# Copyright The Royal Society of Chemistry, 1998 # Manuscript No. 7/08714D/DAP data_global _publ_contact_author 'G. P. Shields' _publ_contact_author_email shields@ccdc.cam.ac.uk loop_ _publ_author_name Buntem,R. Lewis,J. Morewood,C.A. Raithby,P.R. Ramirez de Arellano,M.C. Shields,G.P. _journal_name_full 'J. Chem. Soc., Dalton Trans.' _journal_volume '' _journal_page_first '' _journal_page_last '' _journal_year '' data_cam15 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H6 O11 Os3 Ru' _chemical_formula_weight 1045.88 _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' '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 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 8.718(2) _cell_length_b 14.026(3) _cell_length_c 33.224(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4062.6(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 20 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.420 _exptl_crystal_density_method ? _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 19.492 _exptl_absorpt_correction_type Semiempirical _exptl_absorpt_correction_T_min 0.164 _exptl_absorpt_correction_T_max 0.047 _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 'Siemens R3mV' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6292 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 22.55 _reflns_number_total 5329 _reflns_number_observed 4498 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics Shelxtl-Plus _computing_publication_material Shelxl-92 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 15 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^)+(0.0700P)^2^+166.4709P] 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 0.22(2) _refine_ls_number_reflns 5314 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_obs 0.0546 _refine_ls_wR_factor_all 0.1503 _refine_ls_wR_factor_obs 0.1261 _refine_ls_goodness_of_fit_all 1.048 _refine_ls_goodness_of_fit_obs 1.032 _refine_ls_restrained_S_all 1.125 _refine_ls_restrained_S_obs 1.032 _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 -0.0611(2) -0.07035(9) 0.66237(4) 0.0299(3) Uani 1 d . . Os2 Os -0.36802(15) 0.00908(9) 0.64703(4) 0.0335(3) Uani 1 d . . Os3 Os -0.2539(2) -0.01217(9) 0.72449(4) 0.0325(3) Uani 1 d . . Ru Ru -0.1231(3) 0.1237(2) 0.67452(8) 0.0288(6) Uani 1 d . . O11 O 0.1200(31) 0.0879(18) 0.6129(8) 0.058(7) Uani 1 d . . O12 O -0.1836(35) -0.2634(17) 0.6918(8) 0.060(8) Uani 1 d . . O13 O 0.2135(33) -0.0783(24) 0.7175(8) 0.070(9) Uani 1 d . . O14 O 0.1075(38) -0.1509(20) 0.5914(8) 0.065(8) Uani 1 d . . O21 O -0.4819(40) 0.0156(22) 0.5602(7) 0.073(10) Uani 1 d . . O22 O -0.6227(33) 0.1324(19) 0.6803(10) 0.070(9) Uani 1 d . . O23 O -0.5319(40) -0.1779(22) 0.6645(10) 0.079(10) Uani 1 d . . O24 O -0.2589(43) 0.1875(19) 0.5963(8) 0.074(10) Uani 1 d . . O31 O -0.4095(47) -0.1860(21) 0.7607(11) 0.093(13) Uani 1 d . . O32 O -0.0120(36) -0.0080(25) 0.7885(7) 0.071(9) Uani 1 d . . O33 O -0.4595(38) 0.1250(22) 0.7707(12) 0.087(11) Uani 1 d . . C11 C 0.0184(42) 0.0637(23) 0.6368(11) 0.039(9) Uiso 1 d . . C12 C -0.1384(53) -0.1867(29) 0.6840(14) 0.060(11) Uiso 1 d . . C13 C 0.1103(41) -0.0736(21) 0.6977(11) 0.032(8) Uiso 1 d . . C14 C 0.0442(49) -0.1202(27) 0.6189(14) 0.051(10) Uiso 1 d . . C21 C -0.4489(48) 0.0116(27) 0.5919(13) 0.053(10) Uiso 1 d . . C22 C -0.5300(42) 0.0862(24) 0.6687(11) 0.040(9) Uiso 1 d . . C23 C -0.4759(50) -0.1073(29) 0.6615(14) 0.055(11) Uiso 1 d . . C24 C -0.2482(45) 0.1371(25) 0.6238(12) 0.044(9) Uiso 1 d . . C31 C -0.3495(46) -0.1195(27) 0.7482(13) 0.049(10) Uiso 1 d . . C32 C -0.1069(42) -0.0117(24) 0.7668(11) 