# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1874 # Data for 3, 5TET and 5TRI are not available as CIF. Hard copy data has # been deposited at the CCDC for these structures #==================================================================== data_global #==================================================================== # 1. SUBMISSION DETAILS _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 1 #========================================================================= data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H10 O10 Os3 Te2' _chemical_formula_weight 1260.10 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' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.96770(10) _cell_length_b 16.86120(10) _cell_length_c 10.86860(10) _cell_angle_alpha 90.00 _cell_angle_beta 111.07 _cell_angle_gamma 90.00 _cell_volume 1362.49(2) _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 'PLATE' _exptl_crystal_colour 'YELLOW' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 16.103 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.052139 _exptl_absorpt_correction_T_max 0.121561 _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 17638 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 29.32 _reflns_number_total 5992 _reflns_number_gt 5778 _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^)+(0.0757P)^2^+1.2949P] 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 0.0038(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(9) _refine_ls_number_reflns 5992 _refine_ls_number_parameters 335 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.005 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 1.28196(6) 0.49122(3) 1.50067(5) 0.03292(13) Uani 1 1 d . . . Os2 Os 1.00179(6) 0.36362(2) 1.41561(4) 0.03009(12) Uani 1 1 d . . . Os3 Os 0.82693(6) 0.44720(3) 1.17159(5) 0.03420(13) Uani 1 1 d . . . Te4 Te 1.14790(11) 0.52469(5) 1.23844(8) 0.03460(18) Uani 1 1 d . . . Te5 Te 1.05271(11) 0.32542(5) 1.19054(9) 0.03808(19) Uani 1 1 d . . . O11 O 1.3638(18) 0.4242(8) 1.7773(10) 0.062(3) Uani 1 1 d . . . O12 O 0.9907(16) 0.6106(7) 1.5147(12) 0.053(3) Uani 1 1 d . . . O13 O 1.5840(18) 0.6128(9) 1.5808(16) 0.072(4) Uani 1 1 d . . . O14 O 1.4988(14) 0.3595(9) 1.4296(15) 0.071(4) Uani 1 1 d . . . O21 O 0.7099(15) 0.2372(6) 1.3536(13) 0.052(3) Uani 1 1 d . . . O22 O 0.8446(14) 0.4541(6) 1.5883(11) 0.048(2) Uani 1 1 d . . . O23 O 1.2751(19) 0.2568(8) 1.6172(14) 0.066(3) Uani 1 1 d . . . O31 O 0.7234(19) 0.5052(12) 0.8859(13) 0.084(5) Uani 1 1 d . . . O32 O 0.6578(16) 0.5655(8) 1.3032(13) 0.061(3) Uani 1 1 d . . . O33 O 0.4823(15) 0.3537(9) 1.1125(15) 0.070(4) Uani 1 1 d . . . C11 C 1.3337(18) 0.4488(10) 1.6756(14) 0.045(3) Uani 1 1 d . . . C12 C 1.0955(17) 0.5661(7) 1.5115(12) 0.037(3) Uani 