Supplementary Material (ESI) for Dalton Transactions Thsi journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Leong, Weng Kee' 'Leong, Wei Lin Janet' 'Zhang, Junlian' _publ_contact_author_name 'Dr Weng Kee Leong' _publ_contact_author_address ; Dr Weng Kee Leong Department of Chemistry National University of Singapore Kent Ridge 119260 SINGAPORE ; _publ_contact_author_email 'chmlwk@nus.edu.sg' data_3 _database_code_CSD 155039 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H15 O9 Os3 P Se' _chemical_formula_weight 1163.92 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' 'Se' 'Se' -0.0929 2.2259 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9599(3) _cell_length_b 9.78440(10) _cell_length_c 20.7467(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.7030(10) _cell_angle_gamma 90.00 _cell_volume 2993.33(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 14.022 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.153960 _exptl_absorpt_correction_T_max 0.036772 _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 7395 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 29.14 _reflns_number_total 7395 _reflns_number_gt 6114 _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^)+(0.0452P)^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 SHELXL _refine_ls_extinction_coef 0.00180(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7395 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.284025(14) 0.62038(2) 0.090116(11) 0.03186(8) Uani 1 1 d . . . Os2 Os 0.439202(15) 0.47904(2) 0.156942(12) 0.03399(8) Uani 1 1 d . . . Os3 Os 0.410119(16) 0.74857(2) 0.188687(12) 0.03689(8) Uani 1 1 d . . . Se4 Se 0.44796(4) 0.67460(6) 0.07950(3) 0.03529(14) Uani 1 1 d . . . P1 P 0.22033(10) 0.67961(15) -0.01967(7) 0.0309(3) Uani 1 1 d . . . O11 O 0.2157(4) 0.9081(5) 0.1165(3) 0.0647(15) Uani 1 1 d . . . O12 O 0.1254(4) 0.5326(6) 0.1555(3) 0.0747(18) Uani 1 1 d . . . O13 O 0.2704(3) 0.3168(5) 0.0505(3) 0.0611(14) Uani 1 1 d . . . O21 O 0.4738(4) 0.2323(6) 0.0738(3) 0.0819(19) Uani 1 1 d . . . O22 O 0.3647(5) 0.3313(7) 0.2659(3) 0.088(2) Uani 1 1 d . . . O23 O 0.6278(4) 0.4625(7) 0.2361(3) 0.088(2) Uani 1 1 d . . . O31 O 0.5959(4) 0.7664(7) 0.2705(3) 0.086(2) Uani 1 1 d . . . O32 O 0.3119(4) 0.6986(8) 0.3042(3) 0.0827(19) Uani 1 1 d . . . O33 O 0.4011(5) 1.0622(6) 0.1846(4) 0.098(2) Uani 1 1 d . . . C11 C 0.2556(4) 0.8082(7) 0.1135(3) 0.0436(15) Uani 1 1 d . . . C12 C 0.1844(4) 0.5675(7) 0.1306(4) 0.0468(16) Uani 1 1 d . . . C13 C 0.2888(4) 0.4255(7) 0.0691(4) 0.0443(15) Uani 1 1 d . . . C21 C 0.4615(5) 0.3252(8) 0.1042(4) 0.0486(16) Uani 1 1 d . . . C22 C 0.3907(5) 0.3853(7) 0.2234(4) 0.0493(16) Uani 1 1 d . . . C23 C 0.5565(5) 0.4691(8) 0.2065(4) 0.0553(19) Uani 1 1 d . . . C31 C 0.5257(6) 0.7578(8) 0.2409(4) 0.0573(19) Uani 1 1 d . . . C32 C 0.3494(5) 0.7204(7) 0.2616(4) 0.0501(17) Uani 1 1 d . . . C33 C 0.4028(5) 0.9427(8) 0.1852(4) 0.0545(18) Uani 1 1 d . . . C111 C 0.2097(4) 0.5329(6) -0.0760(3) 0.0376(13) Uani 1 1 d . . . C112 C 0.2892(5) 0.4615(7) -0.0828(4) 0.0508(17) Uani 1 1 d . . . H112 H 0.3449 0.4903 -0.0600 0.061 Uiso 1 1 calc R . . C113 C 0.2850(6) 0.3507(8) -0.1226(4) 0.061(2) Uani 1 1 d . . . H113 H 0.3381 0.3061 -0.1281 0.074 Uiso 1 1 calc R . . C114 C 0.2034(7) 0.3040(9) -0.1547(4) 0.076(3) Uani 1 1 d . . . H114 H 0.2013 0.2239 -0.1791 0.091 Uiso 1 1 calc R . . C115 C 0.1238(7) 0.3739(9) -0.1514(4) 0.072(2) Uani 1 1 d . . . H115 H 0.0690 0.3447 -0.1756 0.087 Uiso 1 1 calc R . . C116 C 0.1272(5) 0.4914(7) -0.1105(4) 0.0517(17) Uani 1 1 d . . . H116 H 0.0746 0.5394 -0.1070 0.062 Uiso 1 1 calc R . . C121 C 0.1063(4) 0.7528(6) -0.0300(3) 0.0375(13) Uani 1 1 d . . . C122 C 0.0815(5) 0.8644(7) -0.0720(4) 0.0494(17) Uani 1 1 d . . . H122 H 0.1238 0.9045 -0.0943 0.059 Uiso 1 1 calc R . . C123 C -0.0070(5) 0.9147(8) -0.0802(4) 0.060(2) Uani 1 1 d . . . H123 H -0.0225 0.9916 -0.1060 0.072 Uiso 1 1 calc R . . C124 C -0.0707(5) 0.8530(8) -0.0510(4) 0.0584(19) Uani 1 1 d . . . H124 H -0.1301 0.8847 -0.0586 0.070 Uiso 1 1 calc R . . C125 C -0.0473(5) 0.7427(9) -0.0099(5) 0.066(2) Uani 1 1 d . . . H125 H -0.0906 0.7020 0.0112 0.080 Uiso 1 1 calc R . . C126 C 0.0416(4) 0.6921(8) 0.0001(4) 0.0532(19) Uani 1 1 d . . . H126 H 0.0568 0.6171 0.0272 0.064 Uiso 1 1 calc R . . C131 C 0.2843(4) 0.8038(6) -0.0597(3) 0.0341(12) Uani 1 1 d . . . C132 C 0.3288(5) 0.9125(6) -0.0243(4) 0.0459(15) Uani 1 1 d . . . H132 H 0.3292 0.9186 0.0205 0.055 Uiso 1 1 calc R . . C133 C 0.3731(5) 1.0127(7) -0.0559(4) 0.0548(19) Uani 1 1 d . . . H133 H 0.4018 1.0858 -0.0322 0.066 Uiso 1 1 calc R . . C134 C 0.3737(5) 1.0022(7) -0.1212(4) 0.0544(19) Uani 1 1 d . . . H134 H 0.4034 1.0682 -0.1420 0.065 Uiso 1 1 calc R . . C135 C 0.3307(5) 0.8951(8) -0.1569(4) 0.0552(18) Uani 1 1 d . . . H135 H 0.3314 0.8891 -0.2015 0.066 Uiso 1 1 calc R . . C136 C 0.2863(4) 0.7955(7) -0.1259(3) 0.0430(14) Uani 1 1 d . . . H136 H 0.2578 0.7229 -0.1501 0.052 Uiso 1 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 0.02930(12) 0.03752(13) 0.02798(13) 0.00553(9) 0.00255(9) 0.00298(8) Os2 0.03509(13) 0.03274(13) 0.03330(14) 0.00651(9) 0.00337(10) 0.00499(9) Os3 0.04560(15) 0.03339(13) 0.03094(14) -0.00084(9) 0.00433(11) -0.00379(10) Se4 0.0339(3) 0.0413(3) 0.0311(3) 0.0076(2) 0.0066(2) -0.0002(2) P1 