0.041(8) Uiso 1 d . . C33 C -0.3843(44) 0.0712(25) 0.7518(12) 0.042(9) Uiso 1 d . . C1 C -0.1055(42) 0.2013(23) 0.7345(12) 0.043(9) Uiso 1 d . . H1 H -0.1394(42) 0.1765(23) 0.7589(12) 0.051 Uiso 1 calc R . C2 C 0.0404(40) 0.1922(21) 0.7194(11) 0.036(8) Uiso 1 d . . H2 H 0.1214(40) 0.1592(21) 0.7312(11) 0.043 Uiso 1 calc R . C3 C 0.0443(42) 0.2429(22) 0.6824(11) 0.039(8) Uiso 1 d . . H3 H 0.1296(42) 0.2487(22) 0.6657(11) 0.046 Uiso 1 calc R . C4 C -0.1058(42) 0.2843(24) 0.6745(12) 0.043(9) Uiso 1 d . . H4 H -0.1364(42) 0.3221(24) 0.6529(12) 0.052 Uiso 1 calc R . C5 C -0.1938(44) 0.2529(23) 0.7078(11) 0.042(9) Uiso 1 d . . H5 H -0.2977(44) 0.2655(23) 0.7112(11) 0.050 Uiso 1 calc R . Os1' Os 0.3732(2) 0.01381(9) 0.89310(4) 0.0329(3) Uani 1 d . . Os2' Os 0.67421(15) 0.09848(8) 0.91107(4) 0.0287(3) Uani 1 d . . Os3' Os 0.4648(2) 0.05215(9) 0.97111(4) 0.0320(3) Uani 1 d . . Ru' Ru 0.6123(3) -0.0923(2) 0.92921(9) 0.0297(6) Uani 1 d . . O11' O 0.3111(37) -0.0105(26) 0.8021(8) 0.080(10) Uani 1 d . . O12' O 0.1881(36) 0.1986(17) 0.9028(9) 0.063(8) Uani 1 d . . O13' O 0.1205(37) -0.1069(21) 0.9281(11) 0.081(10) Uani 1 d . . O14' O 0.4907(45) -0.1768(21) 0.8551(10) 0.083(11) Uani 1 d . . O21' O 0.8592(35) -0.0629(19) 0.8691(9) 0.069(9) Uani 1 d . . O22' O 0.9440(32) 0.1081(22) 0.9671(8) 0.061(8) Uani 1 d . . O23' O 0.5375(32) 0.2956(16) 0.9339(9) 0.057(8) Uani 1 d . . O24' O 0.8428(41) 0.1749(19) 0.8378(10) 0.076(9) Uani 1 d . . O31' O 0.6852(37) 0.0730(22) 1.0410(7) 0.068(9) Uani 1 d . . O32' O 0.2746(36) 0.2249(15) 0.9944(10) 0.067(9) Uani 1 d . . O33' O 0.2534(41) -0.0766(21) 1.0163(10) 0.089(12) Uani 1 d . . C11' C 0.3245(43) 0.0024(25) 0.8323(13) 0.044(9) Uiso 1 d . . C12' C 0.2503(52) 0.1290(30) 0.8997(14) 0.060(11) Uiso 1 d . . C13' C 0.2139(39) -0.0617(22) 0.9175(10) 0.033(8) Uiso 1 d . . C14' C 0.5028(49) -0.1209(29) 0.8805(14) 0.057(11) Uiso 1 d . . C21' C 0.7631(41) -0.0394(22) 0.8886(11) 0.035(8) Uiso 1 d . . C22' C 0.8392(37) 0.1047(21) 0.9473(10) 0.028(7) Uiso 1 d . . C23' C 0.5893(44) 0.2177(26) 0.9273(12) 0.046(10) Uiso 1 d . . C24' C 0.7865(48) 0.1449(28) 0.8681(13) 0.051(10) Uiso 1 d . . C31' C 0.5994(43) 0.0664(24) 1.0146(12) 0.042(9) Uiso 1 d . . C32' C 0.3503(42) 0.1588(24) 0.9851(11) 0.041(9) Uiso 1 d . . C33' C 0.3372(45) -0.0283(25) 0.9982(12) 0.047(10) Uiso 1 d . . C1' C 0.6402(53) -0.2466(29) 0.9367(14) 0.064(12) Uiso 1 d . . H1' H 0.6102(53) -0.2866(29) 0.9158(14) 0.077 Uiso 1 calc R . C2' C 0.5457(63) -0.2137(31) 0.9677(16) 0.075(14) Uiso 1 d . . H2' H 0.4427(63) -0.2296(31) 0.9704(16) 0.090 Uiso 1 calc R . C3' C 0.6213(45) -0.1573(25) 0.9925(12) 0.047(10) Uiso 1 d . . H3' H 0.5863(45) -0.1297(25) 1.0162(12) 0.057 Uiso 1 calc R . C4' C 0.7647(55) -0.1487(30) 0.9750(15) 0.067(12) Uiso 1 d . . H4' H 0.8390(55) -0.1065(30) 0.9843(15) 0.081 Uiso 1 calc R . C5' C 0.7876(52) -0.2092(28) 0.9422(14) 0.059(12) Uiso 1 d . . H5' H 0.8769(52) -0.2214(28) 0.9278(14) 0.071 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0304(7) 0.0309(7) 0.0285(8) -0.0002(6) 0.0012(6) 0.0079(6) Os2 0.0284(7) 0.0337(7) 0.0384(8) -0.0036(6) -0.0034(7) 0.0037(6) Os3 0.0360(7) 0.0338(7) 0.0277(7) 0.0014(6) 0.0064(6) 0.0023(6) Ru 0.0283(14) 0.0287(13) 0.029(2) -0.0002(11) -0.0008(13) 0.0022(12) O11 0.058(17) 0.065(16) 0.052(18) 0.003(14) 0.022(15) -0.002(15) O12 0.088(22) 0.045(14) 0.046(17) 0.003(13) 0.034(16) -0.021(15) O13 0.057(18) 0.115(25) 0.039(17) 0.023(17) -0.010(15) 0.028(17) O14 0.090(23) 0.074(18) 0.032(17) 0.002(14) -0.009(17) 0.011(17) O21 0.119(28) 0.084(19) 0.015(14) 0.003(13) -0.037(16) 0.023(20) O22 0.050(17) 