Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 #==================================================================== # 1. SUBMISSION DETAILS loop_ _publ_author_name 'Lum, Mien Wei' 'Leong, Weng Kee' _publ_contact_author ; Weng Kee Leong Department of Chemistry National University of Singapore Kent Ridge Singapore 119260 ; _publ_contact_author_phone (65)-874-5131 _publ_contact_author_fax (65)-779-1691 _publ_contact_author_email chmlwk@nus.edu.sg _publ_requested_journal J. Chem. Soc., Dalton Trans. _publ_requested_coeditor_name ? #==================================================================== # CRYSTAL DATA FOR COMPOUND 2b #==================================================================== data_mw7 _database_code_CSD 163860 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C13 H8 O12 Os3' _chemical_formula_weight 926.79 _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' '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 P21/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 7.5248(2) _cell_length_b 16.6875(4) _cell_length_c 16.1098(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.1110(10) _cell_angle_gamma 90.00 _cell_volume 2014.87(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7862 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.055 _exptl_crystal_density_method ? _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 18.928 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.044451 _exptl_absorpt_correction_T_max 0.106451 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13123 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 29.23 _reflns_number_total 4946 _reflns_number_observed 3789 _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^)+(0.0686P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4945 _refine_ls_number_parameters 250 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_obs 0.0466 _refine_ls_wR_factor_all 0.1241 _refine_ls_wR_factor_obs 0.1149 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 1.131 _refine_ls_restrained_S_all 1.063 _refine_ls_restrained_S_obs 1.131 _refine_ls_shift/esd_max -0.001 _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 0.24342(5) 0.69222(2) 0.71495(2) 0.03135(12) Uani 1 d D . Os2 Os 0.25416(5) 0.59175(2) 0.85475(2) 0.03128(12) Uani 1 d D . Os3 Os -0.03796(6) 0.69725(2) 0.82052(3) 0.03504(13) Uani 1 d . . O1 O 0.1992(9) 0.5666(4) 0.7264(4) 0.0327(15) Uani 1 d . . O11 O 0.5551(14) 0.6811(6) 0.6076(6) 0.068(3) Uani 1 d . . O12 O -0.0297(13) 0.7210(7) 0.5683(6) 0.075(3) Uani 1 d . . O13 O 0.3088(16) 0.8700(5) 0.7389(7) 0.078(3) Uani 1 d . . O21 O 0.6037(13) 0.4959(6) 0.8885(6) 0.076(3) Uani 1 d . . O22 O 0.0143(12) 0.4579(6) 0.9121(7) 0.075(3) Uani 1 d . . O23 O 0.3150(13) 0.6618(6) 1.0279(5) 0.062(2) Uani 1 d . . O31 O -0.1979(11) 0.5557(5) 0.7169(6) 0.059(2) Uani 1 d . . O32 O -0.2569(15) 0.8222(6) 0.7173(7) 0.086(4) Uani 1 d . . O33 O 0.1964(13) 0.8232(5) 0.9205(6) 0.066(3) Uani 1 d . . O34 O -0.2698(14) 0.6631(8) 0.9632(7) 0.086(3) Uani 1 d . . C1 C 0.2998(16) 0.5066(7) 0.6870(7) 0.044(3) Uani 1 d . . H1A H 0.3005(16) 0.4574(7) 0.7190(7) 0.052 Uiso 1 calc R 1 H1B H 0.4223(16) 0.5245(7) 0.6859(7) 0.052 Uiso 1 calc R 1 C3 C 0.3194(26) 0.4269(10) 0.5547(11) 0.096(6) Uani 1 d . . H3A H 0.2630(26) 0.4195(10) 0.4994(11) 0.145 Uiso 1 calc R 1 H3B H 0.3167(26) 0.3774(10) 0.5849(11) 0.145 Uiso 1 calc R 1 H3C H 0.4409(26) 0.4432(10) 0.5517(11) 0.145 Uiso 1 calc R 1 C11 C 0.4395(15) 0.6824(6) 0.6485(7) 0.037(2) Uani 1 d . . C12 C 0.0710(16) 0.7111(7) 0.6226(7) 0.044(3) Uani 1 d . . C13 C 0.2828(18) 0.8042(7) 0.7280(8) 0.050(3) Uani 1 d . . C21 C 0.4747(16) 0.5297(7) 0.8710(7) 0.045(3) Uani 1 d . . C22 C 0.0998(16) 0.5102(7) 0.8929(7) 0.046(3) Uani 1 d . . C23 C 0.2916(15) 0.6361(6) 0.9628(6) 0.041(2) Uani 1 d . . C31 C -0.1379(14) 0.6074(7) 0.7557(7) 0.041(2) Uani 1 d . . C32 C -0.1788(16) 0.7772(8) 0.7582(8) 0.053(3) Uani 1 d . . C33 C 0.1112(16) 0.7773(7) 0.8848(7) 0.045(3) Uani 1 d . . C34 C -0.1848(15) 0.6751(8) 0.9098(9) 0.051(3) Uani 1 d . . H12 H 0.3830(159) 0.6600(57) 0.8028(45) 0.056(34) Uiso 1 d D . C2A C 0.2203(19) 0.4909(9) 0.5992(9) 0.068(4) Uiso 0.50 d PD 1 H2A H 0.2376(19) 0.5407(9) 0.5686(9) 0.081 Uiso 0.50 calc PR 1 O2A O 0.0394(26) 0.4785(13) 0.5927(14) 0.082(4) Uiso 0.50 d PD 1 H2AA H 0.0040(26) 0.4703(13) 0.5438(14) 0.123 Uiso 0.50 calc PR 1 C2B C 0.2203(19) 0.4909(9) 0.5992(9) 0.068(4) Uiso 0.50 d PD 2 H2B H 0.0999(28) 0.4700(13) 0.6039(13) 0.081 Uiso 0.50 calc PR 2 O2B O 0.1999(28) 0.5597(13) 0.5528(13) 0.082(4) Uiso 0.50 d PD 2 H2BA H 0.1315(28) 0.5513(13) 0.5112(13) 0.123 Uiso 0.50 calc PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0382(2) 0.0268(2) 0.0287(2) 0.00240(15) 0.0016(2) 0.00008(15) Os2 0.0377(2) 0.0288(2) 0.0268(2) 0.00158(15) -0.00005(15) 0.0018(2) Os3 0.0347(2) 0.0339(2) 0.0361(2) -0.0044(2) 0.0012(2) 0.0025(2) O1 0.044(4) 0.023(3) 0.031(3) -0.003(3) 0.000(3) 0.001(3) O11 0.065(6) 0.075(7) 0.067(6) -0.009(5) 0.024(5) -0.012(5) O12 0.066(6) 0.105(8) 0.051(6) 0.024(6) -0.018(5) 0.006(6) O13 0.127(9) 0.030(5) 0.080(7) -0.002(5) 0.028(6) -0.009(5) O21 0.059(6) 0.080(7) 0.085(7) -0.003(6) -0.007(5) 0.036(5) O22 0.061(6) 0.077(7) 0.088(7) 0.026(6) 0.014(5) -0.022(5) O23 0.083(6) 0.066(6) 0.037(5) -0.007(4) 0.005(4) 0.011(5) O31 0.042(5) 0.060(6) 0.074(6) -0.015(5) -0.001(4) -0.016(4) O32 0.101(9) 0.054(6) 0.097(8) -0.004(6) -0.031(7) 0.031(6) O33 0.075(6) 0.054(5) 0.064(6) -0.027(5) -0.010(5) -0.013(5) O34 0.065(7) 0.124(10) 0.072(7) -0.019(7) 0.028(6) -0.033(7) C1 0.058(7) 0.033(6) 0.040(6) -0.005(5) 0.006(5) 0.010(5) C3 0.132(16) 0.083(12) 0.076(11) -0.051(10) 0.019(10) 0.020(11) C11 0.045(6) 0.035(6) 0.031(5) -0.006(4) 0.005(4) -0.003(4) C12 0.048(7) 0.044(6) 0.039(6) 0.010(5) 0.004(5) 0.005(5) C13 0.060(8) 0.042(7) 0.049(7) -0.002(5) 0.011(6) -0.006(5) C21 0.059(7) 0.042(6) 0.035(6) 0.005(5) 0.003(5) 0.006(5) C22 0.049(7) 0.046(7) 0.042(6) 0.001(5) 0.003(5) 0.013(6) C23 0.057(7) 0.035(6) 0.030(5) 0.000(4) 0.001(5) 0.005(5) C31 0.033(5) 0.049(7) 0.038(6) 0.007(5) -0.003(4) 0.004(5) C32 0.045(7) 0.052(7) 0.059(8) -0.007(6) -0.006(6) 0.015(6) C33 0.048(7) 0.043(6) 0.046(6) -0.006(5) 0.010(5) 0.005(5) C34 0.029(6) 0.063(8) 0.060(8) -0.010(6) 0.005(5) -0.011(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 C13 1.901(12) . ? Os1 C11 1.905(12) . ? Os1 C12 1.911(11) . ? Os1 O1 2.133(6) . ? Os1 Os2 2.8029(5) . ? Os1 Os3 2.8327(6) . ? Os2 C23 1.890(11) . ? Os2 C22 1.926(13) . ? Os2 C21 1.954(12) . ? Os2 O1 2.114(6) . ? Os2 Os3 2.8318(6) . ? Os3 C34 1.926(13) . ? Os3 C32 1.929(12) . ? Os3 C31 1.940(12) . ? Os3 C33 1.977(12) . ? O1 C1 