0.0313(7) 0.0315(7) 0.0283(7) 0.0025(6) 0.0008(6) 0.0022(6) O11 0.076(4) 0.059(3) 0.058(4) 0.003(3) 0.011(3) 0.028(3) O12 0.057(3) 0.095(4) 0.081(5) 0.019(3) 0.037(3) -0.010(3) O13 0.057(3) 0.043(3) 0.077(4) 0.001(3) -0.005(3) -0.008(2) O21 0.090(4) 0.083(4) 0.072(4) -0.016(3) 0.010(4) 0.039(3) O22 0.123(6) 0.090(5) 0.059(4) 0.017(4) 0.042(4) -0.021(4) O23 0.066(4) 0.089(5) 0.092(5) 0.030(4) -0.036(3) 0.008(3) O31 0.072(4) 0.105(5) 0.069(4) -0.010(4) -0.022(3) -0.010(4) O32 0.082(4) 0.121(6) 0.050(4) 0.014(4) 0.024(3) -0.003(4) O33 0.136(6) 0.035(3) 0.127(7) -0.002(3) 0.035(5) 0.001(3) C11 0.050(4) 0.046(4) 0.031(3) 0.001(3) 0.000(3) 0.007(3) C12 0.044(3) 0.049(4) 0.048(4) 0.007(3) 0.009(3) 0.006(3) C13 0.033(3) 0.047(4) 0.051(4) 0.015(3) 0.002(3) 0.002(3) C21 0.049(4) 0.057(4) 0.039(4) 0.000(3) 0.004(3) 0.018(3) C22 0.060(4) 0.043(4) 0.045(4) 0.006(3) 0.007(3) 0.000(3) C23 0.055(4) 0.052(4) 0.052(5) 0.016(3) -0.008(4) 0.004(3) C31 0.065(5) 0.056(4) 0.048(5) -0.010(3) 0.002(4) -0.005(4) C32 0.058(4) 0.055(4) 0.035(4) -0.002(3) 0.001(3) 0.005(3) C33 0.065(5) 0.049(4) 0.051(5) -0.003(3) 0.015(4) -0.003(3) C111 0.044(3) 0.038(3) 0.030(3) 0.002(2) 0.005(3) -0.005(3) C112 0.054(4) 0.048(4) 0.052(5) -0.002(3) 0.013(3) 0.003(3) C113 0.086(6) 0.045(4) 0.055(5) -0.012(4) 0.018(4) 0.008(4) C114 0.120(8) 0.053(5) 0.057(5) -0.019(4) 0.023(6) -0.007(5) C115 0.086(6) 0.073(6) 0.053(5) -0.015(4) -0.002(5) -0.029(5) C116 0.056(4) 0.057(4) 0.039(4) -0.004(3) 0.000(3) -0.010(3) C121 0.035(3) 0.037(3) 0.038(3) 0.000(3) -0.001(3) 0.004(2) C122 0.048(4) 0.046(4) 0.053(4) 0.015(3) 0.004(3) 0.010(3) C123 0.056(4) 0.052(4) 0.066(5) 0.015(4) -0.004(4) 0.016(3) C124 0.043(4) 0.067(5) 0.063(5) 0.002(4) 0.001(4) 0.013(3) C125 0.036(4) 0.086(6) 0.076(6) 0.021(5) 0.005(4) 0.005(4) C126 0.032(3) 0.062(4) 0.062(5) 0.020(4) 0.000(3) 0.005(3) C131 0.035(3) 0.036(3) 0.032(3) 0.006(2) 0.007(2) 0.003(2) C132 0.061(4) 0.034(3) 0.043(4) 0.005(3) 0.010(3) -0.004(3) C133 0.071(5) 0.033(3) 0.061(5) 0.003(3) 0.014(4) -0.012(3) C134 0.059(4) 0.045(4) 0.062(5) 0.015(3) 0.018(4) -0.001(3) C135 0.068(5) 0.062(5) 0.038(4) 0.010(3) 0.017(4) -0.005(4) C136 0.044(3) 0.048(4) 0.036(3) 0.002(3) 0.003(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C12 1.902(7) . ? Os1 C13 1.960(7) . ? Os1 C11 1.965(7) . ? Os1 P1 2.3875(15) . ? Os1 Se4 2.5548(6) . ? Os1 Os3 2.8308(3) . ? Os1 Os2 2.8528(3) . ? Os2 C23 1.882(7) . ? Os2 C22 1.898(7) . ? Os2 C21 1.923(7) . ? Os2 Se4 2.5161(6) . ? Os2 Os3 2.7703(3) . ? Os3 C31 1.881(8) . ? Os3 C33 1.903(8) . ? Os3 C32 1.912(8) . ? Os3 Se4 2.5315(7) . ? P1 C121 1.828(6) . ? P1 C131 1.830(6) . ? P1 C111 1.842(6) . ? O11 C11 1.153(8) . ? O12 C12 1.146(8) . ? O13 C13 1.149(8) . ? O21 C21 1.139(8) . ? O22 C22 1.152(8) . ? O23 C23 1.139(8) . ? O31 C31 1.127(9) . ? O32 C32 1.144(9) . ? O33 C33 1.170(9) . ? C111 C116 1.379(9) . ? C111 C112 1.407(9) . ? C112 C113 1.358(10) . ? C113 C114 1.367(12) . ? C114 C115 1.385(13) . ? C115 C116 1.425(11) . ? C121 C126 1.373(9) . ? C121 C122 1.408(9) . ? C122 C123 1.395(9) . ? C123 C124 1.353(11) . ? C124 C125 1.384(11) . ? C125 C126 1.401(9) . ? C131 C136 1.382(9) . ? C131 C132 1.396(9) . ? C132 C133 1.405(9) . ? C133 C134 1.361(11) . ? C134 C135 1.378(11) . ? C135 C136 1.396(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Os1 C13 84.0(3) . . ? C12 Os1 C11 85.8(3) . . ? C13 Os1 C11 169.2(3) . . ? C12 Os1 P1 105.7(2) . . ? C13 Os1 P1 92.7(2) . . ? C11 Os1 P1 86.57(19) . . ? C12 Os1 Se4 158.4(2) . . ? C13 Os1 Se4 96.37(18) . . ? C11 Os1 Se4 94.5(2) . . ? P1 Os1 Se4 95.85(4) . . ? C12 Os1 Os3 106.1(2) . . ? C13 Os1 Os3 123.16(18) . . ? C11 Os1 Os3 63.45(18) . . ? P1 Os1 Os3 133.78(4) . . ? Se4 Os1 Os3 55.791(16) . . ? C12 Os1 Os2 106.7(2) . . ? C13 Os1 Os2 65.12(18) . . ? C11 Os1 Os2 121.71(18) . . ? P1 Os1 Os2 137.95(4) . . ? Se4 Os1 Os2 55.126(14) . . ? Os3 Os1 Os2 58.340(8) . . ? C23 Os2 C22 90.8(3) . . ? C23 Os2 C21 92.0(3) . . ? C22 Os2 C21 99.2(3) . . ? C23 Os2 Se4 104.1(2) . . ? C22 Os2 Se4 153.9(2) . . ? C21 Os2 Se4 101.5(2) . . ? C23 Os2 Os3 95.1(2) . . ? C22 Os2 Os3 101.1(2) . . ? C21 Os2 Os3 158.4(2) . . ? Se4 Os2 Os3 56.978(16) . . ? C23 Os2 Os1 154.0(2) . . ? C22 Os2 Os1 102.0(2) . . ? C21 Os2 Os1 107.91(19) . . ? Se4 Os2 Os1 56.409(14) . . ? Os3 Os2 Os1 60.432(8) . . ? C31 Os3 C33 90.9(3) . . ? C31 Os3 C32 93.7(3) . . ? C33 Os3 C32 98.2(3) . . ? C31 Os3 Se4 102.0(3) . . ? C33 Os3 Se4 105.7(2) . . ? C32 Os3 Se4 151.0(2) . . ? C31 Os3 Os2 91.0(2) . . ? C33 Os3 Os2 162.0(2) . . ? C32 Os3 Os2 99.5(2) . . ? Se4 Os3 Os2 56.448(15) . . ? C31 Os3 Os1 150.8(2) . . ? C33 Os3 Os1 112.8(2) . . ? C32 Os3 Os1 99.2(2) . . ? Se4 Os3 Os1 56.574(14) . . ? Os2 Os3 Os1 61.228(8) . . ? Os2 Se4 Os3 66.574(16) . . ? Os2 Se4 Os1 68.465(16) . . ? Os3 Se4 Os1 67.635(16) . . ? C121 P1 C131 103.6(3) . . ? C121 P1 C111 104.6(3) . . ? C131 P1 C111 103.0(3) . . ? C121 P1 Os1 114.9(2) . . ? C131 P1 Os1 116.0(2) . . ? C111 P1 Os1 113.2(2) . . ? O11 C11 Os1 160.4(6) . . ? O12 C12 Os1 178.3(6) . . ? O13 C13 Os1 163.6(5) . . ? O21 C21 Os2 178.5(8) . . ? O22 C22 Os2 176.6(7) . . ? O23 C23 Os2 179.4(9) . . ? O31 C31 Os3 177.4(8) . . ? O32 C32 Os3 177.3(7) . . ? O33 C33 Os3 177.6(7) . . ? C116 C111 C112 120.0(6) . . ? C116 C111 P1 122.2(5) . . ? C112 C111 P1 