0.062(17) 0.097(25) -0.014(17) 0.033(18) 0.022(15) O23 0.086(24) 0.080(20) 0.071(24) -0.013(17) 0.032(20) -0.048(19) O24 0.136(30) 0.062(17) 0.026(16) 0.028(13) -0.011(18) -0.021(18) O31 0.137(34) 0.062(18) 0.080(26) 0.006(17) 0.056(25) -0.035(21) O32 0.077(21) 0.121(25) 0.014(14) 0.013(15) -0.007(14) -0.015(20) O33 0.068(21) 0.069(19) 0.123(33) -0.002(20) 0.008(23) 0.006(17) Os1' 0.0286(7) 0.0355(7) 0.0348(8) 0.0006(6) -0.0035(6) -0.0035(6) Os2' 0.0278(7) 0.0285(6) 0.0299(8) 0.0003(6) 0.0008(6) -0.0047(5) Os3' 0.0338(8) 0.0335(7) 0.0288(8) -0.0005(6) 0.0062(7) 0.0011(6) Ru' 0.0303(14) 0.0253(13) 0.034(2) 0.0023(12) 0.0012(13) 0.0005(12) O11' 0.083(22) 0.125(26) 0.031(17) -0.031(18) -0.026(16) -0.019(21) O12' 0.087(21) 0.049(15) 0.053(19) -0.008(13) -0.004(17) 0.041(15) O13' 0.072(20) 0.074(20) 0.099(27) 0.015(18) 0.005(20) -0.055(18) O14' 0.125(32) 0.070(19) 0.054(22) -0.006(16) -0.028(22) -0.013(20) O21' 0.067(20) 0.068(17) 0.071(21) 0.004(15) 0.052(18) 0.019(16) O22' 0.050(16) 0.109(22) 0.024(15) -0.031(15) -0.008(14) 0.006(16) O23' 0.056(17) 0.031(13) 0.083(22) -0.010(13) 0.017(16) 0.006(13) O24' 0.093(25) 0.060(17) 0.074(24) 0.001(16) -0.004(21) -0.021(17) O31' 0.078(20) 0.112(24) 0.014(14) 0.003(15) 0.014(14) -0.013(19) O32' 0.086(22) 0.026(13) 0.090(23) -0.011(14) 0.018(19) 0.028(14) O33' 0.109(27) 0.068(19) 0.090(26) 0.029(17) 0.074(23) 0.012(19) _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 C14 1.85(5) . ? Os1 C13 1.90(4) . ? Os1 C12 1.91(4) . ? Os1 C11 2.18(3) . ? Os1 Os3 2.784(2) . ? Os1 Ru 2.804(3) . ? Os1 Os2 2.943(2) . ? Os2 C22 1.92(4) . ? Os2 C23 1.94(4) . ? Os2 C21 1.96(4) . ? Os2 C24 2.22(4) . ? Os2 Os3 2.775(2) . ? Os2 Ru 2.824(3) . ? Os3 C33 1.87(4) . ? Os3 C31 1.89(4) . ? Os3 C32 1.90(4) . ? Os3 Ru 2.772(3) . ? Ru C11 1.95(4) . ? Ru C24 2.01(4) . ? Ru C5 2.21(3) . ? Ru C3 2.23(3) . ? Ru C4 2.26(3) . ? Ru C1 2.28(4) . ? Ru C2 2.28(3) . ? O11 C11 1.24(4) . ? O12 C12 1.17(4) . ? O13 C13 1.12(4) . ? O14 C14 1.15(5) . ? O21 C21 1.10(5) . ? O22 C22 1.11(4) . ? O23 C23 1.11(4) . ? O24 C24 1.16(4) . ? O31 C31 1.15(4) . ? O32 C32 1.10(4) . ? O33 C33 1.18(5) . ? C1 C2 1.37(5) . ? C1 C5 1.38(5) . ? C2 C3 1.42(5) . ? C3 C4 1.46(5) . ? C4 C5 1.42(5) . ? Os1' C13' 1.93(4) . ? Os1' C12' 1.95(4) . ? Os1' C11' 2.07(4) . ? Os1' C14' 2.24(4) . ? Os1' Os3' 2.765(2) . ? Os1' Ru' 2.828(3) . ? Os1' Os2' 2.942(2) . ? Os2' C24' 1.85(5) . ? Os2' C22' 1.88(3) . ? Os2' C23' 1.91(4) . ? Os2' C21' 2.21(3) . ? Os2' Os3' 2.781(2) . ? Os2' Ru' 2.795(3) . ? Os3' C33' 1.82(4) . ? Os3' C32' 1.86(4) . ? Os3' C31' 1.87(4) . ? Os3' Ru' 2.774(3) . ? Ru' C14' 1.92(5) . ? Ru' C21' 2.03(4) . ? Ru' C4' 2.17(5) . ? Ru' C1' 2.19(4) . ? Ru' C2' 2.21(5) . ? Ru' C5' 2.28(4) . ? Ru' C3' 2.29(4) . ? O11' C11' 1.03(4) . ? O12' C12' 1.12(5) . ? O13' C13' 1.09(4) . ? O14' C14' 1.16(5) . ? O21' C21' 1.11(4) . ? O22' C22' 1.13(4) . ? O23' C23' 1.20(4) . ? O24' C24' 1.20(5) . ? O31' C31' 1.16(4) . ? O32' C32' 1.18(4) . ? O33' C33' 1.16(4) . ? C1' C2' 1.40(6) . ? C1' C5' 1.40(6) . ? C2' C3' 1.32(6) . ? C3' C4' 1.38(6) . ? C4' C5' 1.40(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 C14 Os1 C13 94.8(16) . . ? C14 Os1 C12 98.4(18) . . ? C13 Os1 C12 91.4(17) . . ? C14 Os1 C11 82.2(15) . . ? C13 Os1 C11 90.7(13) . . ? C12 Os1 C11 177.8(17) . . ? C14 Os1 Os3 171.8(13) . . ? C13 Os1 Os3 91.4(10) . . ? C12 Os1 Os3 76.0(14) . . ? C11 Os1 Os3 103.2(10) . . ? C14 Os1 Ru 125.1(12) . . ? C13 Os1 Ru 94.9(9) . . ? C12 Os1 Ru 135.1(14) . . ? C11 Os1 Ru 43.8(10) . . ? Os3 Os1 Ru 59.49(7) . . ? C14 Os1 Os2 117.3(13) . . ? C13 Os1 Os2 146.2(10) . . ? C12 Os1 