1 1 d . . . C13 C 1.4735(17) 0.5698(9) 1.5471(13) 0.039(3) Uani 1 1 d . . . C14 C 1.4168(18) 0.4081(10) 1.4554(15) 0.045(3) Uani 1 1 d . . . C21 C 0.8161(17) 0.2863(8) 1.3720(13) 0.037(2) Uani 1 1 d . . . C22 C 0.9073(16) 0.4208(7) 1.5252(12) 0.035(3) Uani 1 1 d . . . C23 C 1.1706(19) 0.2960(7) 1.5401(15) 0.041(3) Uani 1 1 d . . . C31 C 0.7651(17) 0.4847(11) 0.9946(13) 0.048(3) Uani 1 1 d . . . C32 C 0.727(2) 0.5231(9) 1.2586(16) 0.048(3) Uani 1 1 d . . . C33 C 0.616(2) 0.3870(9) 1.1345(16) 0.047(3) Uani 1 1 d . . . C41 C 1.089(2) 0.6488(9) 1.2239(14) 0.042(3) Uani 1 1 d . . . C42 C 1.224(3) 0.7017(10) 1.2823(17) 0.059(4) Uani 1 1 d . . . H42 H 1.3363 0.6833 1.3357 0.070 Uiso 1 1 calc R . . C43 C 1.194(3) 0.7830(12) 1.2627(18) 0.067(5) Uani 1 1 d . . . H43 H 1.2863 0.8191 1.3013 0.081 Uiso 1 1 calc R . . C44 C 1.029(4) 0.8079(11) 1.1866(19) 0.071(6) Uani 1 1 d . . . H44 H 1.0079 0.8622 1.1747 0.085 Uiso 1 1 calc R . . C45 C 0.891(3) 0.7574(12) 1.1266(19) 0.066(5) Uani 1 1 d . . . H45 H 0.7781 0.7763 1.0747 0.079 Uiso 1 1 calc R . . C46 C 0.924(2) 0.6769(11) 1.1451(18) 0.054(4) Uani 1 1 d . . . H46 H 0.8322 0.6412 1.1031 0.065 Uiso 1 1 calc R . . C51 C 0.892(2) 0.2218(8) 1.1210(13) 0.040(3) Uani 1 1 d . . . C52 C 0.727(2) 0.2236(11) 1.0224(14) 0.054(4) Uani 1 1 d . . . H52 H 0.6781 0.2713 0.9827 0.065 Uiso 1 1 calc R . . C53 C 0.634(2) 0.1539(12) 0.9828(19) 0.062(4) Uani 1 1 d . . . H53 H 0.5234 0.1551 0.9142 0.074 Uiso 1 1 calc R . . C54 C 0.700(3) 0.0825(11) 1.0411(19) 0.064(5) Uani 1 1 d . . . H54 H 0.6324 0.0364 1.0163 0.077 Uiso 1 1 calc R . . C55 C 0.869(3) 0.0809(10) 1.1367(18) 0.058(4) Uani 1 1 d . . . H55 H 0.9178 0.0326 1.1743 0.070 Uiso 1 1 calc R . . C56 C 0.968(2) 0.1503(10) 1.1785(16) 0.050(3) Uani 1 1 d . . . H56 H 1.0826 0.1489 1.2433 0.060 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 0.0278(2) 0.0369(2) 0.0303(2) -0.00202(19) 0.00598(17) -0.00215(17) Os2 0.0300(2) 0.0321(2) 0.0280(2) -0.00195(17) 0.01028(17) -0.00147(16) Os3 0.0292(2) 0.0417(3) 0.0282(2) 0.00020(19) 0.00601(17) -0.00470(18) Te4 0.0323(4) 0.0391(4) 0.0317(4) 0.0005(3) 0.0107(3) -0.0052(3) Te5 0.0346(4) 0.0450(4) 0.0370(4) -0.0111(4) 0.0157(3) -0.0066(3) O11 0.078(8) 0.068(8) 0.027(5) 0.003(5) 0.005(5) -0.009(6) O12 0.055(6) 0.045(5) 0.061(7) 0.005(5) 0.024(5) 0.014(5) O13 0.056(7) 0.067(8) 0.085(10) -0.014(7) 0.014(7) -0.022(6) O14 0.034(5) 0.080(8) 0.092(10) -0.032(8) 0.014(6) 0.012(5) O21 0.052(6) 0.035(5) 0.068(7) -0.015(5) 0.020(5) -0.012(4) O22 0.051(5) 0.049(5) 0.056(6) -0.002(5) 0.035(5) 0.009(5) O23 0.065(8) 0.055(7) 0.066(8) 0.018(6) 0.008(6) 0.017(6) O31 0.062(8) 0.136(15) 0.040(7) 0.015(8) 0.000(6) -0.020(9) O32 0.054(6) 0.072(8) 0.058(7) -0.008(6) 0.020(6) 0.017(6) O33 0.039(5) 0.089(9) 0.083(9) -0.031(8) 