117.8(5) . . ? C113 C112 C111 120.2(7) . . ? C112 C113 C114 120.7(8) . . ? C113 C114 C115 121.1(8) . . ? C114 C115 C116 118.8(8) . . ? C111 C116 C115 119.1(7) . . ? C126 C121 C122 118.9(6) . . ? C126 C121 P1 119.5(5) . . ? C122 C121 P1 121.4(5) . . ? C123 C122 C121 119.7(7) . . ? C124 C123 C122 120.9(7) . . ? C123 C124 C125 120.0(7) . . ? C124 C125 C126 120.1(7) . . ? C121 C126 C125 120.4(7) . . ? C136 C131 C132 118.6(6) . . ? C136 C131 P1 120.9(5) . . ? C132 C131 P1 120.4(5) . . ? C131 C132 C133 120.5(7) . . ? C134 C133 C132 119.6(7) . . ? C133 C134 C135 120.8(7) . . ? C134 C135 C136 119.9(7) . . ? C131 C136 C135 120.6(6) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.955 _refine_diff_density_min -1.839 _refine_diff_density_rms 0.205 #========END data_4a _database_code_CSD 155040 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H17 O8 Os3 P Se' _chemical_formula_weight 1137.93 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' 'Se' 'Se' -0.0929 2.2259 '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+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.6945(7) _cell_length_b 14.1174(7) _cell_length_c 15.9671(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.1240(10) _cell_angle_gamma 90.00 _cell_volume 3056.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 13.729 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 7433 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 29.24 _reflns_number_total 7433 _reflns_number_gt 6189 _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^)+(0.0402P)^2^+7.9176P] 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 7433 _refine_ls_number_parameters 358 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.025 _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 0.405549(19) 0.750142(19) 0.227205(17) 0.03836(8) Uani 1 1 d D . . Os2 Os 0.44321(2) 0.92228(2) 0.132731(19) 0.04428(9) Uani 1 1 d D . . Os3 Os 0.45332(2) 0.93628(2) 0.30901(2) 0.04887(9) Uani 1 1 d D . . Se4 Se 0.29924(5) 0.89644(6) 0.21105(5) 0.04788(18) Uani 1 1 d . . . P1 P 0.53795(13) 0.64076(13) 0.24567(11) 0.0397(4) Uani 1 1 d . . . O11 O 0.2849(6) 0.6446(6) 0.0806(5) 0.093(2) Uani 1 1 d . . . O12 O 0.3024(5) 0.6561(6) 0.3620(5) 0.087(2) Uani 1 1 d . . . O21 O 0.3777(6) 0.8462(6) -0.0461(4) 0.086(2) Uani 1 1 d . . . O22 O 0.3943(6) 1.1294(5) 0.0873(6) 0.103(3) Uani 1 1 d . . . O23 O 0.6644(5) 0.9511(6) 0.1365(6) 0.092(2) Uani 1 1 d . . . O31 O 0.3961(9) 0.9074(8) 0.4858(6) 0.132(4) Uani 1 1 d . . . O32 O 0.6768(6) 0.9554(7) 0.3566(7) 0.117(3) Uani 1 1 d . . . O33 O 0.4168(7) 1.1496(6) 0.3074(6) 0.109(3) Uani 1 1 d . . . C11 C 0.3312(6) 0.6826(7) 0.1368(6) 0.059(2) Uani 1 1 d . . . C12 C 0.3409(6) 0.6909(6) 0.3105(6) 0.058(2) Uani 1 1 d . . . C21 C 0.4004(7) 0.8762(6) 0.0195(5) 0.057(2) Uani 1 1 d . . . C22 C 0.4133(7) 1.0515(6) 0.1056(6) 0.063(2) Uani 1 1 d . . . C23 C 0.5809(7) 0.9383(6) 0.1342(6) 0.062(2) Uani 1 1 d . . . C31 C 0.4176(9) 0.9184(8) 0.4195(7) 0.078(3) Uani 1 1 d . . . C32 C 0.5912(8) 0.9492(7) 0.3387(7) 0.071(3) Uani 1 1 d . . . C33 C 0.4324(8) 1.0703(7) 0.3081(7) 0.072(3) Uani 1 1 d . . . C511 C 0.5733(5) 0.6025(5) 0.3559(5) 0.0450(16) Uani 1 1 d . . . C512 C 0.5720(7) 0.6642(6) 0.4222(5) 0.064(2) Uani 1 1 d . . . H512 H 0.5526 0.7267 0.4113 0.077 Uiso 1 1 calc R . . C513 C 0.5991(8) 0.6350(7) 0.5054(6) 0.075(3) Uani 1 1 d . . . H513 H 0.5968 0.6777 0.5494 0.090 Uiso 1 1 calc R . . C514 C 0.6291(6) 0.5440(7) 0.5230(6) 0.063(2) Uani 1 1 d . . . H514 H 0.6477 0.5250 0.5787 0.075 Uiso 1 1 calc R . . C515 C 0.6319(7) 0.4801(7) 0.4572(6) 0.065(2) Uani 1 1 d . . . H515 H 0.6519 0.4180 0.4690 0.078 Uiso 1 1 calc R . . C516 C 0.6046(7) 0.5089(6) 0.3736(5) 0.059(2) Uani 1 1 d . . . H516 H 0.6071 0.4662 0.3297 0.071 Uiso 1 1 calc R . . C521 C 0.6524(5) 0.6820(5) 0.2115(5) 0.0428(15) Uani 1 1 d . . . C522 C 0.7407(6) 0.6882(7) 0.2653(6) 0.061(2) Uani 1 1 d . . . H522 H 0.7430 0.6732 0.3223 0.074 Uiso 1 1 calc R . . C523 C 0.8262(7) 0.7167(9) 0.2346(7) 0.084(3) Uani 1 1 d . . . H523 H 0.8852 0.7206 0.2713 0.101 Uiso 1 1 calc R . . C524 C 0.8247(7) 0.7389(7) 0.1511(7) 0.070(3) Uani 1 1 d . . . H524 H 0.8825 0.7572 0.1313 0.084 Uiso 1 1 calc R . . C525 C 0.7396(7) 0.7344(7) 0.0977(6) 0.064(2) Uani 1 1 d . . . H525 H 0.7390 0.7502 0.0411 0.077 Uiso 1 1 calc R . . C526 C 0.6528(6) 0.7065(6) 0.1258(5) 0.0556(19) Uani 1 1 d . . . H526 H 0.5946 0.7040 0.0881 0.067 Uiso 1 1 calc R . . C531 C 0.5136(6) 0.5283(5) 0.1877(5) 0.0460(16) Uani 1 1 d . . . C532 C 0.4262(7) 0.4805(6) 0.1935(6) 0.065(2) Uani 1 1 d . . . H532 H 0.3799 0.5063 0.2243 0.078 Uiso 1 1 calc R . . C533 C 0.4082(9) 0.3935(7) 0.1528(7) 0.082(3) Uani 1 1 d . . . H533 H 0.3508 0.3604 0.1584 0.098 Uiso 1 1 calc R . . C534 C 0.4737(8) 0.3567(7) 0.1052(7) 0.076(3) Uani 1 1 d . . . H534 H 0.4607 0.2995 0.0770 0.091 Uiso 1 1 calc R . . C535 C 0.5592(9) 0.4051(7) 0.0993(8) 0.083(3) Uani 1 1 d . . . H535 H 0.6037 0.3803 0.0662 0.099 Uiso 1 1 calc R . . C536 C 0.5804(7) 0.4878(6) 0.1401(6) 0.062(2) Uani 1 1 d . . . H536 H 0.6400 0.5180 0.1364 0.075 Uiso 1 1 calc R . . H12 H 0.492(3) 0.8037(19) 0.162(4) 0.050 Uiso 1 1 d D . . H13 H 0.488(3) 0.8103(9) 0.312(3) 0.050 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 0.03656(14) 0.04090(16) 0.03802(14) 0.00541(10) 