1.436(12) . ? O11 C11 1.138(13) . ? O12 C12 1.118(13) . ? O13 C13 1.126(13) . ? O21 C21 1.137(13) . ? O22 C22 1.142(14) . ? O23 C23 1.133(13) . ? O31 C31 1.136(13) . ? O32 C32 1.129(14) . ? O33 C33 1.124(13) . ? O34 C34 1.135(15) . ? C1 C2B 1.51(2) . ? C1 C2A 1.51(2) . ? C3 C2B 1.52(2) . ? C3 C2A 1.52(2) . ? C2A O2A 1.37(2) . ? C2B O2B 1.37(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 C13 Os1 C11 91.5(5) . . ? C13 Os1 C12 90.7(5) . . ? C11 Os1 C12 94.7(5) . . ? C13 Os1 O1 168.7(4) . . ? C11 Os1 O1 95.7(4) . . ? C12 Os1 O1 97.4(4) . . ? C13 Os1 Os2 120.4(4) . . ? C11 Os1 Os2 115.6(3) . . ? C12 Os1 Os2 133.9(4) . . ? O1 Os1 Os2 48.4(2) . . ? C13 Os1 Os3 91.3(4) . . ? C11 Os1 Os3 175.9(3) . . ? C12 Os1 Os3 88.3(4) . . ? O1 Os1 Os3 81.2(2) . . ? Os2 Os1 Os3 60.326(14) . . ? C23 Os2 C22 91.6(5) . . ? C23 Os2 C21 91.7(5) . . ? C22 Os2 C21 96.4(5) . . ? C23 Os2 O1 168.2(4) . . ? C22 Os2 O1 95.8(4) . . ? C21 Os2 O1 96.6(4) . . ? C23 Os2 Os1 119.8(3) . . ? C22 Os2 Os1 134.8(3) . . ? C21 Os2 Os1 112.8(3) . . ? O1 Os2 Os1 49.0(2) . . ? C23 Os2 Os3 89.2(3) . . ? C22 Os2 Os3 91.3(3) . . ? C21 Os2 Os3 172.3(4) . . ? O1 Os2 Os3 81.5(2) . . ? Os1 Os2 Os3 60.358(14) . . ? C34 Os3 C32 101.3(6) . . ? C34 Os3 C31 91.9(5) . . ? C32 Os3 C31 94.9(5) . . ? C34 Os3 C33 94.3(5) . . ? C32 Os3 C33 93.7(5) . . ? C31 Os3 C33 168.2(5) . . ? C34 Os3 Os2 102.8(4) . . ? C32 Os3 Os2 155.8(4) . . ? C31 Os3 Os2 83.2(3) . . ? C33 Os3 Os2 85.6(3) . . ? C34 Os3 Os1 162.1(4) . . ? C32 Os3 Os1 96.5(4) . . ? C31 Os3 Os1 85.9(3) . . ? C33 Os3 Os1 85.1(3) . . ? Os2 Os3 Os1 59.316(14) . . ? C1 O1 Os2 120.4(6) . . ? C1 O1 Os1 123.6(7) . . ? Os2 O1 Os1 82.6(2) . . ? O1 C1 C2B 110.8(10) . . ? O1 C1 C2A 110.8(10) . . ? O11 C11 Os1 176.1(10) . . ? O12 C12 Os1 179.0(12) . . ? O13 C13 Os1 177.2(12) . . ? O21 C21 Os2 173.2(10) . . ? O22 C22 Os2 175.1(11) . . ? O23 C23 Os2 179.2(10) . . ? O31 C31 Os3 178.9(10) . . ? O32 C32 Os3 175.5(12) . . ? O33 C33 Os3 179.2(11) . . ? O34 C34 Os3 178.7(11) . . ? O2A C2A C1 113.9(15) . . ? O2A C2A C3 112.5(15) . . ? C1 C2A C3 113.2(12) . . ? O2B C2B C1 112.4(15) . . ? O2B C2B C3 111.6(16) . . ? C1 C2B C3 113.2(12) . . ? _refine_diff_density_max 1.816 _refine_diff_density_min -4.272 _refine_diff_density_rms 0.364 #==================================================================== # CRYSTAL DATA FOR COMPOUND 2c #========================================================================= data_mw9 _database_code_CSD 163861 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H8 O12 Os3' _chemical_formula_weight 926.79 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' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.96630(10) _cell_length_b 13.941 _cell_length_c 16.6032(2) _cell_angle_alpha 105.2250(10) _cell_angle_beta 90.3450(10) _cell_angle_gamma 98.6290(10) _cell_volume 1977.65(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.113 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 19.284 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.010223 _exptl_absorpt_correction_T_max 0.060868 _exptl_absorpt_process_details ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15111 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 29.30 _reflns_number_total 9413 _reflns_number_gt 7483 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+8.7761P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9413 _refine_ls_number_parameters 511 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.1009 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.119 _refine_ls_shift/su_mean 0.010 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os -0.17124(4) 0.17627(3) 0.09689(2) 0.03497(10) Uani 1 1 d D . . Os2 Os 0.12427(5) 0.19197(3) 0.15966(3) 0.03546(10) Uani 1 1 d D . . Os3 Os 0.06098(5) 0.31045(3) 0.05251(3) 0.03650(10) Uani 1 1 d D . . Os4 Os 0.60243(5) 0.16148(3) 0.63761(3) 0.03738(10) Uani 1 1 d D . . Os5 Os 0.37959(5) 0.25979(3) 0.59301(3) 0.03973(11) Uani 1 1 d D . . Os6 Os 0.41278(5) 0.25302(3) 0.76069(3) 0.04003(11) Uani 1 1 d D . . O1 O -0.0678(8) 0.2466(5) 0.2178(4) 0.0365(15) Uani 1 1 d . . . O2 O -0.0088(14) 0.3824(8) 0.3913(7) 0.094(4) Uani 1 1 d . . . H2B H 0.0515 0.4069 0.4313 0.140 Uiso 1 1 calc R . . O3 O 0.6152(7) 0.3061(5) 0.6165(4) 0.0360(15) Uani 1 1 d . . . O4 O 0.7784(16) 0.4882(9) 0.5049(9) 0.110(4) Uani 1 1 d . . . H4D H 0.8642 0.4987 0.5260 0.164 Uiso 1 1 calc R . . O11 O -0.3924(11) 0.0131(7) 0.1432(6) 0.072(3) Uani 1 1 d . . . O12 O -0.3857(10) 0.3278(7) 0.1083(6) 0.071(3) Uani 1 1 d . . . O13 O -0.2499(11) 0.0827(7) -0.0876(5) 0.062(2) Uani 1 1 d . . . O21 O 0.1549(12) 0.0416(8) 0.2633(6) 0.073(3) Uani 1 1 d . . . O22 O 0.3662(11) 0.3605(7) 0.2580(6) 0.069(3) Uani 1 1 d . . . O23 O 0.3637(11) 0.1139(7) 0.0444(6) 0.068(3) Uani 1 1 d . . . O31 O -0.0101(11) 0.4614(6) 0.2163(6) 0.066(2) Uani 1 1 d . . . O32 O -0.1315(12) 0.3949(8) -0.0539(6) 0.074(3) Uani 1 1 d . . . O33 O 0.1097(11) 0.1321(7) -0.0927(6) 0.070(3) Uani 1 1 d . . . O34 O 0.3714(11) 0.4288(8) 0.0342(7) 0.076(3) Uani 1 1 d . . . O41 O 0.7664(11) 0.0644(8) 0.4820(6) 0.081(3) Uani 1 1 d . . . O42 O 0.8625(12) 0.2081(8) 0.7682(7) 0.077(3) Uani 1 1 d . . . O43 O 0.5052(12) -0.0421(6) 0.6680(7) 0.081(3) Uani 1 1 d . . . O51 O 0.3654(13) 0.2523(9) 0.4068(6) 0.085(3) Uani 1 1 d . . . O52 O 0.2894(15) 0.4671(8) 0.6638(7) 0.096(4) Uani 1 1 d . . . O53 O 0.0600(11) 0.1513(9) 0.5809(9) 0.097(4) Uani 1 1 d . . . O61 O 0.6566(12) 0.4407(7) 0.7849(6) 0.076(3) Uani 1 1 d . . . O62 O 0.5296(12) 0.2221(8) 0.9246(6) 0.076(3) Uani 1 1 d . . . O63 O 0.1953(12) 0.0504(8) 0.7139(7) 0.074(3) Uani 1 1 d . . . O64 O 0.1691(13) 0.3776(9) 0.8348(7) 0.088(3) Uani 1 1 d . . . C1 C -0.2829(14) 0.2611(11) 0.3063(8) 0.061(3) Uani 1 1 d . . . H1A H -0.3497 0.2291 0.2582 0.092 Uiso 1 1 calc R . . H1B H -0.2688 0.3327 0.3147 0.092 Uiso 1 1 calc R . . H1C H -0.3258 0.2445 0.3547 0.092 Uiso 1 1 calc R . . C2 C -0.1313(13) 0.2245(9) 0.2925(7) 0.045(2) Uani 1 1 d . . . H2A H -0.1474 0.1514 0.2842 0.054 Uiso 1 1 calc R . . C3 C -0.0187(15) 0.2733(11) 0.3677(8) 0.061(3) Uani 1 1 d . . . H3A H -0.0510 0.2475 0.4147 0.073 Uiso 1 1 calc R . . H3B H 0.0802 0.2556 0.3535 0.073 Uiso 1 1 calc R . . C4 C 0.8800(15) 0.3610(11) 0.6006(10) 0.069(4) Uani 1 1 d . . . H4A H 0.9052 0.2979 0.6047 0.103 Uiso 1 1 calc R . . H4B H 0.8858 0.4070 0.6553 0.103 Uiso 1 1 calc R . . H4C H 0.9497 0.3886 0.5658 0.103 Uiso 1 1 calc R . . C5 C 0.7172(12) 0.3442(8) 0.5618(6) 0.040(2) Uani 1 1 d . . . H5A H 0.7094 0.2960 0.5065 0.048 Uiso 1 1 calc R . . C6 C 0.6762(16) 0.4432(10) 0.5550(9) 0.062(3) Uani 1 1 d . . . H6A H 0.5745 0.4320 0.5305 0.075 Uiso 1 1 calc R . . H6B H 0.6780 0.4888 0.6104 0.075 Uiso 1 1 calc R . . C11 C -0.3102(13) 0.0735(8) 0.1286(7) 0.044(2) Uani 1 1 d . . . C12 C -0.3105(14) 0.2705(8) 0.1023(7) 0.044(2) Uani 1 1 d . . . C13 C -0.2220(12) 0.1173(7) -0.0180(7) 0.044(2) Uani 1 1 d . . . C21 C 0.1397(12) 0.0984(8) 0.2266(7) 0.044(2) Uani 1 1 d . . . C22 C 0.2740(13) 0.2979(8) 0.2212(7) 0.041(2) Uani 1 1 d . . . C23 C 0.2740(13) 0.1436(8) 0.0882(7) 0.045(3) Uani 1 1 d . . . C31 C 0.0160(14) 0.4057(8) 0.1565(7) 0.046(3) Uani 1 1 d . . . C32 C -0.0583(13) 0.3631(8) -0.0161(7) 0.044(2) Uani 1 1 d . . . C33 C 0.0924(14) 0.1962(8) -0.0396(7) 0.048(3) Uani 1 1 d . . . C34 C 0.2559(15) 0.3851(9) 0.0436(8) 0.053(3) Uani 1 1 d . . . C41 C 0.7052(12) 0.1042(9) 0.5412(8) 0.052(3) Uani 1 1 d . . . C42 C 0.7687(12) 0.1897(9) 0.7192(8) 0.046(3) Uani 1 1 d . . . C43 C 0.5402(15) 0.0345(9) 0.6575(8) 0.055(3) Uani 1 1 d . . . C51 C 0.3745(13) 0.2560(10) 0.4751(8) 0.056(3) Uani 1 1 d . . . C52 C 0.3226(16) 0.3905(11) 0.6359(9) 0.063(4) Uani 1 1 d . . . C53 C 0.1804(15) 0.1918(10) 0.5843(9) 0.055(3) Uani 1 1 d . . . C61 C 0.5697(15) 0.3733(9) 0.7732(7) 0.050(3) Uani 1 1 d . . . C62 C 0.4844(14) 0.2298(8) 0.8619(8) 0.049(3) Uani 1 1 d . . . C63 C 0.2733(13) 0.1233(9) 0.7294(8) 0.051(3) Uani 1 1 d . . . C64 C 0.2561(15) 0.3302(10) 0.8062(9) 0.059(3) Uani 1 1 d . . . H12 H -0.0105(12) 0.1064(6) 0.0791(10) 0.040 Uiso 1 1 d D . . H45 H 0.4138(15) 0.1308(8) 0.5847(7) 0.040 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0366(2) 0.03365(19) 0.0337(2) 0.00837(15) -0.00009(16) 0.00352(15) Os2 0.0371(2) 0.03473(19) 0.0361(2) 0.01161(16) 0.00108(17) 0.00673(15) Os3 0.0433(2) 0.03259(19) 0.0351(2) 0.01184(16) 0.00434(17) 0.00557(16) Os4 0.0346(2) 0.0373(2) 0.0394(2) 0.00833(16) -0.00137(17) 0.00661(15) Os5 0.0366(2) 0.0479(2) 0.0367(2) 0.01241(18) -0.00083(17) 0.01098(17) Os6 0.0432(2) 0.0428(2) 0.0358(2) 0.01301(17) 0.00520(18) 0.00730(17) O1 0.044(4) 0.038(3) 0.027(3) 0.009(3) 0.006(3) 0.005(3) O2 0.108(9) 0.074(7) 0.078(8) 0.004(6) -0.016(7) -0.021(6) O3 0.035(4) 0.040(4) 0.033(4) 0.012(3) -0.002(3) 0.004(3) O4 0.127(11) 0.096(9) 0.103(10) 0.042(8) -0.013(9) -0.018(8) O11 0.071(6) 0.070(6) 0.071(7) 0.026(5) 0.009(5) -0.013(5) O12 0.062(6) 0.081(6) 0.073(7) 0.011(5) -0.003(5) 0.038(5) O13 0.077(6) 0.063(5) 0.040(5) 0.002(4) -0.012(4) 0.012(5) O21 0.093(7) 0.081(6) 0.063(6) 0.042(5) 0.004(5) 0.032(6) O22 0.069(6) 0.054(5) 0.073(7) 0.010(5) -0.009(5) -0.007(5) O23 0.068(6) 0.065(5) 0.075(7) 0.019(5) 0.021(5) 0.021(5) O31 0.083(7) 0.047(5) 0.061(6) 0.001(4) 0.006(5) 0.016(4) O32 0.085(7) 0.081(7) 0.070(7) 0.039(6) -0.003(6) 0.025(6) O33 0.080(7) 0.069(6) 0.059(6) 0.008(5) 0.022(5) 0.018(5) O34 0.055(6) 0.085(7) 0.084(8) 0.028(6) 0.014(5) -0.010(5) O41 0.067(6) 0.092(7) 0.064(6) -0.018(5) 0.013(5) 0.019(5) O42 0.069(7) 0.090(7) 0.070(7) 0.018(6) -0.028(5) 0.013(5) O43 0.097(8) 0.043(5) 0.112(9) 0.039(5) 0.008(7) 0.007(5) O51 0.094(8) 0.123(9) 0.046(6) 0.031(6) 0.000(6) 0.027(7) O52 0.148(11) 0.077(7) 0.076(7) 0.010(6) 0.004(7) 0.073(8) O53 0.039(6) 0.100(8) 0.146(12) 0.031(8) -0.014(6) -0.007(5) O61 0.091(7) 0.062(6) 0.055(6) 0.001(5) 0.011(5) -0.026(5) O62 0.088(7) 0.084(7) 0.062(6) 0.031(5) -0.018(6) 0.017(6) O63 0.070(6) 0.073(6) 0.074(7) 0.023(5) 0.005(5) -0.012(5) O64 0.090(8) 0.105(8) 0.088(8) 0.039(7) 0.036(7) 0.055(7) C1 0.056(8) 0.077(9) 0.041(7) 0.000(6) 0.011(6) 0.006(6) C2 0.050(7) 0.055(6) 0.029(5) 0.012(5) 0.004(5) 0.003(5) C3 0.055(8) 0.089(10) 0.037(6) 0.015(6) 0.016(6) 0.007(7) C4 0.061(8) 0.066(8) 0.074(10) 0.018(7) -0.022(7) -0.001(6) C5 0.041(6) 0.044(5) 0.029(5) 0.008(4) 0.009(4) -0.004(4) C6 0.067(9) 0.060(7) 0.068(9) 0.035(7) 0.001(7) -0.002(6) C11 0.045(6) 0.037(5) 0.046(6) 0.008(5) 0.006(5) -0.001(5) C12 0.055(7) 0.047(6) 0.033(5) 0.014(5) -0.002(5) 0.007(5) C13 0.045(6) 0.034(5) 0.047(7) 0.001(5) -0.001(5) 0.007(4) C21 0.042(6) 0.046(6) 0.048(6) 0.017(5) 0.008(5) 0.012(5) C22 0.047(6) 0.039(5) 0.036(6) 0.009(4) 0.003(5) 0.006(5) C23 0.053(7) 0.043(5) 0.040(6) 0.010(5) 0.004(5) 0.015(5) C31 0.059(7) 0.038(5) 0.040(6) 0.008(5) 0.009(5) 0.005(5) C32 0.048(6) 0.046(6) 0.040(6) 0.017(5) 0.001(5) 0.004(5) C33 0.059(7) 0.040(5) 0.043(6) 0.005(5) 0.009(6) 0.014(5) C34 0.063(8) 0.043(6) 0.055(7) 0.013(5) -0.005(6) 0.011(6) C41 0.028(5) 0.053(7) 0.064(8) -0.002(6) -0.009(5) 0.001(5) C42 0.033(6) 0.052(6) 0.057(7) 0.021(5) -0.003(5) 0.011(5) C43 0.066(8) 0.049(6) 0.064(8) 0.033(6) 0.004(7) 0.018(6) C51 0.039(6) 0.074(8) 0.048(7) 0.006(6) -0.011(6) 0.008(6) C52 0.072(9) 0.071(9) 0.063(8) 0.039(7) 0.004(7) 0.024(7) C53 0.049(7) 0.062(7) 0.061(8) 0.027(6) -0.004(6) 0.011(6) C61 0.060(7) 0.050(6) 0.037(6) 0.008(5) 0.008(5) 0.006(6) C62 0.055(7) 0.044(6) 0.048(7) 0.014(5) 0.000(6) 0.007(5) C63 0.043(6) 0.055(7) 0.054(7) 0.018(6) 0.006(6) -0.002(5) C64 0.057(8) 0.074(8) 0.057(8) 0.029(7) 0.020(7) 0.023(7) _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 1.891(12) . ? Os1 C12 1.930(11) . ? Os1 C11 1.936(11) . ? Os1 O1 2.126(7) . ? Os1 Os2 2.7978(6) . ? Os1 Os3 2.8198(6) . ? Os2 C23 1.880(11) . ? Os2 C22 1.904(11) . ? Os2 C21 1.942(11) . ? Os2 O1 2.122(7) . ? Os2 Os3 2.8333(6) . ? Os3 C32 1.908(11) . ? Os3 C34 1.923(14) . ? Os3 C33 1.953(10) . ? Os3 C31 1.967(11) . ? Os4 C43 1.888(11) . ? Os4 C41 1.901(12) . ? Os4 C42 1.932(12) . ? Os4 O3 2.123(7) . ? Os4 Os5 2.7850(5) . ? Os4 Os6 2.8319(6) . ? Os5 C53 1.878(14) . ? Os5 C52 1.921(14) . ? Os5 C51 1.945(14) . ? Os5 O3 2.117(7) . ? Os5 Os6 2.8257(6) . ? Os6 C62 1.918(13) . ? Os6 C64 1.934(12) . ? Os6 C63 1.981(12) . ? Os6 C61 1.985(13) . ? O1 C2 1.454(12) . ? O2 C3 1.456(17) . ? O3 C5 1.435(11) . ? O4 C6 1.426(17) . ? O11 C11 1.112(13) . ? O12 C12 1.106(13) . ? O13 C13 1.139(13) . ? O21 C21 1.139(13) . ? O22 C22 1.147(13) . ? O23 C23 1.139(13) . ? O31 C31 1.139(13) . ? O32 C32 1.117(13) . ? O33 C33 1.109(13) . ? O34 C34 1.153(15) . ? O41 C41 1.178(14) . ? O42 C42 1.120(14) . ? O43 C43 1.126(13) . ? O51 C51 1.123(15) . ? O52 C52 1.133(15) . ? O53 C53 1.134(15) . ? O61 C61 1.100(14) . ? O62 C62 1.151(15) . ? O63 C63 1.111(14) . ? O64 C64 1.126(14) . ? C1 C2 1.519(16) . ? C2 C3 1.541(17) . ? C4 C5 1.552(16) . ? C5 C6 1.512(16) . ? 