3(11) . . ? C51 Ru5 C1 129.8(12) . . ? C52 Ru5 C1 140.6(12) . . ? C5' Ru5 C1 90.9(6) . . ? C3 Ru5 C1 62.0(9) . . ? C4 Ru5 C1 61.3(9) . . ? C5 Ru5 C1 36.7(6) . . ? C2 Ru5 C1 36.5(6) . . ? C51 Ru5 C1A 116.6(11) . . ? C52 Ru5 C1A 150.2(9) . . ? C5' Ru5 C1A 95.4(9) . . ? C2A Ru5 C1A 36.7(6) . . ? C3A Ru5 C1A 61.2(9) . . ? C51 Ru5 C4A 141.9(13) . . ? C52 Ru5 C4A 89.9(9) . . ? C5' Ru5 C4A 126.6(13) . . ? C2A Ru5 C4A 60.6(11) . . ? C3A Ru5 C4A 36.2(6) . . ? C1A Ru5 C4A 60.3(10) . . ? O102 P1 O101 101.7(8) . . ? O102 P1 O103 104.4(6) . . ? O101 P1 O103 98.6(6) . . ? O102 P1 Os1 112.0(4) . . ? O101 P1 Os1 117.6(5) . . ? O103 P1 Os1 120.0(4) . . ? C111 O101 P1 151.9(37) . . ? C101 O101 P1 117.2(18) . . ? C102 O102 P1 124.7(12) . . ? C103 O103 P1 120.4(11) . . ? C2 C1 C5 108.3(15) . . ? C2 C1 Ru5 71.6(24) . . ? C5 C1 Ru5 71.1(20) . . ? C1 C2 C3 107.7(16) . . ? C1 C2 Ru5 71.9(21) . . ? C3 C2 Ru5 68.4(25) . . ? C4 C3 C2 108.3(16) . . ? C4 C3 Ru5 73.8(25) . . ? C2 C3 Ru5 74.4(28) . . ? C3 C4 C5 107.8(16) . . ? C3 C4 Ru5 69.0(24) . . ? C5 C4 Ru5 71.7(23) . . ? C1 C5 C4 107.7(15) . . ? C1 C5 Ru5 72.3(18) . . ? C4 C5 Ru5 71.3(23) . . ? C2A C1A C5A 107.0(15) . . ? C2A C1A Ru5 69.8(22) . . ? C5A C1A Ru5 74.8(19) . . ? C3A C2A C1A 108.6(15) . . ? C3A C2A Ru5 72.1(20) . . ? C1A C2A Ru5 73.5(21) . . ? C2A C3A C4A 108.2(16) . . ? C2A C3A Ru5 71.0(21) . . ? C4A C3A Ru5 75.1(22) . . ? C5A C4A C3A 107.5(16) . . ? C5A C4A Ru5 73.3(21) . . ? C3A C4A Ru5 68.8(20) . . ? C4A C5A C1A 108.7(16) . . ? C4A C5A Ru5 71.4(21) . . ? C1A C5A Ru5 69.3(18) . . ? C5' C1' C2' 111.0(12) . . ? C5' C1' Ru4 74.7(7) . . ? C2' C1' Ru4 70.6(7) . . ? C3' C2' C1' 107.4(14) . . ? C3' C2' Ru4 72.1(8) . . ? C1' C2' Ru4 71.8(7) . . ? C4' C3' C2' 106.8(13) . . ? C4' C3' Ru4 71.9(8) . . ? C2' C3' Ru4 71.0(8) . . ? C3' C4' C5' 112.0(14) . . ? C3' C4' Ru4 72.1(9) . . ? C5' C4' Ru4 73.8(7) . . ? C1' C5' C4' 102.7(12) . . ? C1' C5' Ru5 122.1(9) . . ? C4' C5' Ru5 125.7(10) . . ? C1' C5' Ru4 69.4(7) . . ? C4' C5' Ru4 68.5(7) . . ? Ru5 C5' Ru4 151.7(6) . . ? C1' C5' Os2 119.9(8) . . ? C4' C5' Os2 108.1(9) . . ? Ru5 C5' Os2 76.2(4) . . ? Ru4 C5' Os2 75.9(3) . . ? O11 C11 Os1 177.3(12) . . ? O12 C12 Os1 174.8(11) . . ? O21 C21 Os2 179.1(13) . . ? O22 C22 Os2 171.8(13) . . ? O31 C31 Os3 176.6(13) . . ? O32 C32 Os3 175.1(14) . . ? O33 C33 Os3 175.0(13) . . ? O41 C41 Ru4 174.3(12) . . ? O42 C42 Ru4 160.6(13) . . ? O51 C51 Ru5 176.6(12) . . ? O52 C52 Ru5 135.5(11) . . ? O52 C52 Os2 137.1(12) . . ? Ru5 C52 Os2 87.3(6) . . ? _refine_diff_density_max 2.093 _refine_diff_density_min -2.596 _refine_diff_density_rms 0.224