0.00673(10) -0.00070(10) Os2 0.04356(15) 0.04367(16) 0.04803(17) 0.01111(12) 0.01484(12) 0.00404(11) Os3 0.04988(17) 0.04829(18) 0.04965(18) -0.00456(12) 0.01124(13) -0.00141(12) Se4 0.0383(3) 0.0532(4) 0.0539(4) 0.0088(3) 0.0129(3) 0.0072(3) P1 0.0403(9) 0.0402(9) 0.0386(9) 0.0041(7) 0.0051(7) -0.0010(7) O11 0.088(5) 0.104(6) 0.077(5) -0.022(4) -0.019(4) -0.016(4) O12 0.082(5) 0.099(6) 0.089(5) 0.038(4) 0.042(4) 0.003(4) O21 0.099(5) 0.099(6) 0.058(4) -0.003(4) 0.008(4) -0.009(4) O22 0.108(6) 0.054(4) 0.158(8) 0.028(5) 0.058(6) 0.021(4) O23 0.057(4) 0.080(5) 0.146(8) 0.004(5) 0.039(4) -0.008(3) O31 0.172(10) 0.167(10) 0.067(5) -0.021(5) 0.050(6) -0.038(8) O32 0.064(5) 0.129(8) 0.153(9) -0.013(6) -0.005(5) -0.019(5) O33 0.127(7) 0.050(4) 0.152(8) -0.019(5) 0.024(6) 0.004(4) C11 0.054(5) 0.069(6) 0.054(5) -0.002(4) 0.003(4) -0.001(4) C12 0.055(5) 0.056(5) 0.064(5) 0.020(4) 0.014(4) 0.000(4) C21 0.067(5) 0.059(5) 0.046(5) 0.013(4) 0.013(4) 0.001(4) C22 0.066(5) 0.050(5) 0.078(6) 0.011(4) 0.030(5) 0.007(4) C23 0.060(5) 0.055(5) 0.075(6) 0.012(4) 0.024(4) 0.001(4) C31 0.101(8) 0.079(7) 0.056(6) -0.011(5) 0.018(5) -0.009(6) C32 0.063(6) 0.066(6) 0.082(7) -0.010(5) 0.001(5) -0.011(5) C33 0.076(6) 0.058(6) 0.083(7) -0.012(5) 0.013(5) 0.002(5) C511 0.041(3) 0.044(4) 0.049(4) 0.011(3) 0.003(3) 0.000(3) C512 0.086(6) 0.048(5) 0.052(5) 0.002(4) -0.007(4) 0.009(4) C513 0.102(8) 0.063(6) 0.053(5) -0.002(4) -0.015(5) 0.003(5) C514 0.055(5) 0.080(6) 0.050(5) 0.020(4) -0.006(4) -0.004(4) C515 0.069(5) 0.062(6) 0.062(5) 0.022(4) 0.008(4) 0.015(4) C516 0.067(5) 0.060(5) 0.051(5) 0.006(4) 0.007(4) 0.019(4) C521 0.039(3) 0.043(4) 0.048(4) -0.001(3) 0.010(3) 0.002(3) C522 0.046(4) 0.080(6) 0.056(5) -0.003(4) 0.002(4) -0.008(4) C523 0.045(5) 0.113(9) 0.091(8) 0.014(7) -0.003(5) -0.023(5) C524 0.058(5) 0.071(6) 0.088(7) 0.007(5) 0.032(5) -0.008(4) C525 0.066(6) 0.070(6) 0.063(5) 0.011(4) 0.027(4) 0.006(4) C526 0.045(4) 0.069(6) 0.055(5) 0.007(4) 0.013(3) 0.001(4) C531 0.050(4) 0.042(4) 0.047(4) 0.001(3) 0.008(3) 0.001(3) C532 0.065(5) 0.053(5) 0.083(6) -0.010(4) 0.031(5) -0.012(4) C533 0.086(7) 0.068(7) 0.094(8) -0.021(6) 0.023(6) -0.027(6) C534 0.095(7) 0.050(5) 0.083(7) -0.015(5) 0.012(6) 0.001(5) C535 0.095(8) 0.063(6) 0.097(8) -0.029(6) 0.038(6) -0.005(6) C536 0.059(5) 0.055(5) 0.077(6) -0.012(4) 0.024(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C12 1.893(8) . ? Os1 C11 1.902(9) . ? Os1 P1 2.3682(18) . ? Os1 Se4 2.5190(8) . ? Os1 Os2 2.9440(4) . ? Os1 Os3 2.9661(4) . ? Os2 C23 1.897(9) . ? Os2 C22 1.906(9) . ? Os2 C21 1.932(9) . ? Os2 Se4 2.5061(7) . ? Os2 Os3 2.8054(4) . ? Os3 C32 1.890(10) . ? Os3 C31 1.913(11) . ? Os3 C33 1.913(10) . ? Os3 Se4 2.5065(8) . ? P1 C521 1.825(7) . ? P1 C511 1.839(7) . ? P1 C531 1.845(8) . ? O11 C11 1.155(10) . ? O12 C12 1.148(10) . ? O21 C21 1.133(10) . ? O22 C22 1.159(10) . ? O23 C23 1.152(11) . ? O31 C31 1.150(13) . ? O32 C32 1.170(12) . ? O33 C33 1.140(12) . ? C511 C512 1.374(11) . ? C511 C516 1.405(11) . ? C512 C513 1.390(12) . ? C513 C514 1.365(13) . ? C514 C515 1.389(14) . ? C515 C516 1.395(12) . ? C521 C522 1.384(10) . ? C521 C526 1.413(11) . ? C522 C523 1.392(12) . ? C523 C524 1.366(15) . ? C524 C525 1.344(14) . ? C525 C526 1.385(11) . ? C531 C532 1.388(11) . ? C531 C536 1.392(11) . ? C532 C533 1.394(13) . ? C533 C534 1.358(15) . ? C534 C535 1.370(15) . ? C535 C536 1.349(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Os1 C11 93.3(4) . . ? C12 Os1 P1 92.9(3) . . ? C11 Os1 P1 94.9(3) . . ? C12 Os1 Se4 96.5(3) . . ? C11 Os1 Se4 95.4(3) . . ? P1 Os1 Se4 165.61(5) . . ? C12 Os1 Os2 149.1(3) . . ? C11 Os1 Os2 98.0(3) . . ? P1 Os1 Os2 114.56(4) . . ? Se4 Os1 Os2 53.934(18) . . ? C12 Os1 Os3 100.2(3) . . ? C11 Os1 Os3 147.1(3) . . ? P1 Os1 Os3 113.92(5) . . ? Se4 Os1 Os3 53.63(2) . . ? Os2 Os1 Os3 56.675(10) . . ? C23 Os2 C22 94.0(4) . . ? C23 Os2 C21 102.8(4) . . ? C22 Os2 C21 94.7(4) . . ? C23 Os2 Se4 149.6(3) . . ? C22 Os2 Se4 95.4(3) . . ? C21 Os2 Se4 105.2(3) . . ? C23 Os2 Os3 94.1(3) . . ? C22 Os2 Os3 98.0(3) . . ? C21 Os2 Os3 158.1(2) . . ? Se4 Os2 Os3 55.97(2) . . ? C23 Os2 Os1 109.8(3) . . ? C22 Os2 Os1 149.2(3) . . ? C21 Os2 Os1 98.6(2) . . ? Se4 Os2 Os1 54.339(19) . . ? Os3 Os2 Os1 62.060(10) . . ? C32 Os3 C31 99.1(5) . . ? C32 Os3 C33 92.8(5) . . ? C31 Os3 C33 94.6(5) . . ? C32 Os3 Se4 154.4(3) . . ? C31 Os3 Se4 104.1(4) . . ? C33 Os3 Se4 96.1(3) . . ? C32 Os3 Os2 99.5(3) . . ? C31 Os3 Os2 158.9(3) . . ? C33 Os3 Os2 94.4(3) . . ? Se4 Os3 Os2 55.961(19) . . ? C32 Os3 Os1 110.3(3) . . ? C31 Os3 Os1 102.7(3) . . ? C33 Os3 Os1 148.2(3) . . ? Se4 Os3 Os1 54.02(2) . . ? Os2 Os3 Os1 61.266(10) . . ? Os2 Se4 Os3 68.06(2) . . ? Os2 Se4 Os1 71.73(2) . . ? Os3 Se4 Os1 72.34(2) . . ? C521 P1 C511 105.0(3) . . ? C521 P1 C531 103.1(3) . . ? C511 P1 C531 103.4(3) . . ? C521 P1 Os1 115.4(2) . . ? C511 P1 Os1 113.8(3) . . ? C531 P1 Os1 114.7(2) . . ? O11 C11 Os1 177.5(9) . . ? O12 C12 Os1 178.8(10) . . ? O21 C21 Os2 177.3(9) . . ? O22 C22 Os2 178.5(10) . . ? O23 C23 Os2 177.6(9) . . ? O31 C31 Os3 179.8(12) . . ? O32 C32 Os3 178.7(10) . . ? O33 C33 Os3 177.8(10) . . ? C512 C511 C516 118.5(7) . . ? C512 C511 P1 121.4(6) . . ? C516 C511 P1 120.1(6) . . ? C511 C512 C513 121.1(8) . . ? C514 C513 C512 120.5(9) . . ? C513 C514 C515 119.7(8) . . ? C514 C515 C516 120.1(8) . . ? C515 C516 C511 120.0(8) . . ? C522 C521 C526 117.6(7) . . ? C522 C521 P1 123.1(6) . . ? C526 C521 P1 119.3(6) . . ? C521 C522 C523 120.3(8) . . ? C524 C523 C522 120.9(9) . . ? C525 C524 C523 120.0(8) . . ? C524 C525 C526 121.0(9) . . ? C525 C526 C521 120.3(8) . . ? C532 C531 C536 118.5(8) . . ? C532 C531 P1 118.8(6) . . ? C536 C531 P1 122.7(6) . . ? C531 C532 C533 119.6(9) . . ? C534 C533 C532 120.7(10) . . ? C533 C534 C535 119.0(9) . . ? C536 C535 C534 121.8(9) . . ? C535 C536 C531 120.3(9) . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 29.24 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.999 _refine_diff_density_min -2.300 _refine_diff_density_rms 0.314 #======END data_5a _database_code_CSD 155041 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H34 O18 Os6 P2 Se' _chemical_formula_weight 2252.91 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' 'Se' 'Se' -0.0929 2.2259 '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 14.049(2) _cell_length_b 14.093(2) _cell_length_c 19.876(3) _cell_angle_alpha 69.815(13) _cell_angle_beta 80.778(11) _cell_angle_gamma 72.182(13) _cell_volume 3509.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 11.440 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.012269 _exptl_absorpt_correction_T_max 0.098735 _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 25625 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.1172 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 29.63 _reflns_number_total 16474 _reflns_number_gt 8784 _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^)+(0.0833P)^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 16474 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1850 _refine_ls_wR_factor_gt 0.1598 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os -0.08251(5) 0.84784(4) -0.29552(3) 0.04200(16) Uani 1 1 d . . . H1 H -0.1108 0.8274 -0.3702 0.050 Uiso 1 1 d R . . Os2 Os -0.00393(5) 0.72287(5) -0.14329(3) 0.04355(16) Uani 1 1 d . . . H12 H -0.0835 0.8521 -0.2006 0.050 Uiso 1 1 d R . . Os3 Os 0.01553(5) 0.60689(5) -0.24634(3) 0.04785(17) Uani 1 1 d . . . H13 H -0.0737 0.7189 -0.3104 0.050 Uiso 1 1 d R . . Os4 Os -0.38558(5) 0.92586(5) -0.35883(3) 0.05275(19) Uani 1 1 d . . . H45 H -0.4025 1.0364 -0.3190 0.050 Uiso 1 1 d R . . Os5 Os -0.40512(5) 0.95277(5) -0.22086(3) 0.05222(18) Uani 1 1 d . . . Os6 Os -0.52881(5) 0.84713(6) -0.25149(4) 0.0664(2) Uani 1 1 d . . . Se7 Se -0.26009(11) 0.81751(12) -0.26210(8) 0.0450(4) Uani 1 1 d . . . P8 P -0.0098(3) 0.8342(3) -0.0758(2) 0.0488(10) Uani 1 1 d . . . P9 P 0.0094(3) 0.5557(3) -0.3474(2) 0.0515(10) Uani 1 1 d . . . O11 O -0.1670(9) 1.0829(8) -0.3402(6) 0.069(3) Uani 1 1 d . . . O12 O 0.1153(10) 0.8871(11) -0.3641(8) 0.093(5) Uani 1 1 d . . . O21 O -0.2106(9) 0.6864(10) -0.0835(7) 0.069(4) Uani 1 1 d . . . O22 O 0.1015(10) 0.5185(10) -0.0336(7) 0.091(5) Uani 1 1 d . . . O23 O 0.1951(10) 0.7711(11) -0.2118(7) 0.079(4) Uani 1 1 d . . . O31 O -0.1696(12) 0.5432(10) -0.1618(7) 0.083(4) Uani 1 1 d . . . O32 O 0.1292(14) 0.3987(11) -0.1466(8) 0.113(6) Uani 1 1 d . . . O33 O 0.2214(10) 0.6460(12) -0.3091(9) 0.091(5) Uani 1 1 d . . . O41 O -0.2386(13) 1.0267(13) -0.4710(7) 0.104(6) Uani 1 1 d . . . O42 O -0.5578(12) 1.0730(14) -0.4528(8) 0.125(7) Uani 1 1 d . . . O43 O -0.3578(11) 0.7442(11) -0.4130(8) 0.094(5) Uani 1 1 d . . . O51 O -0.2740(12) 1.0772(13) -0.1992(8) 0.098(5) Uani 1 1 d . . . O52 O -0.5937(11) 1.1194(12) -0.1972(8) 0.103(6) Uani 1 1 d . . . O53 O -0.4241(12) 0.8174(14) -0.0648(7) 0.113(6) Uani 1 1 d . . . O61 O -0.3769(13) 0.6274(12) -0.1961(12) 0.127(7) Uani 1 1 d . . . O62 O -0.6215(16) 0.761(2) -0.3393(15) 0.191(12) Uani 1 1 d . . . O63 O -0.6749(12) 1.0597(13) -0.3138(9) 0.109(6) Uani 1 1 d . . . O64 O -0.6454(11) 0.7966(14) -0.1060(9) 0.113(6) Uani 1 1 d . . . C11 C -0.1362(12) 0.9932(13) -0.3211(8) 0.050(4) Uani 1 1 d . . . C12 C 0.0419(14) 0.8694(14) -0.3357(9) 0.061(5) Uani 1 1 d . . . C21 C -0.1346(15) 0.7000(12) -0.1061(7) 0.057(5) Uani 1 1 d . . . C22 C 0.0637(13) 0.5929(13) -0.0763(10) 0.067(5) Uani 1 1 d . . . C23 C 0.1224(15) 0.7532(14) -0.1874(8) 0.059(5) Uani 1 1 d . . . C31 C -0.1026(13) 0.5735(12) -0.1970(9) 0.053(4) Uani 1 1 d . . . C32 C 0.0833(17) 0.4777(14) -0.1831(10) 0.084(7) Uani 1 1 d . . . C33 C 0.1472(16) 0.6355(13) -0.2881(9) 0.063(5) Uani 1 1 d . . . C41 C -0.2881(16) 0.9915(17) -0.4292(11) 0.079(6) Uani 1 1 d . . . C42 C -0.4922(14) 1.0181(16) -0.4165(9) 0.071(6) Uani 1 1 d . . . C43 C -0.3665(15) 0.8138(15) -0.3961(11) 0.075(6) Uani 1 1 d . . . C51 C -0.3209(14) 1.0309(17) -0.2090(10) 0.072(5) Uani 1 1 d . . . C52 C -0.5274(15) 1.0599(17) -0.2078(10) 0.074(5) Uani 1 1 d . . . C53 C -0.4166(14) 0.8700(15) -0.1252(12) 0.075(6) Uani 1 1 d . . . C61 C -0.4303(19) 0.710(2) -0.2178(13) 0.097(8) Uani 1 1 d . . . C62 C -0.5859(15) 0.792(2) -0.3068(14) 0.098(8) Uani 1 1 d . . . C63 C -0.6181(15) 0.9840(17) -0.2894(10) 0.073(5) Uani 1 1 d . . . C64 C -0.6057(16) 0.814(2) -0.1587(13) 0.095(7) Uani 1 1 d . . . C811 C 0.0366(12) 0.9476(12) -0.1307(8) 0.047(4) Uani 1 1 d . . . C812 C -0.0023(15) 1.0075(13) -0.1909(9) 0.064(5) Uani 1 1 d . . . H812 H -0.0569 0.9953 -0.2043 0.076 Uiso 1 1 calc R . . C813 C 0.0340(19) 1.0865(15) -0.2343(11) 0.085(6) Uani 1 1 d . . . H813 H 0.0037 1.1291 -0.2768 0.102 Uiso 1 1 calc R . . C814 C 0.1160(15) 1.1054(16) -0.2167(12) 0.075(6) Uani 1 1 d . . . H814 H 0.1427 1.1582 -0.2485 0.090 Uiso 1 1 calc R . . C815 C 0.1579(16) 1.0470(15) -0.1531(12) 0.076(6) Uani 1 1 d . . . H815 H 0.2107 1.0599 -0.1380 0.091 Uiso 1 1 calc R . . C816 C 0.1169(13) 0.9695(14) -0.1139(9) 0.061(4) Uani 1 1 d . . . H816 H 0.1457 0.9260 -0.0710 0.073 Uiso 1 1 calc R . . C821 C -0.1370(13) 0.8922(13) -0.0384(8) 0.053(4) Uani 1 1 d . . . C822 C -0.1901(15) 0.8276(16) 0.0066(9) 0.067(5) Uani 1 1 d . . . H822 H -0.1648 0.7552 0.0175 0.081 Uiso 1 1 calc R . . C823 C -0.2812(17) 0.870(2) 0.0357(11) 0.082(6) Uani 1 1 d . . . H823 H -0.3164 0.8257 0.0691 0.099 Uiso 1 1 calc R . . C824 C -0.3185(16) 0.971(2) 0.0169(12) 0.091(7) Uani 1 1 d . . . H824 H -0.3828 0.9982 0.0344 0.109 Uiso 1 1 calc R . . C825 C -0.2679(15) 1.0352(19) -0.0263(11) 0.084(6) Uani 1 1 d . . . H825 H -0.2963 1.1073 -0.0382 0.101 Uiso 1 1 calc R . . C826 C -0.1755(13) 0.9977(15) -0.0533(9) 0.064(5) Uani 1 1 d . . . H826 H -0.1384 1.0433 -0.0818 0.077 Uiso 1 1 calc R . . C831 C 0.0669(12) 0.7716(12) 0.0014(8) 0.048(4) Uani 1 1 d . . . C832 C 0.0331(14) 0.7830(14) 0.0673(9) 0.063(5) Uani 1 1 d . . . H832 H -0.0326 0.8208 0.0743 0.076 Uiso 1 1 calc R . . C833 C 0.0981(18) 0.7373(15) 0.1258(10) 0.084(6) Uani 1 1 d . . . H833 H 0.0749 0.7465 0.1702 0.100 Uiso 1 1 calc R . . C834 C 0.1961(17) 0.6789(15) 0.1156(10) 0.075(6) Uani 1 1 d . . . H834 H 0.2384 0.6475 0.1533 0.090 Uiso 1 1 calc R . . C835 C 0.2283(15) 0.6689(15) 0.0502(10) 0.074(6) Uani 1 1 d . . . H835 H 0.2939 0.6310 0.0431 0.089 Uiso 1 1 calc R . . C836 C 0.1669(14) 0.7132(14) -0.0064(9) 0.067(5) Uani 1 1 d . . . H836 H 0.1920 0.7044 -0.0507 0.080 Uiso 1 1 calc R . . C911 C 0.1254(7) 0.4691(9) -0.3742(6) 0.062(5) Uani 1 1 d G . . C912 C 0.1809(10) 0.3861(10) -0.3215(6) 0.083(6) Uani 1 1 d G . . H912 H 0.1585 0.3740 -0.2734 0.100 Uiso 1 1 calc R . . C913 C 0.2699(10) 0.3212(9) -0.3406(8) 0.121(10) Uani 1 1 d G . . H913 H 0.3071 0.2657 -0.3054 0.145 Uiso 1 1 calc R . . C914 C 0.3034(8) 0.3393(11) -0.4125(10) 0.104(8) Uani 1 1 d G . . H914 H 0.3629 0.2959 -0.4253 0.124 Uiso 1 1 calc R . . C915 C 0.2478(11) 0.4223(12) -0.4652(7) 0.110(9) Uani 1 1 d G . . H915 H 0.2702 0.4344 -0.5133 0.131 Uiso 1 1 calc R . . C916 C 0.1588(10) 0.4872(9) -0.4460(6) 0.076(6) Uani 1 1 d G . . H916 H 0.1217 0.5427 -0.4813 0.091 Uiso 1 1 calc R . . C921 C -0.0808(8) 0.4855(8) -0.3404(6) 0.052(4) Uani 1 1 d G . . C922 C -0.1787(9) 0.5271(8) -0.3177(6) 0.064(5) Uani 1 1 d G . . H922 H -0.1951 0.5878 -0.3047 0.076 Uiso 1 1 calc R . . C923 C -0.2522(7) 0.4781(10) -0.3145(7) 0.082(6) Uani 1 1 d G . . H923 H -0.3178 0.5060 -0.2993 0.099 Uiso 1 1 calc R . . C924 C -0.2277(10) 0.3873(10) -0.3339(7) 0.087(7) Uani 1 1 d G . . H924 H -0.2769 0.3545 -0.3318 0.105 Uiso 1 1 calc R . . C925 C -0.1297(11) 0.3457(8) -0.3566(7) 0.094(7) Uani 1 1 d G . . H925 H -0.1133 0.2850 -0.3696 0.113 Uiso 1 1 calc R . . C926 C -0.0563(8) 0.3947(8) -0.3599(6) 0.065(5) Uani 1 1 d G . . H926 H 0.0093 0.3668 -0.3750 0.078 Uiso 1 1 calc R . . C931 C -0.0195(9) 0.6669(7) -0.4281(5) 0.057(4) Uani 1 1 d G . . C932 C 0.0432(8) 0.7330(10) -0.4528(6) 0.074(6) Uani 1 1 d G . . H932 H 0.1018 0.7168 -0.4300 0.089 Uiso 1 1 calc R . . C933 C 0.0185(11) 0.8233(9) -0.5113(7) 0.087(7) Uani 1 1 d G . . H933 H 0.0604 0.8675 -0.5278 0.104 Uiso 1 1 calc R . . C934 C -0.0690(12) 0.8476(8) -0.5453(6) 0.108(9) Uani 1 1 d G . . H934 H -0.0856 0.9080 -0.5844 0.129 Uiso 1 1 calc R . . C935 C -0.1317(9) 0.7815(11) -0.5207(7) 0.088(7) Uani 1 1 d G . . H935 H -0.1903 0.7977 -0.5434 0.106 Uiso 1 1 calc R . . C936 C -0.1070(9) 0.6912(10) -0.4621(7) 0.081(6) Uani 1 1 d G . . H936 H -0.1490 0.6470 -0.4456 0.098 Uiso 1 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 0.0470(4) 0.0388(3) 0.0387(3) -0.0089(2) -0.0028(3) -0.0132(3) Os2 0.0464(4) 0.0447(3) 0.0404(3) -0.0096(3) -0.0071(3) -0.0155(3) Os3 0.0550(4) 0.0401(3) 0.0495(3) -0.0130(3) -0.0087(3) -0.0127(3) Os4 0.0547(4) 0.0605(4) 0.0405(3) -0.0177(3) -0.0129(3) -0.0049(3) Os5 0.0491(4) 0.0655(4) 0.0410(3) -0.0193(3) -0.0053(3) -0.0097(3) Os6 0.0469(4) 0.0827(5) 0.0753(5) -0.0314(4) -0.0029(4) -0.0187(4) Se7 0.0442(9) 0.0497(9) 0.0391(7) -0.0096(7) -0.0063(6) -0.0129(7) P8 0.056(3) 0.053(2) 0.042(2) -0.0143(19) -0.0081(19) -0.0181(19) P9 0.061(3) 0.041(2) 0.052(2) -0.0156(19) -0.006(2) -0.0112(19) O11 0.082(9) 0.037(7) 0.066(8) -0.001(6) 0.001(6) -0.006(6) O12 0.061(9) 0.081(9) 0.112(12) 0.002(8) 0.019(8) -0.032(7) O21 0.050(7) 0.090(9) 0.071(8) -0.024(7) 0.013(6) -0.035(7) O22 0.081(10) 0.078(10) 0.085(10) 0.021(8) -0.030(8) -0.021(8) O23 0.060(9) 0.121(12) 0.067(8) -0.025(8) 0.000(7) -0.046(8) O31 0.117(12) 0.069(9) 0.066(8) -0.018(7) 0.007(8) -0.040(8) O32 0.170(17) 0.068(10) 0.087(11) -0.012(9) -0.048(11) -0.007(10) O33 0.037(8) 0.109(11) 0.137(14) -0.051(10) 0.008(8) -0.026(8) O41 0.115(13) 0.112(12) 0.053(8) 0.002(8) 0.026(9) -0.033(10) O42 0.111(12) 0.154(15) 0.076(10) -0.051(10) -0.056(9) 0.053(11) O43 0.106(12) 0.092(11) 0.105(11) -0.062(10) -0.029(9) -0.008(9) O51 0.103(12) 0.138(14) 0.091(11) -0.058(10) -0.003(9) -0.062(11) O52 0.079(11) 0.116(12) 0.087(10) -0.052(9) 0.006(8) 0.029(9) O53 0.103(12) 0.161(16) 0.041(7) 