Os2 93.9(14) . . ? C11 Os1 Os2 84.0(10) . . ? Os3 Os1 Os2 57.89(5) . . ? Ru Os1 Os2 58.82(7) . . ? C22 Os2 C23 91.4(16) . . ? C22 Os2 C21 94.3(16) . . ? C23 Os2 C21 94.2(17) . . ? C22 Os2 C24 91.2(14) . . ? C23 Os2 C24 174.0(17) . . ? C21 Os2 C24 80.2(15) . . ? C22 Os2 Os3 88.7(11) . . ? C23 Os2 Os3 81.6(13) . . ? C21 Os2 Os3 174.9(11) . . ? C24 Os2 Os3 103.9(10) . . ? C22 Os2 Ru 96.6(10) . . ? C23 Os2 Ru 139.8(13) . . ? C21 Os2 Ru 124.3(12) . . ? C24 Os2 Ru 45.2(10) . . ? Os3 Os2 Ru 59.34(7) . . ? C22 Os2 Os1 144.9(11) . . ? C23 Os2 Os1 94.6(12) . . ? C21 Os2 Os1 119.7(12) . . ? C24 Os2 Os1 86.5(10) . . ? Os3 Os2 Os1 58.17(5) . . ? Ru Os2 Os1 58.12(6) . . ? C33 Os3 C31 91.6(16) . . ? C33 Os3 C32 92.8(15) . . ? C31 Os3 C32 89.6(16) . . ? C33 Os3 Ru 96.4(11) . . ? C31 Os3 Ru 167.7(12) . . ? C32 Os3 Ru 99.4(10) . . ? C33 Os3 Os2 99.5(12) . . ? C31 Os3 Os2 108.2(12) . . ? C32 Os3 Os2 157.9(10) . . ? Ru Os3 Os2 61.21(7) . . ? C33 Os3 Os1 155.8(11) . . ? C31 Os3 Os1 109.9(12) . . ? C32 Os3 Os1 98.2(10) . . ? Ru Os3 Os1 60.61(7) . . ? Os2 Os3 Os1 63.94(5) . . ? C11 Ru C24 81.1(16) . . ? C11 Ru C5 148.4(14) . . ? C24 Ru C5 101.0(14) . . ? C11 Ru C3 89.1(14) . . ? C24 Ru C3 112.4(14) . . ? C5 Ru C3 60.7(13) . . ? C11 Ru C4 112.8(14) . . ? C24 Ru C4 86.7(14) . . ? C5 Ru C4 36.9(13) . . ? C3 Ru C4 37.8(13) . . ? C11 Ru C1 136.6(15) . . ? C24 Ru C1 136.3(14) . . ? C5 Ru C1 35.8(12) . . ? C3 Ru C1 59.7(13) . . ? C4 Ru C1 61.2(13) . . ? C11 Ru C2 101.9(14) . . ? C24 Ru C2 147.9(13) . . ? C5 Ru C2 60.0(13) . . ? C3 Ru C2 36.7(12) . . ? C4 Ru C2 62.4(13) . . ? C1 Ru C2 35.1(13) . . ? C11 Ru Os3 110.4(10) . . ? C24 Ru Os3 110.0(11) . . ? C5 Ru Os3 98.6(9) . . ? C3 Ru Os3 135.5(9) . . ? C4 Ru Os3 135.5(10) . . ? C1 Ru Os3 80.3(9) . . ? C2 Ru Os3 99.0(8) . . ? C11 Ru Os1 50.7(10) . . ? C24 Ru Os1 94.3(10) . . ? C5 Ru Os1 157.2(9) . . ? C3 Ru Os1 128.1(9) . . ? C4 Ru Os1 162.9(9) . . ? C1 Ru Os1 125.3(9) . . ? C2 Ru Os1 112.6(8) . . ? Os3 Ru Os1 59.90(6) . . ? C11 Ru Os2 91.5(11) . . ? C24 Ru Os2 51.2(11) . . ? C5 Ru Os2 114.7(10) . . ? C3 Ru Os2 163.2(9) . . ? C4 Ru Os2 128.2(10) . . ? C1 Ru Os2 127.3(10) . . ? C2 Ru Os2 157.8(9) . . ? Os3 Ru Os2 59.44(7) . . ? Os1 Ru Os2 63.06(6) . . ? O11 C11 Ru 138.4(27) . . ? O11 C11 Os1 135.6(27) . . ? Ru C11 Os1 85.4(14) . . ? O12 C12 Os1 170.3(39) . . ? O13 C13 Os1 177.2(33) . . ? O14 C14 Os1 178.8(38) . . ? O21 C21 Os2 173.9(40) . . ? O22 C22 Os2 178.1(34) . . ? O23 C23 Os2 170.1(40) . . ? O24 C24 Ru 139.4(33) . . ? O24 C24 Os2 136.9(33) . . ? Ru C24 Os2 83.6(14) . . ? O31 C31 Os3 176.7(38) . . ? O32 C32 Os3 172.9(32) . . ? O33 C33 Os3 176.0(35) . . ? C2 C1 C5 109.3(35) . . ? C2 C1 Ru 72.5(21) . . ? C5 C1 Ru 69.6(21) . . ? C1 C2 C3 106.9(33) . . ? C1 C2 Ru 72.4(21) . . ? C3 C2 Ru 70.1(20) . . ? C2 C3 C4 109.5(33) . . ? C2 C3 Ru 73.2(19) . . ? C4 C3 Ru 72.0(19) . . ? C5 C4 C3 102.8(32) . . ? C5 C4 Ru 69.7(19) . . ? C3 C4 Ru 70.2(18) . . ? C1 C5 C4 111.3(33) . . ? C1 C5 Ru 74.7(21) . . ? C4 C5 Ru 73.4(20) . . ? C13' Os1' C12' 90.7(16) . . ? C13' Os1' C11' 102.7(14) . . ? C12' Os1' C11' 93.5(16) . . ? C13' Os1' C14' 88.7(14) . . ? C12' Os1' C14' 175.0(18) . . ? C11' Os1' C14' 81.7(16) . . ? C13' Os1' Os3' 85.5(10) . . ? C12' Os1' Os3' 83.8(13) . . ? C11' Os1' Os3' 171.4(10) . . ? C14' Os1' Os3' 101.1(12) . . ? C13' Os1' Ru' 93.7(9) . . ? C12' Os1' Ru' 142.4(13) . . ? C11' Os1' Ru' 121.6(10) . . ? C14' Os1' Ru' 42.6(12) . . ? Os3' Os1' Ru' 59.46(7) . . ? C13' Os1' Os2' 141.3(10) . . ? C12' Os1' Os2' 97.6(13) . . ? C11' Os1' Os2' 114.3(10) . . ? C14' Os1' Os2' 85.9(11) . . ? Os3' Os1' Os2' 