0.024(6) -0.033(6) C11 0.043(7) 0.044(7) 0.037(7) 0.002(6) 0.001(5) -0.003(6) C12 0.041(6) 0.032(6) 0.026(6) -0.006(5) -0.002(5) -0.008(5) C13 0.031(6) 0.047(7) 0.031(6) -0.010(6) 0.002(5) -0.007(5) C14 0.037(6) 0.055(8) 0.043(7) 0.001(6) 0.015(6) 0.002(6) C21 0.037(6) 0.035(6) 0.037(6) 0.001(5) 0.011(5) -0.001(5) C22 0.035(6) 0.033(6) 0.033(6) -0.004(5) 0.008(5) -0.019(4) C23 0.049(7) 0.031(6) 0.043(7) 0.006(5) 0.015(6) 0.006(5) C31 0.031(6) 0.072(9) 0.030(6) 0.014(7) -0.003(5) -0.014(6) C32 0.041(7) 0.047(7) 0.052(9) 0.018(7) 0.011(6) -0.001(6) C33 0.044(7) 0.050(8) 0.045(8) -0.008(6) 0.015(6) -0.012(6) C41 0.046(7) 0.048(7) 0.035(7) 0.004(6) 0.019(6) -0.011(6) C42 0.067(10) 0.047(8) 0.046(9) -0.015(7) 0.001(7) -0.026(8) C43 0.092(13) 0.049(9) 0.043(9) -0.014(8) 0.004(9) -0.006(9) C44 0.128(19) 0.044(9) 0.058(11) 0.010(8) 0.054(13) 0.012(10) C45 0.090(14) 0.062(11) 0.050(10) 0.014(8) 0.030(10) 0.020(10) C46 0.046(8) 0.065(10) 0.049(9) 0.010(7) 0.014(7) 0.006(7) C51 0.051(7) 0.041(6) 0.033(6) -0.017(5) 0.020(6) -0.015(6) C52 0.064(10) 0.058(9) 0.027(7) -0.003(7) 0.000(6) 0.003(7) C53 0.053(9) 0.072(11) 0.054(10) -0.021(9) 0.011(8) -0.015(8) C54 0.087(13) 0.057(10) 0.052(10) -0.025(8) 0.029(9) -0.026(9) C55 0.081(12) 0.045(8) 0.050(9) -0.005(7) 0.027(9) -0.011(8) C56 0.050(8) 0.055(8) 0.041(8) -0.015(7) 0.009(6) -0.010(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 C11 1.932(14) . ? Os1 C14 1.934(15) . ? Os1 C13 1.945(13) . ? Os1 C12 1.985(14) . ? Os1 Te4 2.7190(9) . ? Os1 Os2 2.9971(6) . ? Os2 C22 1.887(13) . ? Os2 C21 1.900(13) . ? Os2 C23 1.906(13) . ? Os2 Te5 2.6976(9) . ? Os2 Os3 2.8816(6) . ? Os3 C33 1.877(14) . ? Os3 C31 1.914(13) . ? Os3 C32 1.928(18) . ? Os3 Te5 2.6886(10) . ? Os3 Te4 2.7274(9) . ? Te4 C41 2.138(16) . ? Te5 C51 2.137(13) . ? O11 C11 1.123(18) . ? O12 C12 1.133(17) . ? O13 C13 1.097(18) . ? O14 C14 1.143(19) . ? O21 C21 1.149(17) . ? O22 C22 1.131(16) . ? O23 C23 1.154(18) . ? O31 C31 1.158(19) . ? O32 C32 1.11(2) . ? O33 C33 1.153(18) . ? C41 C42 1.36(2) . ? C41 C46 1.37(2) . ? C42 C43 1.39(3) . ? C43 C44 1.35(3) . ? C44 C45 1.36(3) . ? C45 C46 1.38(3) . ? C51 C52 1.37(2) . ? C51 C56 1.39(2) . ? C52 C53 1.37(2) . ? C53 C54 1.38(3) . ? C54 C55 1.37(3) . ? C55 C56 1.40(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Os1 C14 92.3(7) . . ? C11 Os1 C13 97.3(6) . . ? C14 Os1 C13 95.9(6) . . ? C11 Os1 C12 94.4(6) . . ? C14 Os1 C12 166.4(6) . . ? C13 Os1 C12 94.9(5) . . ? C11 Os1 Te4 166.6(4) . . ? C14 Os1 Te4 85.9(4) . . ? C13 Os1 Te4 96.1(4) . . ? C12 Os1 Te4 84.8(4) . . ? C11 Os1 Os2 84.8(5) . . ? C14 Os1 Os2 79.7(4) . . ? C13 Os1 Os2 175.3(4) . . ? C12 Os1 Os2 89.1(3) . . ? Te4 Os1 Os2 81.80(2) . . ? C22 Os2 C21 93.2(5) . . ? C22 Os2 C23 101.4(6) . . ? C21 Os2 C23 93.1(6) . . ? C22 Os2 Te5 