0.002(9) -0.023(8) -0.016(11) O61 0.092(12) 0.063(10) 0.19(2) -0.010(12) 0.010(12) -0.022(9) O62 0.115(17) 0.30(3) 0.28(3) -0.23(3) 0.021(17) -0.086(18) O63 0.090(12) 0.099(12) 0.106(12) -0.019(10) -0.033(9) 0.014(9) O64 0.069(10) 0.157(16) 0.090(11) -0.027(11) 0.027(9) -0.028(10) C11 0.049(10) 0.051(10) 0.045(8) -0.014(7) 0.002(7) -0.012(7) C12 0.061(12) 0.067(12) 0.054(10) -0.017(9) -0.001(9) -0.018(9) C21 0.093(14) 0.046(9) 0.020(6) 0.003(6) -0.022(8) -0.008(9) C22 0.056(11) 0.049(10) 0.070(12) 0.006(9) -0.011(9) -0.004(8) C23 0.070(13) 0.070(12) 0.035(8) -0.008(8) -0.010(8) -0.022(10) C31 0.064(12) 0.052(10) 0.049(9) -0.009(8) -0.014(8) -0.026(8) C32 0.123(18) 0.042(10) 0.064(12) 0.011(9) -0.039(12) -0.004(10) C33 0.084(15) 0.053(11) 0.055(10) -0.022(9) -0.026(10) -0.006(10) C41 0.068(14) 0.091(15) 0.065(13) -0.023(12) -0.019(11) 0.003(11) C42 0.062(12) 0.106(15) 0.048(9) -0.050(10) -0.015(9) 0.008(10) C43 0.079(14) 0.074(13) 0.093(14) -0.051(12) -0.041(11) -0.003(10) C51 0.054(12) 0.096(15) 0.073(13) -0.045(12) 0.004(9) -0.013(10) C52 0.064(13) 0.099(16) 0.062(12) -0.029(11) -0.010(10) -0.021(11) C53 0.061(12) 0.066(12) 0.096(16) -0.032(12) -0.031(11) 0.007(9) C61 0.100(19) 0.103(19) 0.092(16) 0.005(14) 0.003(14) -0.079(16) C62 0.048(13) 0.15(2) 0.13(2) -0.087(18) 0.022(13) -0.048(13) C63 0.059(12) 0.083(14) 0.067(12) -0.013(11) -0.011(10) -0.016(11) C64 0.052(13) 0.16(2) 0.086(16) -0.045(16) 0.011(12) -0.044(14) C811 0.059(10) 0.050(9) 0.043(8) -0.024(7) 0.004(7) -0.023(8) C812 0.096(15) 0.049(10) 0.049(9) -0.012(8) -0.009(9) -0.026(10) C813 0.12(2) 0.062(13) 0.066(13) -0.019(11) -0.020(13) -0.016(12) C814 0.065(13) 0.076(14) 0.089(15) -0.036(12) 0.025(11) -0.028(11) C815 0.076(14) 0.073(13) 0.090(15) -0.030(12) 0.005(12) -0.036(11) C816 0.063(12) 0.070(12) 0.060(10) -0.026(9) 0.005(9) -0.032(9) C821 0.061(11) 0.057(10) 0.045(9) -0.020(8) 0.000(8) -0.017(8) C822 0.078(14) 0.081(13) 0.058(11) -0.036(10) 0.007(10) -0.033(11) C823 0.087(17) 0.112(19) 0.063(12) -0.041(13) 0.018(11) -0.044(14) C824 0.053(13) 0.15(2) 0.080(15) -0.061(17) 0.006(11) -0.020(15) C825 0.065(14) 0.114(18) 0.075(14) -0.048(13) 0.017(11) -0.017(13) C826 0.052(11) 0.075(13) 0.061(11) -0.023(10) -0.004(8) -0.011(9) C831 0.056(10) 0.053(9) 0.039(8) -0.004(7) -0.010(7) -0.027(8) C832 0.070(12) 0.077(12) 0.051(10) -0.018(9) -0.025(9) -0.025(10) C833 0.13(2) 0.073(14) 0.051(11) -0.018(10) -0.016(12) -0.020(13) C834 0.103(17) 0.068(13) 0.056(11) -0.011(10) -0.027(11) -0.025(12) C835 0.073(13) 0.088(14) 0.074(13) -0.036(11) -0.030(10) -0.012(10) C836 0.078(14) 0.077(13) 0.053(10) -0.024(9) -0.001(9) -0.030(10) C911 0.050(10) 0.055(11) 0.088(13) -0.040(10) 0.002(9) -0.009(8) C912 0.075(14) 0.072(13) 0.085(14) -0.024(12) -0.010(11) 0.006(11) C913 0.12(2) 0.078(16) 0.16(3) -0.059(17) -0.071(19) 0.038(14) C914 0.074(16) 0.110(19) 0.13(2) -0.081(19) -0.005(15) 0.013(13) C915 0.093(18) 0.107(19) 0.14(2) -0.085(18) 0.023(16) -0.002(14) C916 0.075(14) 0.092(15) 0.065(12) -0.048(11) -0.007(10) -0.001(11) C921 0.057(11) 0.044(9) 0.052(9) -0.010(7) -0.014(8) -0.012(7) C922 0.065(12) 0.079(13) 0.063(11) -0.019(9) 0.005(9) -0.050(10) C923 0.092(16) 0.083(15) 0.066(12) -0.019(11) -0.013(11) -0.019(12) C924 0.105(19) 0.086(15) 0.103(17) -0.039(13) -0.023(14) -0.053(14) C925 0.13(2) 0.068(14) 0.092(16) -0.031(12) -0.032(15) -0.015(14) C926 0.081(13) 0.044(10) 0.086(13) -0.019(9) -0.019(10) -0.035(9) C931 0.079(13) 0.047(10) 0.045(9) -0.015(7) 0.006(8) -0.021(9) C932 0.109(17) 0.058(12) 0.060(11) -0.021(10) 0.006(11) -0.032(11) C933 0.14(2) 0.079(15) 0.064(12) -0.032(11) 0.010(13) -0.063(14) C934 0.15(3) 0.089(18) 0.065(14) -0.029(13) -0.008(15) 0.001(17) C935 0.091(16) 0.086(15) 0.078(14) 0.000(12) -0.020(12) -0.033(13) C936 0.111(18) 0.062(12) 0.061(12) -0.005(10) -0.028(12) -0.014(11) _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 1.866(16) . ? Os1 C12 1.869(19) . ? Os1 Se7 2.6026(17) . ? Os1 Os3 3.1084(10) . ? Os1 Os2 3.1111(10) . ? Os2 C22 1.921(16) . ? Os2 C21 1.95(2) . ? Os2 C23 1.95(2) . ? Os2 P8 2.366(4) . ? Os2 Os3 2.9663(9) . ? Os3 C32 1.883(17) . ? Os3 C31 1.891(18) . ? Os3 C33 2.00(2) . ? Os3 P9 2.378(4) . ? Os4 C42 1.892(17) . ? Os4 C43 1.896(18) . ? Os4 C41 1.99(2) . ? Os4 Se7 2.5591(16) . ? Os4 Os5 2.8552(9) . ? Os4 Os6 2.8616(11) . ? Os5 C53 1.87(2) . ? Os5 C51 1.93(2) . ? Os5 C52 1.96(2) . ? Os5 Se7 2.5735(17) . ? Os5 Os6 2.8557(11) . ? Os6 C63 1.92(2) . ? Os6 C62 1.92(2) . ? Os6 C64 1.97(2) . ? Os6 C61 1.97(3) . ? P8 C831 1.820(15) . ? P8 C811 1.838(16) . ? P8 C821 1.874(17) . ? P9 C921 1.795(9) . ? P9 C931 1.812(9) . ? P9 C911 1.838(9) . ? O11 C11 1.148(17) . ? O12 C12 1.148(19) . ? O21 C21 1.14(2) . ? O22 C22 1.136(18) . ? O23 C23 1.12(2) . ? O31 C31 1.178(19) . ? O32 C32 1.155(19) . ? O33 C33 1.09(2) . ? O41 C41 1.08(2) . ? O42 C42 1.165(19) . ? O43 C43 1.111(19) . ? O51 C51 1.14(2) . ? O52 C52 1.09(2) . ? O53 C53 1.18(2) . ? O61 C61 1.15(3) . ? O62 C62 1.14(3) . ? O63 C63 1.12(2) . ? O64 C64 1.09(2) . ? C811 C812 1.29(2) . ? C811 C816 1.37(2) . ? C812 C813 1.34(3) . ? C813 C814 1.38(3) . ? C814 C815 1.36(3) . ? C815 C816 1.34(2) . ? C821 C822 1.35(2) . ? C821 C826 1.36(2) . ? C822 C823 1.36(3) . ? C823 C824 1.30(3) . ? C824 C825 1.32(3) . ? C825 C826 1.34(2) . ? C831 C832 1.36(2) . ? C831 C836 1.41(2) . ? C832 C833 1.44(2) . ? C833 C834 1.39(3) . ? C834 C835 1.35(2) . ? C835 C836 1.38(2) . ? C911 C912 1.3900 . ? C911 C916 1.3900 . ? C912 C913 1.3900 . ? C913 C914 1.3900 . ? C914 C915 1.3900 . ? C915 C916 1.3900 . ? C921 C922 1.3900 . ? C921 C926 1.3900 . ? C922 C923 1.3900 . ? C923 C924 1.3900 . ? C924 C925 1.3900 . ? C925 C926 1.3900 . ? C931 C932 1.3900 . ? C931 C936 1.3900 . ? C932 C933 1.3900 . ? C933 C934 1.3900 . ? C934 C935 1.3900 . ? C935 C936 1.3900 . ? 