58.23(5) . . ? Ru' Os1' Os2' 57.92(6) . . ? C24' Os2' C22' 94.1(16) . . ? C24' Os2' C23' 96.6(17) . . ? C22' Os2' C23' 94.3(15) . . ? C24' Os2' C21' 82.0(15) . . ? C22' Os2' C21' 89.4(13) . . ? C23' Os2' C21' 176.2(15) . . ? C24' Os2' Os3' 169.6(12) . . ? C22' Os2' Os3' 93.1(10) . . ? C23' Os2' Os3' 75.4(12) . . ? C21' Os2' Os3' 105.5(9) . . ? C24' Os2' Ru' 127.3(12) . . ? C22' Os2' Ru' 93.1(9) . . ? C23' Os2' Ru' 134.7(12) . . ? C21' Os2' Ru' 45.9(9) . . ? Os3' Os2' Ru' 59.66(7) . . ? C24' Os2' Os1' 117.3(13) . . ? C22' Os2' Os1' 146.4(10) . . ? C23' Os2' Os1' 93.8(12) . . ? C21' Os2' Os1' 83.7(9) . . ? Os3' Os2' Os1' 57.70(5) . . ? Ru' Os2' Os1' 59.00(6) . . ? C33' Os3' C32' 92.7(16) . . ? C33' Os3' C31' 93.9(17) . . ? C32' Os3' C31' 93.3(15) . . ? C33' Os3' Os1' 99.6(12) . . ? C32' Os3' Os1' 103.7(11) . . ? C31' Os3' Os1' 157.7(11) . . ? C33' Os3' Ru' 94.5(11) . . ? C32' Os3' Ru' 164.3(11) . . ? C31' Os3' Ru' 100.1(11) . . ? Os1' Os3' Ru' 61.40(7) . . ? C33' Os3' Os2' 154.1(11) . . ? C32' Os3' Os2' 110.1(11) . . ? C31' Os3' Os2' 96.7(11) . . ? Os1' Os3' Os2' 64.06(5) . . ? Ru' Os3' Os2' 60.42(7) . . ? C14' Ru' C21' 80.7(17) . . ? C14' Ru' C4' 144.9(17) . . ? C21' Ru' C4' 101.7(16) . . ? C14' Ru' C1' 86.8(17) . . ? C21' Ru' C1' 111.4(15) . . ? C4' Ru' C1' 59.5(17) . . ? C14' Ru' C2' 101.3(19) . . ? C21' Ru' C2' 147.0(16) . . ? C4' Ru' C2' 58.2(19) . . ? C1' Ru' C2' 37.0(16) . . ? C14' Ru' C5' 110.0(16) . . ? C21' Ru' C5' 87.4(15) . . ? C4' Ru' C5' 36.4(16) . . ? C1' Ru' C5' 36.4(15) . . ? C2' Ru' C5' 60.8(18) . . ? C14' Ru' C3' 134.9(16) . . ? C21' Ru' C3' 137.3(14) . . ? C4' Ru' C3' 36.0(15) . . ? C1' Ru' C3' 60.0(15) . . ? C2' Ru' C3' 34.0(15) . . ? C5' Ru' C3' 61.2(15) . . ? C14' Ru' Os3' 110.2(13) . . ? C21' Ru' Os3' 111.6(9) . . ? C4' Ru' Os3' 101.4(12) . . ? C1' Ru' Os3' 135.7(12) . . ? C2' Ru' Os3' 98.7(13) . . ? C5' Ru' Os3' 137.8(11) . . ? C3' Ru' Os3' 81.1(10) . . ? C14' Ru' Os2' 96.6(12) . . ? C21' Ru' Os2' 51.7(9) . . ? C4' Ru' Os2' 112.5(12) . . ? C1' Ru' Os2' 161.4(12) . . ? C2' Ru' Os2' 156.1(13) . . ? C5' Ru' Os2' 126.8(11) . . ? C3' Ru' Os2' 124.9(9) . . ? Os3' Ru' Os2' 59.91(6) . . ? C14' Ru' Os1' 52.2(12) . . ? C21' Ru' Os1' 90.2(10) . . ? C4' Ru' Os1' 160.2(12) . . ? C1' Ru' Os1' 130.5(12) . . ? C2' Ru' Os1' 117.3(14) . . ? C5' Ru' Os1' 162.1(11) . . ? C3' Ru' Os1' 128.6(10) . . ? Os3' Ru' Os1' 59.14(7) . . ? Os2' Ru' Os1' 63.08(6) . . ? O11' C11' Os1' 172.3(38) . . ? O12' C12' Os1' 175.4(40) . . ? O13' C13' Os1' 174.0(34) . . ? O14' C14' Ru' 143.3(37) . . ? O14' C14' Os1' 131.5(36) . . ? Ru' C14' Os1' 85.2(17) . . ? O21' C21' Ru' 140.5(28) . . ? O21' C21' Os2' 136.2(28) . . ? Ru' C21' Os2' 82.4(13) . . ? O22' C22' Os2' 176.0(29) . . ? O23' C23' Os2' 173.9(35) . . ? O24' C24' Os2' 172.0(37) . . ? O31' C31' Os3' 178.0(34) . . ? O32' C32' Os3' 178.2(31) . . ? O33' C33' Os3' 177.3(33) . . ? C2' C1' C5' 108.8(43) . . ? C2' C1' Ru' 72.1(26) . . ? C5' C1' Ru' 75.3(25) . . ? C3' C2' C1' 111.4(47) . . ? C3' C2' Ru' 76.6(27) . . ? C1' C2' Ru' 70.9(28) . . ? C2' C3' C4' 103.9(43) . . ? C2' C3' Ru' 69.4(28) . . ? C4' C3' Ru' 67.1(26) . . ? C3' C4' C5' 113.8(43) . . ? C3' C4' Ru' 76.9(27) . . ? C5' C4' Ru' 76.2(28) . . ? C4' C5' C1' 101.5(41) . . ? C4' C5' Ru' 67.4(25) . . ? C1' C5' Ru' 68.3(24) . . ? _refine_diff_density_max 2.142 _refine_diff_density_min -2.181 _refine_diff_density_rms 0.368 data_dar10 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C21 H10 O11 Os3 Ru2' _chemical_formula_weight 1211.03 _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' '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.678(3) _cell_length_b 12.117(5) _cell_length_c 10.497(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.59(2) _cell_angle_gamma 90.00 _cell_volume 1228.