156.7(4) . . ? C21 Os2 Te5 88.1(4) . . ? C23 Os2 Te5 101.7(4) . . ? C22 Os2 Os3 99.2(4) . . ? C21 Os2 Os3 91.8(4) . . ? C23 Os2 Os3 158.5(4) . . ? Te5 Os2 Os3 57.50(2) . . ? C22 Os2 Os1 82.0(3) . . ? C21 Os2 Os1 175.2(4) . . ? C23 Os2 Os1 87.3(4) . . ? Te5 Os2 Os1 96.48(2) . . ? Os3 Os2 Os1 89.590(18) . . ? C33 Os3 C31 94.3(6) . . ? C33 Os3 C32 88.2(6) . . ? C31 Os3 C32 105.8(7) . . ? C33 Os3 Te5 97.2(5) . . ? C31 Os3 Te5 104.6(6) . . ? C32 Os3 Te5 148.6(5) . . ? C33 Os3 Te4 175.3(5) . . ? C31 Os3 Te4 89.3(4) . . ? C32 Os3 Te4 93.8(4) . . ? Te5 Os3 Te4 78.93(3) . . ? C33 Os3 Os2 91.8(5) . . ? C31 Os3 Os2 162.1(5) . . ? C32 Os3 Os2 91.3(4) . . ? Te5 Os3 Os2 57.81(2) . . ? Te4 Os3 Os2 83.82(2) . . ? C41 Te4 Os1 105.9(4) . . ? C41 Te4 Os3 106.8(4) . . ? Os1 Te4 Os3 99.04(3) . . ? C51 Te5 Os3 107.3(4) . . ? C51 Te5 Os2 104.5(3) . . ? Os3 Te5 Os2 64.69(2) . . ? O11 C11 Os1 180.0(19) . . ? O12 C12 Os1 177.5(12) . . ? O13 C13 Os1 175.8(15) . . ? O14 C14 Os1 179.0(14) . . ? O21 C21 Os2 175.5(13) . . ? O22 C22 Os2 177.5(11) . . ? O23 C23 Os2 178.2(13) . . ? O31 C31 Os3 177.6(15) . . ? O32 C32 Os3 175.4(14) . . ? O33 C33 Os3 176.2(15) . . ? C42 C41 C46 118.8(16) . . ? C42 C41 Te4 119.4(13) . . ? C46 C41 Te4 121.4(12) . . ? C41 C42 C43 120.8(19) . . ? C44 C43 C42 118.3(19) . . ? C43 C44 C45 122.8(18) . . ? C44 C45 C46 118(2) . . ? C41 C46 C45 121.3(19) . . ? C52 C51 C56 120.8(14) . . ? C52 C51 Te5 123.0(12) . . ? C56 C51 Te5 116.1(11) . . ? C51 C52 C53 119.0(16) . . ? C52 C53 C54 122.2(17) . . ? C55 C54 C53 118.3(16) . . ? C54 C55 C56 121.1(18) . . ? C51 C56 C55 118.4(16) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 29.32 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 2.393 _refine_diff_density_min -2.819 _refine_diff_density_rms 0.304 #==================================================================== # CRYSTAL DATA FOR COMPOUND 2 #========================================================================= data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H10 O10 Os3 Te2' _chemical_formula_weight 1260.10 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' 'Te' 'Te' -0.5308 1.6751 '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 15.74110(10) _cell_length_b 12.736 _cell_length_c 14.6953(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.71 _cell_angle_gamma 90.00 _cell_volume 2697.29(4) _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 'IRREGULAR BLOCK' _exptl_crystal_colour 'YELLOW' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.103 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 16.269 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.027065 _exptl_absorpt_correction_T_max 0.080829 _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 18176 