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 C12 91.3(4) . . ? C13 Os1 C11 92.0(5) . . ? C12 Os1 C11 96.9(5) . . ? C13 Os1 O1 168.1(4) . . ? C12 Os1 O1 95.4(4) . . ? C11 Os1 O1 96.8(4) . . ? C13 Os1 Os2 120.2(3) . . ? C12 Os1 Os2 134.2(3) . . ? C11 Os1 Os2 112.7(3) . . ? O1 Os1 Os2 48.75(18) . . ? C13 Os1 Os3 88.9(3) . . ? C12 Os1 Os3 90.7(3) . . ? C11 Os1 Os3 172.4(3) . . ? O1 Os1 Os3 81.33(18) . . ? Os2 Os1 Os3 60.576(14) . . ? C23 Os2 C22 88.8(5) . . ? C23 Os2 C21 93.1(5) . . ? C22 Os2 C21 97.2(5) . . ? C23 Os2 O1 168.4(4) . . ? C22 Os2 O1 97.8(4) . . ? C21 Os2 O1 95.5(4) . . ? C23 Os2 Os1 120.4(4) . . ? C22 Os2 Os1 135.9(3) . . ? C21 Os2 Os1 111.9(3) . . ? O1 Os2 Os1 48.88(19) . . ? C23 Os2 Os3 89.4(3) . . ? C22 Os2 Os3 90.9(3) . . ? C21 Os2 Os3 171.6(3) . . ? O1 Os2 Os3 81.07(18) . . ? Os1 Os2 Os3 60.097(14) . . ? C32 Os3 C34 99.6(5) . . ? C32 Os3 C33 93.1(5) . . ? C34 Os3 C33 92.9(5) . . ? C32 Os3 C31 93.5(5) . . ? C34 Os3 C31 94.6(5) . . ? C33 Os3 C31 169.0(5) . . ? C32 Os3 Os1 98.2(3) . . ? C34 Os3 Os1 162.2(4) . . ? C33 Os3 Os1 86.0(4) . . ? C31 Os3 Os1 84.4(3) . . ? C32 Os3 Os2 157.5(3) . . ? C34 Os3 Os2 102.9(4) . . ? C33 Os3 Os2 86.3(3) . . ? C31 Os3 Os2 84.2(3) . . ? Os1 Os3 Os2 59.327(14) . . ? C43 Os4 C41 92.1(6) . . ? C43 Os4 C42 90.9(5) . . ? C41 Os4 C42 98.3(5) . . ? C43 Os4 O3 166.0(4) . . ? C41 Os4 O3 96.2(4) . . ? C42 Os4 O3 99.1(4) . . ? C43 Os4 Os5 117.6(4) . . ? C41 Os4 Os5 109.6(4) . . ? C42 Os4 Os5 138.3(3) . . ? O3 Os4 Os5 48.84(18) . . ? C43 Os4 Os6 91.4(4) . . ? C41 Os4 Os6 169.8(4) . . ? C42 Os4 Os6 91.3(3) . . ? O3 Os4 Os6 78.63(18) . . ? Os5 Os4 Os6 60.401(15) . . ? C53 Os5 C52 93.9(6) . . ? C53 Os5 C51 91.8(5) . . ? C52 Os5 C51 98.0(6) . . ? C53 Os5 O3 165.1(4) . . ? C52 Os5 O3 96.6(5) . . ? C51 Os5 O3 97.1(4) . . ? C53 Os5 Os4 116.3(4) . . ? C52 Os5 Os4 134.4(4) . . ? C51 Os5 Os4 113.2(4) . . ? O3 Os5 Os4 49.03(18) . . ? C53 Os5 Os6 91.2(4) . . ? C52 Os5 Os6 87.2(4) . . ? C51 Os5 Os6 173.8(4) . . ? O3 Os5 Os6 78.86(19) . . ? Os4 Os5 Os6 60.622(15) . . ? C62 Os6 C64 98.6(5) . . ? C62 Os6 C63 93.1(5) . . ? C64 Os6 C63 93.8(6) . . ? C62 Os6 C61 91.8(5) . . ? C64 Os6 C61 94.3(5) . . ? C63 Os6 C61 169.8(5) . . ? C62 Os6 Os5 163.3(4) . . ? C64 Os6 Os5 98.1(4) . . ? C63 Os6 Os5 87.4(4) . . ? C61 Os6 Os5 85.3(3) . . ? C62 Os6 Os4 104.3(4) . . ? C64 Os6 Os4 157.0(4) . . ? C63 Os6 Os4 86.8(3) . . ? C61 Os6 Os4 83.3(3) . . ? Os5 Os6 Os4 58.977(14) . . ? C2 O1 Os2 125.1(6) . . ? C2 O1 Os1 121.8(6) . . ? Os2 O1 Os1 82.4(2) . . ? C5 O3 Os5 125.7(6) . . ? C5 O3 Os4 124.8(6) . . ? Os5 O3 Os4 82.1(2) . . ? O1 C2 C1 109.7(9) . . ? O1 C2 C3 109.4(9) . . ? C1 C2 C3 112.0(10) . . ? O2 C3 C2 110.9(11) . . ? O3 C5 C6 108.3(9) . . ? O3 C5 C4 108.2(9) . . ? C6 C5 C4 109.9(10) . . ? O4 C6 C5 111.4(12) . . ? O11 C11 Os1 176.8(11) . . ? O12 C12 Os1 176.6(11) . . ? O13 C13 Os1 178.7(11) . . ? O21 C21 Os2 176.3(10) . . ? O22 C22 Os2 178.7(10) . . ? O23 C23 Os2 179.4(13) . . ? O31 C31 Os3 179.4(11) . . ? O32 C32 Os3 177.4(11) . . ? O33 C33 Os3 178.9(12) . . ? O34 C34 Os3 176.8(12) . . ? O41 C41 Os4 177.0(12) . . ? O42 C42 Os4 177.7(11) . . ? O43 C43 Os4 178.4(13) . . ? O51 C51 Os5 177.2(12) . . ? O52 C52 Os5 177.8(12) . . ? O53 C53 Os5 178.5(14) . . ? O61 C61 Os6 176.0(11) . . ? O62 C62 Os6 175.8(11) . . ? O63 C63 Os6 178.3(12) . . ? O64 C64 Os6 177.3(15) . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 29.30 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 2.227 _refine_diff_density_min -1.967 _refine_diff_density_rms 0.261 #==================================================================== # CRYSTAL DATA FOR COMPOUND 2e #========================================================================= data_mw5 _database_code_CSD 163862 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H10 O12 Os3' _chemical_formula_weight 988.86 _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' '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.5756(4) _cell_length_b 9.8496(2) _cell_length_c 14.1537(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.1980(10) _cell_angle_gamma 90.00 _cell_volume 4537.97(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.895 _exptl_crystal_density_method ? _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 16.819 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.030565 _exptl_absorpt_correction_T_max 0.068504 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23031 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 23.30 _reflns_number_total 3264 _reflns_number_observed 3023 _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^)+(0.0312P)^2^+40.1681P] 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_number_reflns 3264 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_obs 0.0252 _refine_ls_wR_factor_all 0.0686 _refine_ls_wR_factor_obs 0.0665 _refine_ls_goodness_of_fit_all 1.150 _refine_ls_goodness_of_fit_obs 1.163 _refine_ls_restrained_S_all 1.150 _refine_ls_restrained_S_obs 1.163 _refine_ls_shift/esd_max 0.001 _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 0.358527(10) -0.15035(3) -0.08215(2) 0.03595(12) Uani 1 d . . Os2 Os 0.398121(10) -0.38083(3) -0.00926(2) 0.03730(12) Uani 1 d . . Os3 Os 0.445075(10) -0.16328(3) -0.07791(2) 0.03734(12) Uani 1 d . . O1 O 0.36869(15) -0.2172(5) 0.0587(3) 0.0356(12) Uani 1 d . . O2 O 0.3740(2) -0.1866(8) 0.2589(5) 0.076(2) Uani 1 d . . H2A H 0.3940(2) -0.1731(8) 0.2266(5) 0.114 Uiso 1 calc R . O11 O 0.3685(3) 0.1484(7) -0.0326(5) 0.071(2) Uani 1 d . . O12 O 0.2648(2) -0.1479(8) -0.0831(6) 0.079(2) Uani 1 d . . O13 O 0.3553(2) -0.1089(8) -0.2946(5) 0.072(2) Uani 1 d . . O21 O 0.4674(2) -0.4273(9) 0.1373(6) 0.079(2) Uani 1 d . . O22 O 0.3411(3) -0.5993(7) 0.0630(6) 0.086(3) Uani 1 d . . O23 O 0.4345(2) -0.5797(8) -0.1468(5) 0.077(2) Uani 1 d . . O31 O 0.4391(2) -0.0411(8) 0.1213(5) 0.062(2) Uani 1 d . . O32 O 0.4650(2) 0.1127(7) -0.1675(5) 0.067(2) Uani 1 d . . O33 O 0.4346(3) -0.3073(9) -0.2706(5) 0.083(2) Uani 1 d . . O34 O 0.5317(2) -0.2718(8) -0.0359(5) 0.074(2) Uani 1 d . . C1 C 0.3348(2) -0.2386(10) 0.1182(6) 0.037(2) Uani 1 d . . C2 C 0.3484(3) -0.2870(10) 0.2149(6) 0.044(2) Uani 1 d . . C11 C 0.3644(3) 0.0387(10) -0.0543(6) 0.045(2) Uani 1 d . . C12 C 0.2993(3) -0.1556(9) -0.0810(6) 0.050(2) Uani 1 d . . C13 C 0.3570(3) -0.1236(9) -0.2139(7) 0.051(2) Uani 1 d . . C21 C 0.4414(3) -0.4137(10) 0.0830(7) 0.051(2) Uani 1 d . . C22 C 0.3609(3) -0.5170(9) 0.0353(7) 0.049(2) Uani 1 d . . C23 C 0.4218(3) -0.5042(10) -0.0930(7) 0.053(2) Uani 1 d . . C31 C 0.4409(2) -0.0864(9) 0.0490(7) 0.045(2) Uani 1 d . . C32 C 0.4569(3) 0.0090(11) -0.1349(6) 0.048(2) Uani 1 d . . C33 C 0.4383(3) -0.2550(11) -0.1989(7) 0.060(3) Uani 1 d . . C34 C 0.4995(3) -0.2326(10) -0.0526(6) 0.049(2) Uani 1 d . . C111 C 0.3123(3) -0.3093(10) 0.2754(6) 0.045(2) Uani 1 d . . C112 C 0.2880(3) -0.2042(11) 0.3040(7) 0.057(2) Uani 1 d . . H11A H 0.2943(3) -0.1160(11) 0.2862(7) 0.068 Uiso 1 calc R . C113 C 0.2547(3) -0.2269(16) 0.3582(8) 0.081(4) Uani 1 d . . H11B H 0.2391(3) -0.1539(16) 0.3782(8) 0.097 Uiso 1 calc R . C114 C 0.2442(4) -0.3566(17) 