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 290(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 20 _cell_measurement_theta_max 25 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark orange' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.274 _exptl_crystal_density_method ? _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 16.716 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.005 _exptl_absorpt_correction_T_max 0.739 _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 'Siemens R3mV' _diffrn_measurement_method omega/2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1788 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.030 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 22.54 _reflns_number_total 1619 _reflns_number_observed 1391 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P3' _computing_cell_refinement 'Siemens P3' _computing_data_reduction 'Siemens XDISK' _computing_structure_solution 'SHELXTL (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 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^)+(0.1673P)^2^+0.0000P] 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 'riding on C atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1616 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_obs 0.0680 _refine_ls_wR_factor_all 0.1991 _refine_ls_wR_factor_obs 0.1865 _refine_ls_goodness_of_fit_all 1.071 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_restrained_S_all 1.073 _refine_ls_restrained_S_obs 1.091 _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 0.59903(13) 0.2500 0.58912(12) 0.0510(5) Uani 1 d S . Os2 Os 0.81391(9) 0.13499(7) 0.71667(8) 0.0450(5) Uani 1 d . . Ru1 Ru 0.8828(2) 0.2500 0.9425(2) 0.0432(7) Uani 1 d S . Ru2 Ru 0.6162(2) 0.2500 0.8527(2) 0.0432(7) Uani 1 d S . C11 C 0.6107(50) 0.2500 0.4127(52) 0.092(15) Uani 1 d S . O11 O 0.6219(41) 0.2500 0.2988(29) 0.117(14) Uani 1 d S . C12 C 0.4657(30) 0.1339(26) 0.5837(28) 0.075(9) Uani 1 d . . O12 O 0.3897(21) 0.0611(18) 0.5781(22) 0.087(6) Uani 1 d . . C21 C 1.0057(26) 0.1042(21) 0.7563(23) 0.057(6) Uani 1 d . . O21 O 1.1161(21) 0.0860(16) 0.7628(22) 0.081(6) Uani 1 d . . C22 C 0.8392(37) 0.1275(21) 0.5398(30) 0.076(9) Uani 1 d . . O22 O 0.8733(28) 0.1133(20) 0.4378(20) 0.092(7) Uani 1 d . . C23 C 0.7459(29) -0.0150(22) 0.7195(24) 0.063(7) Uani 1 d . . O23 O 0.6984(28) -0.0987(18) 0.7223(22) 0.096(7) Uani 1 d . . C1 C 0.7445(21) 0.1236(19) 0.9297(23) 0.047(5) Uani 1 d . . O1 O 0.7202(17) 0.0404(13) 0.9857(16) 0.059(4) Uani 1 d . . C2 C 0.9310(27) 0.1963(23) 1.1420(24) 0.069(7) Uani 1 d . . H2 H 0.8725(27) 0.1516(23) 1.1865(24) 0.082 Uiso 1 calc R . C3 C 1.0354(27) 0.1586(26) 1.0626(29) 0.071(8) Uani 1 d . . H3 H 1.0562(27) 0.0859(26) 1.0428(29) 0.085 Uiso 1 calc R . C4 C 1.0972(36) 0.2500 1.0225(38) 0.079(13) Uani 1 d S . H4 H 1.1735(36) 0.2500 0.9729(38) 0.095 Uiso 1 calc SR . C5 C 0.3869(29) 0.2500 0.8210(33) 0.055(8) Uani 1 d S . H5 H 0.3423(29) 0.2500 0.7400(33) 0.066 Uiso 1 calc SR . C6 C 0.4256(24) 0.1579(23) 0.8913(29) 0.067(7) Uani 1 d . . H6 H 0.4134(24) 0.0855(23) 0.8637(29) 0.080 Uiso 1 calc R . C7 C 0.4855(21) 0.1893(19) 1.0094(20) 0.047(5) Uani 1 d . . H7 H 0.5188(21) 0.1431(19) 1.0750(20) 0.056 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0437(8) 0.0626(9) 0.0454(8) 0.000 -0.0084(6) 0.000 Os2 0.0408(7) 0.0468(7) 0.0468(7) -0.0031(3) -0.0025(4) 0.0011(3) Ru1 0.0364(13) 0.0511(14) 0.0414(13) 0.000 -0.0029(10) 0.000 Ru2 0.0352(13) 0.0490(14) 0.0449(13) 0.000 -0.0021(10) 0.000 C11 0.065(27) 0.110(35) 0.097(37) 0.000 -0.037(25) 0.000 O11 0.097(26) 0.203(44) 0.048(17) 0.000 -0.015(16) 0.000 C12 0.047(14) 0.102(23) 0.073(17) -0.045(15) -0.028(13) -0.001(15) O12 0.059(11) 0.091(14) 0.111(16) -0.047(13) 0.008(10) -0.019(12) C21 0.041(15) 0.063(14) 0.065(15) 0.001(12) -0.019(11) 0.017(11) O21 0.051(12) 0.072(12) 0.117(16) -0.004(11) -0.009(10) 0.006(10) C22 0.098(23) 0.053(15) 0.073(20) -0.033(13) -0.014(17) 0.003(13) O22 0.130(21) 0.083(14) 0.063(13) -0.004(11) 0.020(12) 0.017(13) C23 0.072(16) 0.052(15) 0.061(14) -0.010(11) -0.022(12) -0.014(13) O23 0.125(20) 0.065(13) 0.093(15) -0.011(12) -0.022(13) -0.044(14) C1 0.027(10) 0.053(13) 0.060(13) 0.008(10) -0.014(9) 0.005(9) O1 0.056(9) 0.049(9) 0.074(10) 0.004(9) 0.010(8) 0.003(8) C2 0.054(14) 0.089(16) 0.058(14) 0.023(12) -0.034(12) -0.016(12) C3 0.043(14) 0.079(17) 0.090(20) 0.031(15) -0.004(13) 0.008(14) C4 0.030(18) 0.143(43) 0.063(22) 0.000 -0.010(16) 0.000 C5 0.021(14) 0.087(26) 0.060(19) 0.000 0.014(13) 0.000 C6 0.032(11) 0.061(14) 0.109(22) -0.001(15) 0.018(13) -0.010(11) C7 0.031(10) 0.067(13) 0.042(11) 0.018(10) 0.005(8) -0.001(9) _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 1.86(6) . ? Os1 C12 1.91(3) . ? Os1 C12 1.91(3) 4_565 ? Os1 Ru2 2.762(3) . ? Os1 Os2 2.7768(14) 4_565 ? Os1 Os2 2.7768(14) . ? Os2 C22 1.89(3) . ? Os2 C21 1.91(2) . ? Os2 C23 1.93(3) . ? Os2 C1 2.38(3) . ? Os2 Os2 2.787(2) 4_565 ? Os2 Ru1 2.794(2) . ? Os2 Ru2 2.825(2) . ? Ru1 C1 2.03(2) . ? Ru1 C1 2.03(2) 4_565 ? Ru1 C3 2.18(2) 4_565 ? Ru1 C3 2.18(2) . ? Ru1 C4 2.19(3) . ? Ru1 C2 2.22(2) 4_565 ? Ru1 C2 2.22(2) . ? Ru1 Ru2 2.691(3) . ? Ru1 Os2 2.794(2) 4_565 ? Ru2 C1 2.10(2) 4_565 ? Ru2 C1 2.10(2) . ? Ru2 C6 2.22(2) . ? Ru2 C6 2.22(2) 4_565 ? Ru2 C5 2.22(3) . ? Ru2 C7 2.26(2) . ? Ru2 C7 2.26(2) 4_565 ? Ru2 Os2 2.825(2) 4_565 ? C11 O11 1.21(6) . ? C12 O12 1.15(4) . ? C21 O21 1.09(3) . ? C22 O22 1.15(4) . ? C23 O23 1.11(3) . ? C1 O1 1.20(3) . ? C2 C2 1.30(6) 4_565 ? C2 C3 1.43(4) . ? C3 C4 1.34(4) . ? C4 C3 1.34(4) 4_565 ? C5 C6 1.38(3) 4_565 ? C5 C6 1.38(3) . ? C6 C7 1.39(4) . ? C7 C7 1.47(5) 4_565 ? 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 93.1(13) . . ? C11 Os1 C12 93.1(13) . 4_565 ? C12 Os1 C12 95.0(17) . 4_565 ? C11 Os1 Ru2 173.1(15) . . ? C12 Os1 Ru2 91.6(9) . . ? C12 Os1 Ru2 91.6(9) 4_565 . ? C11 Os1 Os2 112.9(12) . 4_565 ? C12 Os1 Os2 150.4(9) . 4_565 ? C12 Os1 Os2 97.4(9) 4_565 4_565 ? Ru2 Os1 Os2 61.35(5) . 4_565 ? C11 Os1 Os2 112.9(12) . . ? C12 Os1 Os2 97.4(9) . . ? C12 Os1 Os2 150.4(9) 4_565 . ? Ru2 Os1 Os2 61.35(5) . . ? Os2 Os1 Os2 60.25(5) 4_565 . ? C22 Os2 C21 91.2(13) . . ? C22 Os2 C23 92.0(11) . . ? C21 Os2 C23 98.0(11) . . ? C22 Os2 C1 169.2(11) . . ? C21 Os2 C1 96.4(9) . . ? C23 Os2 C1 79.3(10) . . ? C22 Os2 Os1 71.9(10) . . ? C21 Os2 Os1 152.9(8) . . ? C23 Os2 Os1 103.5(7) . . ? C1 Os2 Os1 103.6(5) . . ? C22 Os2 Os2 92.7(8) . 4_565 ? C21 Os2 Os2 101.3(8) . 4_565 ? C23 Os2 Os2 160.0(9) . 4_565 ? C1 Os2 Os2 93.3(6) . 4_565 ? Os1 Os2 Os2 59.88(2) . 4_565 ? C22 Os2 Ru1 144.9(9) . . ? C21 Os2 Ru1 74.7(8) . . ? C23 Os2 Ru1 121.3(7) . . ? C1 Os2 Ru1 45.4(5) . . ? Os1 Os2 Ru1 106.89(5) . . ? Os2 Os2 Ru1 60.08(3) 4_565 . ? C22 Os2 Ru2 130.8(10) . . ? C21 Os2 Ru2 131.6(8) . . ? C23 Os2 Ru2 102.3(9) . . ? C1 Os2 Ru2 46.6(5) . . ? Os1 Os2 Ru2 59.06(6) . . ? Os2 Os2 Ru2 60.45(3) 4_565 . ? Ru1 Os2 Ru2 57.21(7) . . ? C1 Ru1 C1 97.7(12) . 4_565 ? C1 Ru1 C3 147.1(11) . 