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 29.15 _reflns_number_total 3302 _reflns_number_gt 2760 _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^)+(0.0526P)^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 3302 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.137 _refine_ls_shift/su_mean 0.008 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 0.0000 0.43873(3) 0.2500 0.03704(13) Uani 1 2 d S . . Os2 Os 0.09324(2) 0.25433(2) 0.20818(2) 0.03443(11) Uani 1 1 d . . . Te3 Te -0.08517(3) 0.17853(4) 0.12048(4) 0.03708(14) Uani 1 1 d . . . O11 O -0.1527(5) 0.4306(6) 0.0369(5) 0.073(2) Uani 1 1 d . . . O12 O 0.1132(6) 0.5960(6) 0.1841(6) 0.075(2) Uani 1 1 d . . . O21 O 0.0646(5) 0.3862(5) 0.0239(5) 0.0609(17) Uani 1 1 d . . . O22 O 0.1921(5) 0.0788(5) 0.1474(6) 0.0692(19) Uani 1 1 d . . . O23 O 0.2814(5) 0.3503(6) 0.3387(5) 0.0663(18) Uani 1 1 d . . . C11 C -0.0970(6) 0.4310(6) 0.1146(7) 0.0467(19) Uani 1 1 d . . . C12 C 0.0737(6) 0.5361(8) 0.2113(7) 0.051(2) Uani 1 1 d . . . C21 C 0.0754(6) 0.3349(6) 0.0922(7) 0.0446(18) Uani 1 1 d . . . C22 C 0.1518(6) 0.1388(7) 0.1719(6) 0.0447(18) Uani 1 1 d . . . C23 C 0.2104(6) 0.3166(6) 0.2900(6) 0.0452(19) Uani 1 1 d . . . C31 C -0.0863(5) 0.0102(6) 0.1264(5) 0.0362(15) Uani 1 1 d . . . C32 C -0.0179(6) -0.0518(7) 0.1163(6) 0.0456(19) Uani 1 1 d . . . H32A H 0.0335 -0.0199 0.1120 0.055 Uiso 1 1 calc R . . C33 C -0.0248(7) -0.1593(7) 0.1125(7) 0.056(2) Uani 1 1 d . . . H33A H 0.0223 -0.1998 0.1073 0.068 Uiso 1 1 calc R . . C34 C -0.1034(7) -0.2077(7) 0.1164(7) 0.056(2) Uani 1 1 d . . . H34A H -0.1082 -0.2805 0.1149 0.067 Uiso 1 1 calc R . . C35 C -0.1735(7) -0.1468(7) 0.1226(7) 0.053(2) Uani 1 1 d . . . H35A H -0.2271 -0.1781 0.1220 0.064 Uiso 1 1 calc R . . C36 C -0.1632(6) -0.0382(7) 0.1297(6) 0.0457(19) Uani 1 1 d . . . H36A H -0.2092 0.0025 0.1368 0.055 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 0.0420(2) 0.0263(2) 0.0407(2) 0.000 0.01437(19) 0.000 Os2 0.03774(18) 0.02804(17) 0.03819(18) 0.00047(11) 0.01596(14) -0.00118(11) Te3 0.0398(3) 0.0325(3) 0.0353(3) -0.00169(18) 0.0113(2) -0.00006(19) O11 0.064(5) 0.068(5) 0.060(4) 0.019(4) -0.003(4) -0.008(4) O12 0.081(5) 0.061(5) 0.089(5) 0.009(4) 0.042(4) -0.017(4) O21 0.091(5) 0.047(4) 0.056(4) 0.010(3) 0.042(4) 0.003(3) O22 0.059(4) 0.052(4) 0.099(5) -0.016(4) 0.035(4) 0.006(3) O23 0.054(4) 0.068(5) 0.068(4) -0.010(4) 0.016(3) -0.023(4) C11 0.050(5) 0.031(4) 0.052(5) 0.008(3) 0.014(4) 0.003(3) C12 0.049(5) 0.051(5) 0.051(5) -0.002(4) 0.018(4) -0.002(4) C21 0.052(5) 0.036(4) 0.053(5) -0.002(4) 0.028(4) 0.000(4) C22 0.041(4) 0.044(5) 0.050(5) 0.001(4) 0.020(4) -0.001(4) C23 0.051(5) 0.038(4) 0.049(5) 0.001(3) 0.023(4) -0.006(4) C31 0.042(4) 0.032(4) 0.028(3) -0.002(3) 0.008(3) -0.003(3) C32 0.046(5) 0.040(4) 0.056(5) -0.010(4) 