0.3832(8) 0.086(4) Uani 1 d . . H11C H 0.2212(4) -0.3720(17) 0.4188(8) 0.103 Uiso 1 calc R . C115 C 0.2682(4) -0.4650(16) 0.3549(9) 0.088(4) Uani 1 d . . H11D H 0.2615(4) -0.5530(16) 0.3726(9) 0.105 Uiso 1 calc R . C116 C 0.3020(3) -0.4424(12) 0.3007(7) 0.066(3) Uani 1 d . . H11E H 0.3178(3) -0.5151(12) 0.2811(7) 0.080 Uiso 1 calc R . H1 H 0.3609(47) -0.3236(161) -0.1065(113) 0.161(63) Uiso 1 d . . H11 H 0.3196(28) -0.3044(101) 0.0980(64) 0.050 Uiso 1 d . . H12 H 0.3223(28) -0.1523(95) 0.1150(62) 0.050 Uiso 1 d . . H21 H 0.3715(27) -0.3797(83) 0.2158(59) 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 0.0313(2) 0.0394(2) 0.0371(2) -0.00007(13) 0.00237(14) -0.00031(13) Os2 0.0337(2) 0.0358(2) 0.0428(2) -0.00037(14) 0.00671(15) 0.00021(14) Os3 0.0317(2) 0.0434(2) 0.0375(2) -0.00142(13) 0.00906(14) -0.00281(14) O1 0.028(3) 0.043(3) 0.036(3) 0.003(2) 0.006(2) 0.002(2) O2 0.062(5) 0.096(6) 0.071(5) -0.009(4) 0.009(4) -0.019(4) O11 0.091(6) 0.045(4) 0.078(5) -0.010(4) -0.001(4) 0.006(4) O12 0.030(4) 0.105(6) 0.101(6) 0.021(5) -0.006(4) -0.005(4) O13 0.083(5) 0.089(6) 0.042(4) 0.003(4) 0.000(4) -0.004(4) O21 0.068(5) 0.093(6) 0.073(5) 0.027(4) -0.020(4) 0.003(4) O22 0.093(6) 0.050(4) 0.120(7) 0.003(4) 0.044(5) -0.022(4) O23 0.088(6) 0.068(5) 0.077(5) -0.016(4) 0.022(4) 0.015(4) O31 0.055(4) 0.088(5) 0.044(4) -0.015(4) 0.004(3) -0.014(4) O32 0.074(5) 0.059(4) 0.067(5) 0.013(4) 0.007(4) -0.010(4) O33 0.109(7) 0.085(6) 0.057(5) -0.030(4) 0.014(4) -0.001(5) O34 0.053(4) 0.088(6) 0.082(5) 0.010(4) 0.012(4) 0.022(4) C1 0.029(4) 0.045(5) 0.037(4) 0.002(4) 0.007(4) 0.003(4) C2 0.034(5) 0.059(6) 0.038(5) 0.000(4) 0.003(4) -0.001(4) C11 0.045(5) 0.047(6) 0.042(5) 0.002(4) 0.004(4) -0.001(4) C12 0.041(6) 0.060(6) 0.048(5) 0.011(4) -0.004(4) 0.000(4) C13 0.057(6) 0.048(5) 0.049(6) -0.004(4) 0.006(5) -0.008(4) C21 0.058(6) 0.048(5) 0.047(5) 0.004(4) 0.012(5) -0.004(5) C22 0.041(5) 0.042(5) 0.064(6) -0.003(4) 0.008(4) 0.003(4) C23 0.052(6) 0.047(5) 0.059(6) 0.000(5) 0.007(5) 0.008(5) C31 0.031(5) 0.054(5) 0.050(6) -0.001(4) 0.001(4) -0.013(4) C32 0.040(5) 0.068(7) 0.036(5) 0.003(4) 0.007(4) 0.001(4) C33 0.062(6) 0.060(6) 0.057(6) -0.003(5) 0.015(5) -0.001(5) C34 0.042(5) 0.063(6) 0.045(5) 0.001(4) 0.014(4) 0.002(5) C111 0.040(5) 0.060(6) 0.036(4) 0.000(4) 0.000(4) -0.011(4) C112 0.050(6) 0.062(6) 0.059(6) -0.010(5) 0.014(5) -0.006(5) C113 0.058(7) 0.121(11) 0.067(7) -0.025(7) 0.025(6) 0.000(7) C114 0.051(7) 0.150(14) 0.059(7) 0.016(7) 0.018(6) -0.026(8) C115 0.062(7) 0.116(11) 0.086(8) 0.033(8) 0.019(7) -0.021(7) C116 0.063(7) 0.072(7) 0.064(6) 0.016(5) 0.009(5) 0.006(6) _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 1.882(10) . ? Os1 C11 1.911(10) . ? Os1 C12 1.932(10) . ? Os1 O1 2.113(5) . ? Os1 Os2 2.7891(5) . ? Os1 Os3 2.8206(4) . ? Os2 C23 1.883(10) . ? Os2 C21 1.913(11) . ? Os2 C22 1.930(10) . ? Os2 O1 2.124(5) . ? Os2 Os3 2.8264(4) . ? Os3 C34 1.922(10) . ? Os3 C32 1.924(10) . ? Os3 C33 1.942(11) . ? Os3 C31 1.959(10) . ? O1 C1 1.430(9) . ? O2 C2 1.423(11) . ? O11 C11 1.130(10) . ? O12 C12 1.123(11) . ? O13 C13 1.150(11) . ? O21 C21 1.129(11) . ? O22 C22 1.117(11) . ? O23 C23 1.152(11) . ? O31 C31 1.119(10) . ? O32 C32 1.155(11) . ? O33 C33 1.140(12) . ? O34 C34 1.131(10) . ? C1 C2 1.500(12) . ? C2 C111 1.496(12) . ? C111 C112 1.373(13) . ? C111 C116 1.404(14) . ? C112 C113 1.373(14) . ? C113 C114 1.37(2) . ? C114 C115 1.39(2) . ? C115 C116 1.383(15) . ? 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 93.8(4) . . ? C13 Os1 C12 91.4(4) . . ? C11 Os1 C12 96.7(4) . . ? C13 Os1 O1 167.2(3) . . ? C11 Os1 O1 95.6(3) . . ? C12 Os1 O1 96.0(3) . . ? C13 Os1 Os2 118.3(3) . . ? C11 Os1 Os2 132.5(3) . . ? C12 Os1 Os2 115.0(3) . . ? O1 Os1 Os2 49.00(14) . . ? C13 Os1 Os3 90.9(3) . . ? C11 Os1 Os3 87.0(3) . . ? C12 Os1 Os3 175.5(3) . . ? O1 Os1 Os3 81.12(13) . . ? Os2 Os1 Os3 60.507(11) . . ? C23 Os2 C21 90.7(4) . . ? C23 Os2 C22 92.0(4) . . ? C21 Os2 C22 96.6(4) . . ? C23 Os2 O1 167.8(3) . . ? C21 Os2 O1 98.8(3) . . ? C22 Os2 O1 94.5(3) . . ? C23 Os2 Os1 119.1(3) . . ? C21 Os2 Os1 135.1(3) . . ? C22 Os2 Os1 113.5(3) . . ? O1 Os2 Os1 48.67(13) . . ? C23 Os2 Os3 91.9(3) . . ? C21 Os2 Os3 88.2(3) . . ? C22 Os2 Os3 173.8(3) . . ? O1 Os2 Os3 80.80(14) . . ? Os1 Os2 Os3 60.297(11) . . ? C34 Os3 C32 101.1(4) . . ? C34 Os3 C33 94.1(4) . . ? C32 Os3 C33 93.4(4) . . ? C34 Os3 C31 93.6(4) . . ? C32 Os3 C31 93.7(4) . . ? C33 Os3 C31 168.3(4) . . ? C34 Os3 Os1 159.2(3) . . ? C32 Os3 Os1 99.7(3) . . ? C33 Os3 Os1 85.5(3) . . ? C31 Os3 Os1 84.2(2) . . ? C34 Os3 Os2 100.0(3) . . ? C32 Os3 Os2 158.8(3) . . ? C33 Os3 Os2 84.6(3) . . ? C31 Os3 Os2 85.5(2) . . ? Os1 Os3 Os2 59.196(11) . . ? C1 O1 Os1 120.3(4) . . ? C1 O1 Os2 121.8(5) . . ? Os1 O1 Os2 82.3(2) . . ? O1 C1 C2 112.1(6) . . ? O2 C2 C111 108.2(7) . . ? O2 C2 C1 109.1(8) . . ? C111 C2 C1 110.9(7) . . ? O11 C11 Os1 176.1(8) . . ? O12 C12 Os1 174.2(8) . . ? O13 C13 Os1 178.4(9) . . ? O21 C21 Os2 177.0(9) . . ? O22 C22 Os2 176.4(9) . . ? O23 C23 Os2 176.7(9) . . ? O31 C31 Os3 178.9(7) . . ? O32 C32 Os3 178.2(8) . . ? O33 C33 Os3 179.0(9) . . ? O34 C34 Os3 178.4(8) . . ? C112 C111 C116 118.9(9) . . ? C112 C111 C2 122.1(8) . . ? C116 C111 C2 119.0(9) . . ? C111 C112 C113 121.3(11) . . ? C114 C113 C112 120.4(12) . . ? C113 C114 C115 119.5(10) . . ? C116 C115 C114 120.3(12) . . ? C115 C116 C111 119.7(11) . . ? _refine_diff_density_max 0.824 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.161 #==================================================================== # CRYSTAL DATA FOR COMPOUND 3 #========================================================================= data_mw2 _database_code_CSD 163863 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H10 O13 Os3' _chemical_formula_weight 1016.87 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' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.54960(10) _cell_length_b 11.53980(10) _cell_length_c 14.343 _cell_angle_alpha 90.9100(10) _cell_angle_beta 93.8750(10) _cell_angle_gamma 93.1970(10) _cell_volume 1244.54(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5467 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.465 _exptl_crystal_size_mid 0.263 _exptl_crystal_size_min 0.150 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 15.339 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.050690 _exptl_absorpt_correction_T_max 0.139959 _exptl_absorpt_process_details ? _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_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8636 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 29.41 _reflns_number_total 5942 _reflns_number_gt 