4_565 ? C1 Ru1 C3 94.3(10) 4_565 4_565 ? C1 Ru1 C3 94.3(10) . . ? C1 Ru1 C3 147.1(11) 4_565 . ? C3 Ru1 C3 61.0(17) 4_565 . ? C1 Ru1 C4 129.0(6) . . ? C1 Ru1 C4 129.0(6) 4_565 . ? C3 Ru1 C4 35.7(9) 4_565 . ? C3 Ru1 C4 35.7(9) . . ? C1 Ru1 C2 112.5(11) . 4_565 ? C1 Ru1 C2 86.6(9) 4_565 4_565 ? C3 Ru1 C2 37.8(11) 4_565 4_565 ? C3 Ru1 C2 60.5(11) . 4_565 ? C4 Ru1 C2 59.9(13) . 4_565 ? C1 Ru1 C2 86.6(9) . . ? C1 Ru1 C2 112.5(11) 4_565 . ? C3 Ru1 C2 60.5(11) 4_565 . ? C3 Ru1 C2 37.8(11) . . ? C4 Ru1 C2 59.9(13) . . ? C2 Ru1 C2 34.2(15) 4_565 . ? C1 Ru1 Ru2 50.5(6) . . ? C1 Ru1 Ru2 50.5(6) 4_565 . ? C3 Ru1 Ru2 143.3(8) 4_565 . ? C3 Ru1 Ru2 143.3(8) . . ? C4 Ru1 Ru2 177.9(11) . . ? C2 Ru1 Ru2 118.1(7) 4_565 . ? C2 Ru1 Ru2 118.1(7) . . ? C1 Ru1 Os2 56.4(7) . . ? C1 Ru1 Os2 101.4(6) 4_565 . ? C3 Ru1 Os2 149.3(8) 4_565 . ? C3 Ru1 Os2 110.7(9) . . ? C4 Ru1 Os2 119.7(9) . . ? C2 Ru1 Os2 166.8(8) 4_565 . ? C2 Ru1 Os2 132.9(7) . . ? Ru2 Ru1 Os2 61.98(7) . . ? C1 Ru1 Os2 101.4(6) . 4_565 ? C1 Ru1 Os2 56.4(7) 4_565 4_565 ? C3 Ru1 Os2 110.7(9) 4_565 4_565 ? C3 Ru1 Os2 149.3(8) . 4_565 ? C4 Ru1 Os2 119.7(9) . 4_565 ? C2 Ru1 Os2 132.9(7) 4_565 4_565 ? C2 Ru1 Os2 166.8(8) . 4_565 ? Ru2 Ru1 Os2 61.98(7) . 4_565 ? Os2 Ru1 Os2 59.83(6) . 4_565 ? C1 Ru2 C1 93.6(12) 4_565 . ? C1 Ru2 C6 140.9(10) 4_565 . ? C1 Ru2 C6 92.4(10) . . ? C1 Ru2 C6 92.4(10) 4_565 4_565 ? C1 Ru2 C6 140.9(10) . 4_565 ? C6 Ru2 C6 60.5(14) . 4_565 ? C1 Ru2 C5 128.1(7) 4_565 . ? C1 Ru2 C5 128.1(7) . . ? C6 Ru2 C5 36.1(8) . . ? C6 Ru2 C5 36.1(8) 4_565 . ? C1 Ru2 C7 107.6(9) 4_565 . ? C1 Ru2 C7 80.0(9) . . ? C6 Ru2 C7 36.1(10) . . ? C6 Ru2 C7 61.3(10) 4_565 . ? C5 Ru2 C7 60.6(10) . . ? C1 Ru2 C7 80.0(9) 4_565 4_565 ? C1 Ru2 C7 107.6(9) . 4_565 ? C6 Ru2 C7 61.3(10) . 4_565 ? C6 Ru2 C7 36.1(10) 4_565 4_565 ? C5 Ru2 C7 60.6(10) . 4_565 ? C7 Ru2 C7 38.0(12) . 4_565 ? C1 Ru2 Ru1 48.3(6) 4_565 . ? C1 Ru2 Ru1 48.3(6) . . ? C6 Ru2 Ru1 136.7(8) . . ? C6 Ru2 Ru1 136.7(8) 4_565 . ? C5 Ru2 Ru1 168.1(9) . . ? C7 Ru2 Ru1 108.3(5) . . ? C7 Ru2 Ru1 108.3(5) 4_565 . ? C1 Ru2 Os1 112.5(7) 4_565 . ? C1 Ru2 Os1 112.5(7) . . ? C6 Ru2 Os1 100.6(8) . . ? C6 Ru2 Os1 100.6(8) 4_565 . ? C5 Ru2 Os1 81.6(9) . . ? C7 Ru2 Os1 136.7(6) . . ? C7 Ru2 Os1 136.7(6) 4_565 . ? Ru1 Ru2 Os1 110.32(11) . . ? C1 Ru2 Os2 55.4(7) 4_565 4_565 ? C1 Ru2 Os2 98.7(7) . 4_565 ? C6 Ru2 Os2 159.9(8) . 4_565 ? C6 Ru2 Os2 116.2(7) 4_565 4_565 ? C5 Ru2 Os2 128.7(7) . 4_565 ? C7 Ru2 Os2 162.9(6) . 4_565 ? C7 Ru2 Os2 129.4(6) 4_565 4_565 ? Ru1 Ru2 Os2 60.81(7) . 4_565 ? Os1 Ru2 Os2 59.59(6) . 4_565 ? C1 Ru2 Os2 98.7(7) 4_565 . ? C1 Ru2 Os2 55.4(7) . . ? C6 Ru2 Os2 116.2(7) . . ? C6 Ru2 Os2 159.9(8) 4_565 . ? C5 Ru2 Os2 128.7(7) . . ? C7 Ru2 Os2 129.4(6) . . ? C7 Ru2 Os2 162.9(6) 4_565 . ? Ru1 Ru2 Os2 60.81(7) . . ? Os1 Ru2 Os2 59.59(6) . . ? Os2 Ru2 Os2 59.10(7) 4_565 . ? O11 C11 Os1 178.4(40) . . ? O12 C12 Os1 177.0(26) . . ? O21 C21 Os2 171.0(24) . . ? O22 C22 Os2 169.0(28) . . ? O23 C23 Os2 175.5(28) . . ? O1 C1 Ru1 138.6(16) . . ? O1 C1 Ru2 132.3(17) . . ? Ru1 C1 Ru2 81.2(8) . . ? O1 C1 Os2 125.8(18) . . ? Ru1 C1 Os2 78.2(8) . . ? Ru2 C1 Os2 77.9(7) . . ? C2 C2 C3 108.7(17) 4_565 . ? C2 C2 Ru1 72.9(7) 4_565 . ? C3 C2 Ru1 69.9(15) . . ? C4 C3 C2 105.4(29) . . ? C4 C3 Ru1 72.4(17) . . ? C2 C3 Ru1 72.3(13) . . ? C3 C4 C3 111.6(40) . 4_565 ? C3 C4 Ru1 71.9(17) . . ? C3 C4 Ru1 71.9(17) 4_565 . ? C6 C5 C6 108.3(34) 4_565 . ? C6 C5 Ru2 71.6(15) 4_565 . ? C6 C5 Ru2 71.6(15) . . ? C5 C6 C7 109.9(24) . . ? C5 C6 Ru2 72.3(16) . . ? C7 C6 Ru2 73.7(13) . . ? C6 C7 C7 105.9(15) . 4_565 ? C6 C7 Ru2 70.2(13) . . ? C7 C7 Ru2 71.0(6) 4_565 . ? _refine_diff_density_max 4.143 _refine_diff_density_min -2.751 _refine_diff_density_rms 0.440