0.027(4) -0.007(3) C33 0.054(5) 0.048(5) 0.073(6) -0.017(4) 0.031(5) -0.002(4) C34 0.079(7) 0.028(4) 0.062(6) -0.004(4) 0.029(5) -0.008(4) C35 0.058(5) 0.048(5) 0.061(5) -0.007(4) 0.032(5) -0.013(4) C36 0.046(4) 0.041(5) 0.055(5) -0.003(4) 0.027(4) -0.001(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 1.933(10) . ? Os1 C12 1.933(10) 2 ? Os1 C11 1.964(9) . ? Os1 C11 1.964(9) 2 ? Os1 Os2 2.9618(4) . ? Os1 Os2 2.9618(4) 2 ? Os2 C21 1.911(9) . ? Os2 C23 1.921(9) . ? Os2 C22 1.923(9) . ? Os2 Te3 2.7469(6) 2 ? Os2 Te3 2.7511(6) . ? Te3 C31 2.145(7) . ? Te3 Os2 2.7469(6) 2 ? O11 C11 1.126(10) . ? O12 C12 1.153(11) . ? O21 C21 1.151(10) . ? O22 C22 1.138(10) . ? O23 C23 1.141(10) . ? C31 C36 1.377(11) . ? C31 C32 1.391(11) . ? C32 C33 1.372(12) . ? C33 C34 1.404(13) . ? C34 C35 1.382(13) . ? C35 C36 1.392(12) . ? 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 C12 100.2(6) . 2 ? C12 Os1 C11 92.8(4) . . ? C12 Os1 C11 90.9(4) 2 . ? C12 Os1 C11 90.9(4) . 2 ? C12 Os1 C11 92.8(4) 2 2 ? C11 Os1 C11 174.2(5) . 2 ? C12 Os1 Os2 92.4(3) . . ? C12 Os1 Os2 167.3(3) 2 . ? C11 Os1 Os2 89.9(2) . . ? C11 Os1 Os2 85.5(2) 2 . ? C12 Os1 Os2 167.3(3) . 2 ? C12 Os1 Os2 92.4(3) 2 2 ? C11 Os1 Os2 85.5(2) . 2 ? C11 Os1 Os2 89.9(3) 2 2 ? Os2 Os1 Os2 75.083(15) . 2 ? C21 Os2 C23 95.6(4) . . ? C21 Os2 C22 94.5(3) . . ? C23 Os2 C22 92.4(4) . . ? C21 Os2 Te3 164.1(2) . 2 ? C23 Os2 Te3 87.6(2) . 2 ? C22 Os2 Te3 100.9(2) . 2 ? C21 Os2 Te3 90.8(3) . . ? C23 Os2 Te3 168.5(3) . . ? C22 Os2 Te3 96.6(2) . . ? Te3 Os2 Te3 83.760(18) 2 . ? C21 Os2 Os1 81.5(2) . . ? C23 Os2 Os1 88.5(3) . . ? C22 Os2 Os1 175.9(3) . . ? Te3 Os2 Os1 83.052(13) 2 . ? Te3 Os2 Os1 82.981(13) . . ? C31 Te3 Os2 108.04(19) . 2 ? C31 Te3 Os2 110.80(19) . . ? Os2 Te3 Os2 82.069(16) 2 . ? O11 C11 Os1 177.4(8) . . ? O12 C12 Os1 176.2(9) . . ? O21 C21 Os2 177.8(7) . . ? O22 C22 Os2 172.2(8) . . ? O23 C23 Os2 177.7(8) . . ? C36 C31 C32 118.6(7) . . ? C36 C31 Te3 118.1(6) . . ? C32 C31 Te3 123.0(6) . . ? C33 C32 C31 121.3(8) . . ? C32 C33 C34 119.5(8) . . ? C35 C34 C33 119.8(8) . . ? C34 C35 C36 119.4(8) . . ? C31 C36 C35 121.3(8) . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 1.393 _refine_diff_density_min -1.979 _refine_diff_density_rms 0.297 #==================================================================== # CRYSTAL DATA FOR COMPOUND 4 #========================================================================= data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H12 O10 Os3 Te2' _chemical_formula_weight 1262.12 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' 'Te' 'Te' -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Os' 'Os' -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ORTHORHOMBIC _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 