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 88.8(7) . . ? C11 Os1 Se7 91.5(5) . . ? C12 Os1 Se7 169.8(5) . . ? C11 Os1 Os3 176.3(5) . . ? C12 Os1 Os3 89.6(5) . . ? Se7 Os1 Os3 90.64(4) . . ? C11 Os1 Os2 119.8(5) . . ? C12 Os1 Os2 93.5(5) . . ? Se7 Os1 Os2 95.20(4) . . ? Os3 Os1 Os2 56.97(2) . . ? C22 Os2 C21 92.0(7) . . ? C22 Os2 C23 92.1(7) . . ? C21 Os2 C23 175.6(6) . . ? C22 Os2 P8 97.6(6) . . ? C21 Os2 P8 94.8(5) . . ? C23 Os2 P8 86.2(5) . . ? C22 Os2 Os3 88.1(6) . . ? C21 Os2 Os3 91.5(5) . . ? C23 Os2 Os3 87.0(5) . . ? P8 Os2 Os3 171.27(10) . . ? C22 Os2 Os1 149.5(6) . . ? C21 Os2 Os1 91.1(4) . . ? C23 Os2 Os1 84.6(4) . . ? P8 Os2 Os1 112.33(10) . . ? Os3 Os2 Os1 61.47(2) . . ? C32 Os3 C31 85.3(9) . . ? C32 Os3 C33 89.8(9) . . ? C31 Os3 C33 173.7(7) . . ? C32 Os3 P9 100.7(6) . . ? C31 Os3 P9 96.5(5) . . ? C33 Os3 P9 88.3(5) . . ? C32 Os3 Os2 93.6(6) . . ? C31 Os3 Os2 84.5(5) . . ? C33 Os3 Os2 91.9(5) . . ? P9 Os3 Os2 165.69(10) . . ? C32 Os3 Os1 155.0(6) . . ? C31 Os3 Os1 94.3(5) . . ? C33 Os3 Os1 88.4(5) . . ? P9 Os3 Os1 104.15(10) . . ? Os2 Os3 Os1 61.56(2) . . ? C42 Os4 C43 95.7(7) . . ? C42 Os4 C41 90.5(8) . . ? C43 Os4 C41 95.2(9) . . ? C42 Os4 Se7 168.7(4) . . ? C43 Os4 Se7 93.6(5) . . ? C41 Os4 Se7 95.1(5) . . ? C42 Os4 Os5 112.3(4) . . ? C43 Os4 Os5 137.3(6) . . ? C41 Os4 Os5 115.2(6) . . ? Se7 Os4 Os5 56.44(4) . . ? C42 Os4 Os6 89.1(6) . . ? C43 Os4 Os6 90.4(7) . . ? C41 Os4 Os6 174.4(6) . . ? Se7 Os4 Os6 84.41(4) . . ? Os5 Os4 Os6 59.94(3) . . ? C53 Os5 C51 98.3(8) . . ? C53 Os5 C52 91.5(8) . . ? C51 Os5 C52 92.1(8) . . ? C53 Os5 Se7 96.9(5) . . ? C51 Os5 Se7 95.0(5) . . ? C52 Os5 Se7 168.2(5) . . ? C53 Os5 Os4 136.8(6) . . ? C51 Os5 Os4 115.4(6) . . ? C52 Os5 Os4 112.3(5) . . ? Se7 Os5 Os4 55.96(4) . . ? C53 Os5 Os6 86.7(6) . . ? C51 Os5 Os6 175.0(6) . . ? C52 Os5 Os6 87.9(6) . . ? Se7 Os5 Os6 84.28(5) . . ? Os4 Os5 Os6 60.14(3) . . ? C63 Os6 C62 90.6(10) . . ? C63 Os6 C64 94.3(9) . . ? C62 Os6 C64 102.2(9) . . ? C63 Os6 C61 176.1(8) . . ? C62 Os6 C61 89.7(11) . . ? C64 Os6 C61 89.4(10) . . ? C63 Os6 Os5 86.1(6) . . ? C62 Os6 Os5 158.3(7) . . ? C64 Os6 Os5 99.5(7) . . ? C61 Os6 Os5 92.2(6) . . ? C63 Os6 Os4 85.2(6) . . ? C62 Os6 Os4 98.4(7) . . ? C64 Os6 Os4 159.4(7) . . ? C61 Os6 Os4 91.0(6) . . ? Os5 Os6 Os4 59.92(3) . . ? Os4 Se7 Os5 67.60(4) . . ? Os4 Se7 Os1 114.36(6) . . ? Os5 Se7 Os1 120.46(6) . . ? C831 P8 C811 105.2(7) . . ? C831 P8 C821 104.5(7) . . ? C811 P8 C821 104.9(7) . . ? C831 P8 Os2 114.1(5) . . ? C811 P8 Os2 111.1(5) . . ? C821 P8 Os2 115.9(5) . . ? C921 P9 C931 104.3(6) . . ? C921 P9 C911 101.9(6) . . ? C931 P9 C911 103.6(6) . . ? C921 P9 Os3 116.5(4) . . ? C931 P9 Os3 112.4(4) . . ? C911 P9 Os3 116.4(4) . . ? O11 C11 Os1 176.6(14) . . ? O12 C12 Os1 175.7(17) . . ? O21 C21 Os2 179.1(13) . . ? O22 C22 Os2 176.0(19) . . ? O23 C23 Os2 178.9(16) . . ? O31 C31 Os3 172.9(15) . . ? O32 C32 Os3 177(2) . . ? O33 C33 Os3 176.4(17) . . ? O41 C41 Os4 175(2) . . ? O42 C42 Os4 178.3(18) . . ? O43 C43 Os4 175(2) . . ? O51 C51 Os5 176.8(17) . . ? O52 C52 Os5 176.1(17) . . ? O53 C53 Os5 180(2) . . ? O61 C61 Os6 176.5(19) . . ? O62 C62 Os6 179(2) . . ? O63 C63 Os6 174(2) . . ? O64 C64 Os6 177(2) . . ? C812 C811 C816 116.5(16) . . ? C812 C811 P8 120.1(14) . . ? C816 C811 P8 123.3(13) . . ? C811 C812 C813 122(2) . . ? C812 C813 C814 121(2) . . ? C815 C814 C813 120.2(19) . . ? C816 C815 C814 114(2) . . ? C815 C816 C811 126.5(19) . . ? C822 C821 C826 119.1(17) . . ? C822 C821 P8 119.3(14) . . ? C826 C821 P8 121.5(13) . . ? C821 C822 C823 119(2) . . ? C824 C823 C822 120(2) . . ? C823 C824 C825 122(2) . . ? C824 C825 C826 120(2) . . ? C825 C826 C821 119(2) . . ? C832 C831 C836 117.5(15) . . ? C832 C831 P8 122.5(13) . . ? C836 C831 P8 119.9(12) . . ? C831 C832 C833 120.7(18) . . ? C834 C833 C832 119.7(18) . . ? C835 C834 C833 118.9(18) . . ? C834 C835 C836 122(2) . . ? C835 C836 C831 121.3(17) . . ? C912 C911 C916 120.0 . . ? C912 C911 P9 119.2(7) . . ? C916 C911 P9 120.8(7) . . ? C913 C912 C911 120.0 . . ? C914 C913 C912 120.0 . . ? C913 C914 C915 120.0 . . ? C916 C915 C914 120.0 . . ? C915 C916 C911 120.0 . . ? C922 C921 C926 120.0 . . ? C922 C921 P9 117.9(7) . . ? C926 C921 P9 122.1(7) . . ? C921 C922 C923 120.0 . . ? C924 C923 C922 120.0 . . ? C923 C924 C925 120.0 . . ? C926 C925 C924 120.0 . . ? C925 C926 C921 120.0 . . ? C932 C931 C936 120.0 . . ? C932 C931 P9 118.9(7) . . ? C936 C931 P9 120.9(7) . . ? C933 C932 C931 120.0 . . ? C932 C933 C934 120.0 . . ? C935 C934 C933 120.0 . . ? C934 C935 C936 120.0 . . ? C935 C936 C931 120.0 . . ? _diffrn_measured_fraction_theta_max 0.832 _diffrn_reflns_theta_full 29.63 _diffrn_measured_fraction_theta_full 0.832 _refine_diff_density_max 2.325 _refine_diff_density_min -2.394 _refine_diff_density_rms 0.305 #=====END