4608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5942 _refine_ls_number_parameters 319 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0638 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.09568(5) -0.71192(3) 0.16272(3) 0.03910(12) Uani 1 1 d D . . Os2 Os 0.11974(5) -0.72305(4) 0.35811(3) 0.04137(12) Uani 1 1 d D . . Os3 Os -0.19001(5) -0.81539(4) 0.25487(3) 0.04334(13) Uani 1 1 d . . . O1 O 0.0729(9) -0.5843(6) 0.2682(4) 0.0420(15) Uani 1 1 d . . . O2 O -0.0487(11) -0.3494(7) 0.2391(5) 0.058(2) Uani 1 1 d . . . O3 O -0.1366(15) -0.2983(11) 0.0961(7) 0.103(4) Uani 1 1 d . . . O11 O -0.1815(12) -0.6241(11) 0.0218(6) 0.087(3) Uani 1 1 d . . . O12 O 0.4206(12) -0.5964(9) 0.0768(7) 0.081(3) Uani 1 1 d . . . O13 O 0.1442(13) -0.9264(9) 0.0443(7) 0.084(3) Uani 1 1 d . . . O21 O -0.1153(16) -0.6540(12) 0.5093(7) 0.109(4) Uani 1 1 d . . . O22 O 0.4733(12) -0.6191(9) 0.4496(7) 0.081(3) Uani 1 1 d . . . O23 O 0.1717(14) -0.9531(9) 0.4515(7) 0.091(3) Uani 1 1 d . . . O31 O -0.3210(11) -0.5676(8) 0.2680(8) 0.077(3) Uani 1 1 d . . . O32 O -0.4140(14) -0.8955(9) 0.4141(7) 0.085(3) Uani 1 1 d . . . O33 O 0.0043(13) -1.0392(8) 0.2399(8) 0.089(3) Uani 1 1 d . . . O34 O -0.4370(14) -0.8794(9) 0.0799(7) 0.090(3) Uani 1 1 d . . . C1 C 0.1813(15) -0.4785(9) 0.2742(8) 0.053(3) Uani 1 1 d . . . H1A H 0.3024 -0.4942 0.2615 0.080 Uiso 1 1 calc R . . H1B H 0.1828 -0.4454 0.3368 0.080 Uiso 1 1 calc R . . C2 C 0.1088(17) -0.3921(10) 0.2036(8) 0.058(3) Uani 1 1 d . . . H2A H 0.1962 -0.3287 0.1964 0.087 Uiso 1 1 calc R . . H2B H 0.0808 -0.4301 0.1432 0.087 Uiso 1 1 calc R . . C3 C -0.1609(18) -0.3015(11) 0.1769(8) 0.061(3) Uani 1 1 d . . . C11 C -0.0798(17) -0.6565(11) 0.0724(8) 0.060(3) Uani 1 1 d . . . C12 C 0.3018(13) -0.6349(10) 0.1124(7) 0.049(2) Uani 1 1 d . . . C13 C 0.1218(14) -0.8455(11) 0.0892(8) 0.054(3) Uani 1 1 d . . . C21 C -0.0286(16) -0.6771(12) 0.4528(8) 0.064(3) Uani 1 1 d . . . C22 C 0.3405(14) -0.6570(11) 0.4133(8) 0.054(3) Uani 1 1 d . . . C23 C 0.1516(14) -0.8657(12) 0.4176(8) 0.059(3) Uani 1 1 d . . . C31 C -0.2699(13) -0.6572(11) 0.2615(8) 0.050(3) Uani 1 1 d . . . C32 C -0.3293(17) -0.8680(10) 0.3565(9) 0.058(3) Uani 1 1 d . . . C33 C -0.0662(13) -0.9553(11) 0.2461(9) 0.055(3) Uani 1 1 d . . . C34 C -0.3484(17) -0.8566(12) 0.1464(10) 0.064(3) Uani 1 1 d . . . C41 C -0.3121(16) -0.2496(10) 0.2193(8) 0.053(3) Uani 1 1 d . . . C42 C -0.341(2) -0.2599(12) 0.3113(9) 0.077(4) Uani 1 1 d . . . H42 H -0.2654 -0.3028 0.3495 0.115 Uiso 1 1 calc R . . C43 C -0.482(2) -0.2068(16) 0.3493(11) 0.101(6) Uani 1 1 d . . . H43 H -0.5001 -0.2134 0.4125 0.151 Uiso 1 1 calc R . . C44 C -0.592(2) -0.1462(13) 0.2940(11) 0.080(4) Uani 1 1 d . . . H44 H -0.6878 -0.1118 0.3183 0.121 Uiso 1 1 calc R . . C45 C -0.561(2) -0.1353(13) 0.1995(13) 0.091(5) Uani 1 1 d . . . H45 H -0.6357 -0.0918 0.1615 0.136 Uiso 1 1 calc R . . C46 C -0.4227(17) -0.1873(12) 0.1615(10) 0.070(4) Uani 1 1 d . . . H46 H -0.4041 -0.1806 0.0984 0.105 Uiso 1 1 calc R . . H12 H 0.227(10) -0.762(11) 0.2582(14) 0.100 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.0340(2) 0.0483(2) 0.0356(2) 0.00262(16) 0.00169(14) 0.00737(16) Os2 0.0366(2) 0.0524(3) 0.0358(2) 0.00641(16) -0.00025(14) 0.01016(17) Os3 0.0315(2) 0.0477(3) 0.0513(2) 0.00874(18) 0.00110(16) 0.00612(16) O1 0.044(4) 0.045(4) 0.039(3) 0.004(3) 0.005(3) 0.009(3) O2 0.072(5) 0.055(5) 0.050(4) 0.001(4) 0.006(4) 0.024(4) O3 0.105(8) 0.158(11) 0.055(6) 0.025(6) 0.013(5) 0.056(8) O11 0.059(5) 0.149(10) 0.056(5) 0.026(6) -0.005(4) 0.033(6) O12 0.052(5) 0.103(8) 0.089(7) 0.013(6) 0.021(5) -0.006(5) O13 0.078(7) 0.078(7) 0.093(7) -0.036(6) -0.001(5) 0.004(5) O21 0.094(8) 0.179(12) 0.061(6) -0.019(7) 0.022(6) 0.044(8) O22 0.059(6) 0.094(7) 0.085(7) -0.003(5) -0.025(5) -0.002(5) O23 0.085(7) 0.089(8) 0.099(8) 0.053(6) 0.003(6) 0.012(6) O31 0.051(5) 0.065(6) 0.119(8) 0.002(5) 0.004(5) 0.024(4) O32 0.082(7) 0.093(7) 0.088(7) 0.032(6) 0.035(6) 0.015(6) O33 0.064(6) 0.052(6) 0.150(10) 0.005(6) -0.008(6) 0.018(5) O34 0.080(7) 0.106(8) 0.077(7) 0.008(6) -0.035(5) -0.014(6) C1 0.049(6) 0.049(7) 0.061(7) 0.000(5) 0.005(5) 0.002(5) C2 0.078(8) 0.043(6) 0.056(7) 0.006(5) 0.013(6) 0.011(6) C3 0.080(9) 0.054(7) 0.049(7) 0.011(5) 0.005(6) 0.011(6) C11 0.061(7) 0.077(9) 0.045(6) 0.016(6) 0.009(5) 0.010(6) C12 0.037(5) 0.061(7) 0.048(6) 0.006(5) 0.000(4) 0.007(5) C13 0.039(6) 0.070(8) 0.054(7) -0.008(6) 0.002(5) 0.003(5) C21 0.053(7) 0.094(10) 0.047(6) 0.006(6) 0.003(5) 0.026(7) C22 0.036(5) 0.067(8) 0.059(7) 0.003(5) -0.007(5) 0.010(5) C23 0.038(6) 0.078(9) 0.060(7) 0.021(6) -0.002(5) -0.004(5) C31 0.031(5) 0.061(7) 0.059(7) 0.002(5) 0.000(4) 0.000(5) C32 0.061(7) 0.040(6) 0.074(8) 0.007(5) 0.007(6) 0.006(5) C33 0.031(5) 0.060(7) 0.073(8) 0.004(6) -0.002(5) 0.008(5) C34 0.057(7) 0.067(8) 0.067(8) 0.004(6) 0.003(6) -0.008(6) C41 0.065(7) 0.044(6) 0.050(6) 0.001(5) 0.002(5) 0.003(5) C42 0.103(11) 0.086(10) 0.045(7) -0.004(6) 0.000(7) 0.052(8) C43 0.117(14) 0.120(15) 0.071(10) -0.012(9) 0.008(9) 0.065(12) C44 0.071(9) 0.080(10) 0.093(11) 0.004(8) 0.005(8) 0.031(8) C45 0.070(10) 0.070(10) 0.132(15) 0.023(9) -0.010(9) 0.021(8) C46 0.056(7) 0.082(10) 0.072(9) 0.020(7) -0.009(6) 0.016(7) _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 1.881(12) . ? Os1 C11 1.932(12) . ? Os1 C12 1.936(11) . ? Os1 O1 2.117(6) . ? Os1 Os2 2.8016(5) . ? Os1 Os3 2.8237(5) . ? Os2 C23 1.886(13) . ? Os2 C21 1.905(12) . ? Os2 C22 1.910(11) . ? Os2 O1 2.102(7) . ? Os2 Os3 2.8286(6) . ? Os3 C33 1.917(12) . ? Os3 C34 1.934(14) . ? Os3 C32 1.940(13) . ? Os3 C31 1.958(12) . ? O1 C1 1.429(12) . ? O2 C3 1.336(14) . ? O2 C2 1.434(14) . ? O3 C3 1.186(15) . ? O11 C11 1.105(14) . ? O12 C12 1.135(13) . ? O13 C13 1.152(13) . ? O21 C21 1.114(14) . ? O22 C22 1.158(13) . ? O23 C23 1.140(14) . ? O31 C31 1.127(13) . ? O32 C32 1.118(14) . ? O33 C33 1.135(13) . ? O34 C34 1.146(14) . ? C1 C2 1.528(16) . ? C3 C41 1.480(17) . ? C41 C42 1.358(16) . ? C41 C46 1.375(16) . ? C42 C43 1.398(19) . ? C43 C44 1.34(2) . ? C44 C45 1.40(2) . ? C45 C46 1.37(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 C13 Os1 C11 91.6(5) . . ? C13 Os1 C12 91.0(5) . . ? C11 Os1 C12 96.9(5) . . ? C13 Os1 O1 168.5(4) . . ? C11 Os1 O1 97.6(4) . . ? C12 Os1 O1 94.8(4) . . ? C13 Os1 Os2 120.3(4) . . ? C11 Os1 Os2 133.6(3) . . ? C12 Os1 Os2 113.7(3) . . ? O1 Os1 Os2 48.17(18) . . ? C13 Os1 Os3 93.3(3) . . ? C11 Os1 Os3 87.3(3) . . ? C12 Os1 Os3 173.9(3) . . ? O1 Os1 Os3 80.27(18) . . ? Os2 Os1 Os3 60.373(14) . . ? C23 Os2 C21 90.4(5) . . ? C23 Os2 C22 92.1(5) . . ? C21 Os2 C22 98.0(5) . . ? C23 Os2 O1 168.8(4) . . ? C21 Os2 O1 96.9(4) . . ? C22 Os2 O1 