20.6376(5) _cell_length_b 15.3639(4) _cell_length_c 9.0517(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2870.06(12) _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 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.921 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 15.290 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.094988 _exptl_absorpt_correction_T_max 0.432068 _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 3763 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 29.26 _reflns_number_total 3763 _reflns_number_gt 3184 _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^)+(0.0398P)^2^+8.4030P] 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 3763 _refine_ls_number_parameters 188 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.179 _refine_ls_shift/su_mean 0.011 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 0.069339(18) 0.2500 0.17250(4) 0.03554(10) Uani 1 2 d SD . . Os2 Os -0.132177(18) 0.2500 -0.15518(4) 0.04240(11) Uani 1 2 d SD . . Os3 Os 0.003668(16) 0.2500 -0.25620(4) 0.03283(9) Uani 1 2 d S . . Te4 Te 0.030188(19) 0.13221(2) -0.03569(4) 0.03283(10) Uani 1 1 d . . . O11 O 0.1227(3) 0.1080(4) 0.3767(7) 0.0779(19) Uani 1 1 d . . . O12 O -0.0694(4) 0.2500 0.3075(8) 0.069(3) Uani 1 2 d S . . O21 O -0.2477(4) 0.2500 0.0542(12) 0.099(4) Uani 1 2 d S . . O22 O -0.1952(4) 0.2500 -0.4674(9) 0.075(3) Uani 1 2 d S . . O23 O -0.1219(3) 0.0494(4) -0.1676(7) 0.0736(18) Uani 1 1 d . . . O31 O -0.0345(3) 0.1019(4) -0.4642(6) 0.0755(19) Uani 1 1 d . . . O32 O 0.1476(4) 0.2500 -0.3362(10) 0.074(3) Uani 1 2 d S . . C11 C 0.1017(4) 0.1601(5) 0.3001(8) 0.0508(17) Uani 1 1 d . . . C12 C -0.0180(5) 0.2500 0.2553(10) 0.046(2) Uani 1 2 d S . . C21 C -0.2073(5) 0.2500 -0.0277(14) 0.063(3) Uani 1 2 d S . . C22 C -0.1726(5) 0.2500 -0.3550(13) 0.052(3) Uani 1 2 d S . . C23 C -0.1253(4) 0.1225(5) -0.1599(9) 0.056(2) Uani 1 1 d . . . C31 C -0.0210(4) 0.1581(5) -0.3867(7) 0.0464(16) Uani 1 1 d . . . C32 C 0.0938(5) 0.2500 -0.3053(11) 0.048(2) Uani 1 2 d S . . C411 C 0.1154(3) 0.0690(4) -0.1182(7) 0.0361(13) Uani 1 1 d . . . C412 C 0.1041(4) 0.0010(5) -0.2187(10) 0.0544(18) Uani 1 1 d . . . H41B H 0.0622 -0.0114 -0.2502 0.065 Uiso 1 1 calc R . . C413 C 0.1560(4) -0.0476(6) -0.2705(11) 0.075(3) Uani 1 1 d . . . H41D H 0.1486 -0.0933 -0.3358 0.090 Uiso 1 1 calc R . . C414 C 0.2183(4) -0.0289(6) -0.2259(11) 0.068(2) Uani 1 1 d . . . H41E H 0.2529 -0.0611 -0.2626 0.082 Uiso 1 1 calc R . . C415 C 0.2289(4) 0.0364(6) -0.1287(10) 0.061(2) Uani 1 1 d . . . H41C H 0.2709 0.0479 -0.0971 0.073 Uiso 1 1 calc R . . C416 C 0.1773(3) 0.0872(5) -0.0746(8) 0.0499(17) Uani 1 1 d . . . H41A H 0.1853 0.1328 -0.0096 0.060 Uiso 1 1 calc R . . H1 H 0.1384(16) 0.2500 0.092(7) 0.050 Uiso 1 2 d SD . . H2 H -0.089(3) 0.2500 -0.008(4) 0.050 Uiso 1 2 d SD . . 