95.2(4) . . ? C23 Os2 Os1 120.5(4) . . ? C21 Os2 Os1 133.8(4) . . ? C22 Os2 Os1 112.8(3) . . ? O1 Os2 Os1 48.61(17) . . ? C23 Os2 Os3 91.5(3) . . ? C21 Os2 Os3 88.0(4) . . ? C22 Os2 Os3 172.9(3) . . ? O1 Os2 Os3 80.38(18) . . ? Os1 Os2 Os3 60.200(13) . . ? C33 Os3 C34 92.9(5) . . ? C33 Os3 C32 94.8(5) . . ? C34 Os3 C32 102.1(5) . . ? C33 Os3 C31 168.6(4) . . ? C34 Os3 C31 93.0(5) . . ? C32 Os3 C31 93.4(5) . . ? C33 Os3 Os1 85.2(3) . . ? C34 Os3 Os1 98.6(4) . . ? C32 Os3 Os1 159.3(4) . . ? C31 Os3 Os1 84.4(3) . . ? C33 Os3 Os2 85.8(3) . . ? C34 Os3 Os2 158.0(4) . . ? C32 Os3 Os2 99.9(4) . . ? C31 Os3 Os2 85.1(3) . . ? Os1 Os3 Os2 59.428(13) . . ? C1 O1 Os2 122.2(6) . . ? C1 O1 Os1 122.3(6) . . ? Os2 O1 Os1 83.2(2) . . ? C3 O2 C2 116.2(9) . . ? O1 C1 C2 110.1(9) . . ? O2 C2 C1 107.1(9) . . ? O3 C3 O2 122.4(13) . . ? O3 C3 C41 124.0(12) . . ? O2 C3 C41 113.5(10) . . ? O11 C11 Os1 178.9(12) . . ? O12 C12 Os1 174.2(11) . . ? O13 C13 Os1 177.5(10) . . ? O21 C21 Os2 177.6(14) . . ? O22 C22 Os2 177.6(11) . . ? O23 C23 Os2 178.3(12) . . ? O31 C31 Os3 177.1(10) . . ? O32 C32 Os3 177.5(12) . . ? O33 C33 Os3 178.6(11) . . ? O34 C34 Os3 177.2(12) . . ? C42 C41 C46 120.6(12) . . ? C42 C41 C3 122.4(11) . . ? C46 C41 C3 117.0(11) . . ? C41 C42 C43 120.7(13) . . ? C44 C43 C42 119.6(15) . . ? C43 C44 C45 119.4(14) . . ? C46 C45 C44 121.4(14) . . ? C45 C46 C41 118.4(14) . . ? _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 29.41 _diffrn_measured_fraction_theta_full 0.863 _refine_diff_density_max 2.201 _refine_diff_density_min -2.977 _refine_diff_density_rms 0.285 #==================================================================== # CRYSTAL DATA FOR COMPOUND 6 #========================================================================= data_mw1 _database_code_CSD 163864 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H21 O11 Os3 P' _chemical_formula_weight 1147.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.80900(10) _cell_length_b 10.84560(10) _cell_length_c 16.42700(10) _cell_angle_alpha 104.8590(10) _cell_angle_beta 102.3200(10) _cell_angle_gamma 93.1600(10) _cell_volume 1639.04(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6398 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.036 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 11.704 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.263592 _exptl_absorpt_correction_T_max 0.404929 _exptl_absorpt_process_details ? _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_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10752 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 29.05 _reflns_number_total 7403 _reflns_number_gt 5766 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7403 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.91412(3) 0.30975(3) 0.135739(18) 0.03415(8) Uani 1 1 d . . . Os2 Os 0.71501(3) 0.32504(3) 0.239305(18) 0.02961(8) Uani 1 1 d . . . Os3 Os 0.70333(3) 0.47888(3) 0.120171(19) 0.03551(8) Uani 1 1 d . . . P1 P 0.75886(19) 0.19716(18) 0.33974(12) 0.0324(4) Uani 1 1 d . . . O1 O 0.7339(5) 0.1795(5) 0.1252(3) 0.0340(11) Uani 1 1 d . . . O2 O 0.6395(8) -0.0220(7) -0.0381(4) 0.079(2) Uani 1 1 d . . . H2 H 0.6158 0.0507 -0.0284 0.119 Uiso 1 1 calc R . . O11 O 1.1348(7) 0.1230(7) 0.1699(5) 0.075(2) Uani 1 1 d . . . O12 O 0.8990(8) 0.2537(8) -0.0604(4) 0.082(2) Uani 1 1 d . . . O13 O 1.1380(7) 0.5383(7) 0.1778(4) 0.0680(19) Uani 1 1 d . . . O22 O 0.3961(6) 0.3144(7) 0.2153(5) 0.072(2) Uani 1 1 d . . . O23 O 0.7422(7) 0.5643(6) 0.3886(4) 0.0708(19) Uani 1 1 d . . . O31 O 0.5267(7) 0.2403(6) -0.0194(4) 0.0641(18) Uani 1 1 d . . . O32 O 0.7748(7) 0.6168(7) -0.0110(4) 0.0698(19) Uani 1 1 d . . . O33 O 0.9009(7) 0.6906(7) 0.2700(5) 0.078(2) Uani 1 1 d . . . O34 O 0.4376(7) 0.5961(7) 0.1581(5) 0.073(2) Uani 1 1 d . . . C1 C 0.7457(9) 0.0428(7) 0.1174(5) 0.0415(18) Uani 1 1 d . . . H1A H 0.6640 0.0042 0.1290 0.062 Uiso 1 1 calc R . . H1B H 0.8265 0.0341 0.1594 0.062 Uiso 1 1 calc R . . C2 C 0.7591(10) -0.0260(8) 0.0273(6) 0.056(2) Uani 1 1 d . . . H2A H 0.8419 0.0132 0.0161 0.067 Uiso 1 1 calc R . . H2B H 0.7719 -0.1149 0.0246 0.067 Uiso 1 1 calc R . . C11 C 1.0512(9) 0.1932(9) 0.1592(6) 0.049(2) Uani 1 1 d . . . C12 C 0.9061(9) 0.2752(9) 0.0132(6) 0.052(2) Uani 1 1 d . . . C13 C 1.0554(8) 0.4521(9) 0.1609(5) 0.045(2) Uani 1 1 d . . . C22 C 0.5174(8) 0.3143(7) 0.2241(5) 0.0425(19) Uani 1 1 d . . . C23 C 0.7322(8) 0.4713(8) 0.3309(5) 0.0425(19) Uani 1 1 d . . . C31 C 0.5938(9) 0.3270(8) 0.0334(6) 0.047(2) Uani 1 1 d . . . C32 C 0.7489(8) 0.5607(8) 0.0363(5) 0.0438(19) Uani 1 1 d . . . C33 C 0.8272(9) 0.6104(8) 0.2150(6) 0.048(2) Uani 1 1 d . . . C34 C 0.5356(9) 0.5539(8) 0.1431(6) 0.050(2) Uani 1 1 d . . . C111 C 0.6369(8) 0.0517(7) 0.3232(5) 0.0392(18) Uani 1 1 d . . . C112 C 0.6521(10) -0.0167(9) 0.3858(6) 0.060(3) Uani 1 1 d . . . H11A H 0.7282 0.0075 0.4336 0.072 Uiso 1 1 calc R . . C113 C 0.5556(12) -0.1194(10) 0.3774(7) 0.070(3) Uani 1 1 d . . . H11B H 0.5674 -0.1632 0.4198 0.085 Uiso 1 1 calc R . . C114 C 0.4419(11) -0.1582(9) 0.3070(7) 0.065(3) Uani 1 1 d . . . H11C H 0.3792 -0.2291 0.3013 0.078 Uiso 1 1 calc R . . C115 C 0.4214(9) -0.0909(9) 0.2445(6) 0.056(2) Uani 1 1 d . . . H11D H 0.3446 -0.1164 0.1972 0.067 Uiso 1 1 calc R . . C116 C 0.5179(8) 0.0165(8) 0.2533(5) 0.0437(19) Uani 1 1 d . . . H11E H 0.5027 0.0637 0.2129 0.052 Uiso 1 1 calc R . . C121 C 0.9361(8) 0.1467(8) 0.3584(5) 0.0375(17) Uani 1 1 d . . . C122 C 1.0509(8) 0.2436(9) 0.3840(5) 0.047(2) Uani 1 1 d . . . H12A H 1.0346 0.3290 0.3914 0.056 Uiso 1 1 calc R . . C123 C 1.1897(9) 0.2127(10) 0.3984(6) 0.060(3) Uani 1 1 d . . . H12B H 1.2641 0.2779 0.4159 0.072 Uiso 1 1 calc R . . C124 C 1.2162(10) 0.0882(11) 0.3871(7) 0.068(3) Uani 1 1 d . . . H12C H 1.3084 0.0687 0.3981 0.082 Uiso 1 1 calc R . . C125 C 1.1050(10) -0.0096(10) 0.3591(7) 0.075(3) Uani 1 1 d . . . H12D H 1.1227 -0.0949 0.3488 0.089 Uiso 1 1 calc R . . C126 C 0.9668(9) 0.0201(8) 0.3463(6) 0.054(2) Uani 1 1 d . . . H12E H 0.8934 -0.0460 0.3294 0.065 Uiso 1 1 calc R . . C131 C 0.7412(8) 0.2878(7) 0.4495(5) 0.0349(16) Uani 1 1 d . . . C132 C 0.6066(8) 0.3147(8) 0.4585(5) 0.045(2) Uani 1 1 d . . . H13A H 0.5305 0.2857 0.4110 0.054 Uiso 1 1 calc R . . C133 C 0.5854(9) 0.3839(8) 0.5373(5) 0.048(2) Uani 1 1 d . . . H13B H 0.4951 0.4012 0.5419 0.058 Uiso 1 1 calc R . . C134 C 0.6961(10) 0.4277(9) 0.6094(6) 0.057(2) Uani 1 1 d . . . H13C H 0.6816 0.4739 0.6623 0.069 Uiso 1 1 calc R . . C135 C 0.8292(10) 0.4006(10) 0.6004(6) 0.067(3) Uani 1 1 d . . . H13D H 0.9049 0.4304 0.6481 0.080 Uiso 1 1 calc R . . C136 C 0.8532(9) 0.3306(9) 0.5226(5) 0.048(2) Uani 1 1 d . . . H13E H 0.9435 0.3119 0.5189 0.058 Uiso 1 1 calc R . . H12 H 0.908(8) 0.332(8) 0.247(5) 0.06(2) Uiso 1 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 0.03067(15) 0.03944(18) 0.03332(16) 0.00949(13) 0.01092(12) 0.00148(12) Os2 0.02985(14) 0.02950(15) 0.03055(15) 0.00820(12) 0.00976(11) 0.00227(11) Os3 0.03780(16) 0.03192(16) 0.03709(16) 0.01223(13) 0.00683(13) 0.00124(12) P1 0.0321(9) 0.0333(10) 0.0322(9) 0.0098(8) 0.0081(8) 0.0011(8) O1 0.034(3) 0.036(3) 0.030(2) 0.004(2) 0.009(2) 0.005(2) O2 0.097(5) 0.074(5) 0.050(4) 0.001(4) 0.001(4) 0.010(4) O11 0.059(4) 0.080(5) 0.087(5) 0.019(4) 0.019(4) 0.028(4) O12 0.088(5) 0.121(7) 0.034(3) 0.013(4) 0.020(3) -0.002(5) O13 0.057(4) 0.077(5) 0.067(4) 0.013(4) 0.022(3) -0.018(4) O22 0.033(3) 0.080(5) 0.104(5) 0.025(4) 0.020(3) 0.008(3) O23 0.100(5) 0.044(4) 0.059(4) -0.010(3) 0.029(4) 0.003(4) O31 0.075(4) 0.044(4) 0.059(4) 0.012(3) -0.010(3) -0.002(3) O32 0.087(5) 0.068(5) 0.065(4) 0.035(4) 0.024(4) -0.003(4) O33 0.083(5) 0.050(4) 0.074(5) -0.005(4) -0.006(4) -0.012(4) O34 0.059(4) 0.068(5) 0.087(5) 0.000(4) 0.030(4) 0.012(4) C1 0.054(5) 0.032(4) 0.040(4) 0.011(4) 0.013(4) 0.006(4) C2 0.066(6) 0.038(5) 0.061(6) -0.003(4) 0.027(5) -0.004(4) C11 0.044(5) 0.057(6) 0.052(5) 0.016(5) 0.022(4) 0.003(4) C12 0.042(5) 0.062(6) 0.049(5) 0.010(5) 0.014(4) -0.002(4) C13 0.039(4) 0.054(5) 0.040(4) 0.009(4) 0.011(4) -0.006(4) C22 0.048(5) 0.035(4) 0.047(5) 0.010(4) 0.019(4) 0.002(4) C23 0.046(4) 0.051(5) 0.035(4) 0.013(4) 0.016(4) 0.007(4) C31 0.057(5) 0.037(5) 0.050(5) 0.022(4) 0.007(4) 0.006(4) C32 0.047(5) 0.039(5) 0.047(5) 0.013(4) 0.013(4) 0.003(4) C33 0.052(5) 0.041(5) 0.053(5) 0.020(4) 0.008(4) 0.007(4) C34 0.048(5) 0.046(5) 0.053(5) 0.010(4) 0.015(4) -0.001(4) C111 0.043(4) 0.029(4) 0.041(4) 0.004(3) 0.009(4) -0.002(3) C112 0.068(6) 0.056(6) 0.053(5) 0.024(5) 0.005(5) -0.010(5) C113 0.089(8) 0.058(7) 0.076(7) 0.035(6) 0.027(6) 0.001(6) C114 0.074(7) 0.043(5) 0.074(7) -0.002(5) 0.036(6) -0.019(5) C115 0.055(5) 0.050(6) 0.055(5) 0.000(5) 0.017(4) -0.011(4) C116 0.050(5) 0.043(5) 0.040(4) 0.009(4) 0.020(4) 0.001(4) C121 0.035(4) 0.045(5) 0.030(4) 0.007(3) 0.008(3) 0.010(3) C122 0.036(4) 0.052(5) 0.053(5) 0.017(4) 0.008(4) 0.010(4) C123 0.044(5) 0.067(7) 0.063(6) 0.012(5) 0.009(5) -0.001(5) C124 0.042(5) 0.080(8) 0.079(7) 0.019(6) 0.006(5) 0.021(5) C125 0.061(6) 0.056(6) 0.098(8) 0.009(6) 0.009(6) 0.031(5) C126 0.047(5) 0.039(5) 0.071(6) 0.008(5) 0.009(5) 0.011(4) C131 0.039(4) 0.034(4) 0.032(4) 0.014(3) 0.005(3) 0.004(3) C132 0.036(4) 0.059(6) 0.039(4) 0.016(4) 0.002(3) 0.005(4) C133 0.050(5) 0.049(5) 0.053(5) 0.017(4) 0.023(4) 0.013(4) C134 0.069(6) 0.060(6) 0.042(5) 0.008(5) 0.017(5) 0.011(5) C135 0.063(6) 0.090(8) 0.035(5) -0.001(5) 0.006(4) 0.010(6) C136 0.043(5) 0.065(6) 0.034(4) 0.011(4) 0.005(4) 0.011(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 C13 1.915(8) . ? Os1 C12 1.934(9) . ? Os1 C11 1.942(10) . ? Os1 O1 2.150(5) . ? Os1 Os2 2.8364(4) . ? Os1 Os3 2.8528(4) . ? Os2 C23 1.857(8) . ? Os2 C22 1.894(8) . ? Os2 O1 2.168(5) . ? Os2 P1 2.4015(19) . ? Os2 Os3 2.8682(4) . ? Os3 C32 1.932(8) . ? Os3 C34 1.941(9) . ? Os3 C33 1.949(9) . ? Os3 C31 1.961(9) . ? P1 C121 1.839(8) . ? P1 C111 1.852(7) . ? P1 C131 1.868(8) . ? O1 C1 1.468(9) . ? O2 C2 1.423(11) . ? O11 C11 1.166(10) . ? O12 C12 1.157(10) . ? O13 C13 1.138(9) . ? O22 C22 1.168(9) . ? O23 C23 1.176(9) . ? O31 C31 1.158(9) . ? O32 C32 1.161(9) . ? O33 C33 1.160(9) . ? O34 C34 1.133(10) . ? C1 C2 1.514(11) . ? C111 C112 1.403(11) . ? C111 C116 1.407(11) . ? C112 C113 1.381(12) . ? C113 C114 1.381(14) . ? C114 C115 1.393(13) . ? C115 C116 1.418(11) . ? C121 C126 1.394(11) . ? C121 C122 1.411(10) . ? C122 C123 1.405(12) . ? C123 C124 1.362(13) . ? C124 C125 1.392(13) . ? C125 C126 1.395(12) . ? C131 C132 1.397(10) . ? C131 C136 1.400(10) . ? C132 C133 1.385(11) . ? C133 C134 1.383(12) . ? C134 C135 1.384(13) . ? C135 C136 1.384(11) . ? 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 C12 90.7(3) . . ? C13 Os1 C11 93.1(4) . . ? C12 Os1 C11 96.4(4) . . ? C13 Os1 O1 167.5(3) . . ? C12 Os1 O1 97.4(3) . . ? C11 Os1 O1 95.5(3) . . ? C13 Os1 Os2 118.8(2) . . ? C12 Os1 Os2 135.8(2) . . ? C11 Os1 Os2 112.7(2) . . ? O1 Os1 Os2 49.22(12) . . ? C13 Os1 Os3 89.3(3) . . ? C12 Os1 Os3 90.1(3) . . ? C11 Os1 Os3 173.0(2) . . ? O1 Os1 Os3 81.17(13) . . ? Os2 Os1 Os3 60.550(10) . . ? C23 Os2 C22 89.0(3) . . ? C23 Os2 O1 166.5(3) . . ? C22 Os2 O1 101.2(3) . . ? C23 Os2 P1 90.0(2) . . ? C22 Os2 P1 97.1(2) . . ? O1 Os2 P1 97.31(14) . . ? C23 Os2 Os1 118.0(2) . . ? C22 Os2 Os1 138.3(2) . . ? O1 Os2 Os1 48.65(12) . . ? P1 Os2 Os1 112.89(5) . . ? C23 Os2 Os3 90.7(2) . . ? C22 Os2 Os3 90.8(2) . . ? O1 Os2 Os3 80.51(13) . . ? P1 Os2 Os3 172.09(4) . . ? Os1 Os2 Os3 60.007(10) . . ? C32 Os3 C34 102.2(4) . . ? C32 Os3 C33 91.1(3) . . ? C34 Os3 C33 92.9(4) . . ? C32 Os3 C31 94.9(3) . . ? C34 Os3 C31 92.5(4) . . ? C33 Os3 C31 170.9(3) . . ? C32 Os3 Os1 102.9(2) . . ? C34 Os3 Os1 154.8(3) . . ? C33 Os3 Os1 88.6(3) . . ? C31 Os3 Os1 83.5(3) . . ? C32 Os3 Os2 162.3(2) . . ? C34 Os3 Os2 95.5(3) . . ? C33 Os3 Os2 86.8(2) . . ? C31 Os3 Os2 85.4(2) . . ? Os1 Os3 Os2 59.443(10) . . ? C121 P1 C111 105.7(4) . . ? C121 P1 C131 104.7(3) . . ? C111 P1 C131 98.9(3) . . ? C121 P1 Os2 114.9(3) . . ? C111 P1 Os2 119.5(3) . . ? C131 P1 Os2 111.2(2) . . ? C1 O1 Os1 120.9(4) . . ? C1 O1 Os2 127.0(4) . . ? Os1 O1 Os2 82.12(16) . . ? O1 C1 C2 110.6(6) . . ? O2 C2 C1 112.5(7) . . ? O11 C11 Os1 177.1(8) . . ? O12 C12 Os1 178.9(8) . . ? O13 C13 Os1 178.2(8) . . ? O22 C22 Os2 176.6(7) . . ? O23 C23 Os2 179.4(8) . . ? O31 C31 Os3 177.5(7) . . ? O32 C32 Os3 175.9(7) . . ? O33 C33 Os3 178.3(8) . . ? O34 C34 Os3 178.2(9) . . ? C112 C111 C116 118.5(7) . . ? C112 C111 P1 120.3(6) . . ? C116 C111 P1 120.7(6) . . ? C113 C112 C111 120.8(9) . . ? C112 C113 C114 121.0(9) . . ? C113 C114 C115 119.8(8) . . ? C114 C115 C116 119.8(8) . . ? C111 C116 C115 119.9(8) . . ? C126 C121 C122 117.1(7) . . ? C126 C121 P1 125.5(6) . . ? C122 C121 P1 117.4(6) . . ? C123 C122 C121 120.8(8) . . ? C124 C123 C122 120.7(9) . . ? C123 C124 C125 119.7(9) . . ? C124 C125 C126 120.1(9) . . ? C121 C126 C125 121.6(8) . . ? C132 C131 C136 118.2(7) . . ? C132 C131 P1 117.3(6) . . ? C136 C131 P1 124.5(6) . . ? C133 C132 C131 120.8(7) . . ? C134 C133 C132 121.1(8) . . ? C133 C134 C135 118.0(8) . . ? C134 C135 C136 122.0(8) . . ? C135 C136 C131 119.8(8) . . ? _diffrn_measured_fraction_theta_max 0.843 _diffrn_reflns_theta_full 29.05 _diffrn_measured_fraction_theta_full 0.843 _refine_diff_density_max 1.137 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.188 #==END====