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 0.04048(19) 0.03630(18) 0.02985(17) 0.000 -0.00186(14) 0.000 Os2 0.03467(19) 0.0460(2) 0.0465(2) 0.000 -0.00628(16) 0.000 Os3 0.03881(19) 0.03095(16) 0.02873(17) 0.000 -0.00233(13) 0.000 Te4 0.0343(2) 0.02933(19) 0.0348(2) 0.00099(14) -0.00048(16) 0.00038(15) O11 0.105(5) 0.062(4) 0.068(4) 0.014(3) -0.019(4) 0.018(4) O12 0.047(5) 0.115(8) 0.045(4) 0.000 0.008(4) 0.000 O21 0.052(5) 0.156(11) 0.088(7) 0.000 0.019(5) 0.000 O22 0.073(6) 0.096(7) 0.055(5) 0.000 -0.024(5) 0.000 O23 0.084(4) 0.043(3) 0.093(5) 0.015(3) -0.023(3) -0.018(3) O31 0.111(5) 0.059(4) 0.057(3) -0.017(3) -0.021(4) -0.015(3) O32 0.053(5) 0.083(6) 0.085(7) 0.000 0.028(4) 0.000 C11 0.056(4) 0.054(4) 0.042(4) 0.000(3) -0.007(3) -0.001(4) C12 0.053(6) 0.056(6) 0.028(4) 0.000 -0.002(4) 0.000 C21 0.038(6) 0.086(9) 0.064(7) 0.000 0.003(5) 0.000 C22 0.046(6) 0.050(6) 0.061(7) 0.000 -0.011(5) 0.000 C23 0.049(4) 0.057(5) 0.060(5) 0.015(4) -0.017(4) -0.015(3) C31 0.061(4) 0.042(4) 0.036(3) 0.000(3) -0.008(3) 0.001(3) C32 0.056(6) 0.048(6) 0.039(5) 0.000 0.006(5) 0.000 C411 0.038(3) 0.035(3) 0.035(3) 0.002(2) 0.005(3) 0.006(3) C412 0.046(4) 0.051(4) 0.067(5) -0.018(4) 0.004(4) 0.000(3) C413 0.061(5) 0.076(6) 0.089(7) -0.040(5) 0.010(5) 0.008(4) C414 0.050(5) 0.072(6) 0.082(6) -0.011(5) 0.013(4) 0.016(4) C415 0.043(4) 0.074(6) 0.066(5) -0.006(4) 0.001(4) 0.001(4) C416 0.038(3) 0.057(4) 0.055(4) -0.004(3) -0.001(3) 0.003(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 C11 1.920(8) 7_565 ? Os1 C11 1.920(8) . ? Os1 C12 1.951(11) . ? Os1 Te4 2.7348(5) . ? Os1 Te4 2.7348(5) 7_565 ? Os2 C21 1.932(12) . ? Os2 C23 1.964(8) 7_565 ? Os2 C23 1.964(8) . ? Os2 C22 1.991(11) . ? Os2 Os3 2.9489(5) . ? Os3 C31 1.910(7) . ? Os3 C31 1.910(7) 7_565 ? Os3 C32 1.913(11) . ? Os3 Te4 2.7493(4) 7_565 ? Os3 Te4 2.7493(4) . ? Te4 C411 2.143(6) . ? O11 C11 1.145(9) . ? O12 C12 1.161(12) . ? O21 C21 1.116(13) . ? O22 C22 1.120(12) . ? O23 C23 1.127(10) . ? O31 C31 1.147(9) . ? O32 C32 1.144(13) . ? C411 C416 1.366(9) . ? C411 C412 1.405(9) . ? C412 C413 1.387(10) . ? C413 C414 1.378(12) . ? C414 C415 1.352(13) . ? C415 C416 1.409(10) . ? 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 C11 91.9(4) 7_565 . ? C11 Os1 C12 95.2(3) 7_565 . ? C11 Os1 C12 95.2(3) . . ? C11 Os1 Te4 173.3(2) 7_565 . ? C11 Os1 Te4 92.4(2) . . ? C12 Os1 Te4 89.5(2) . . ? C11 Os1 Te4 92.4(2) 7_565 7_565 ? C11 Os1 Te4 173.3(2) . 7_565 ? C12 Os1 Te4 89.5(2) . 7_565 ? Te4 Os1 Te4 82.864(18) . 7_565 ? C21 Os2 C23 94.0(2) . 7_565 ? C21 Os2 C23 94.0(2) . . ? C23 Os2 C23 171.4(5) 7_565 . ? C21 Os2 C22 101.9(5) . . ? C23 Os2 C22 90.6(2) 7_565 . ? C23 Os2 C22 90.6(2) . . ? C21 Os2 Os3 161.4(4) . . ? C23 Os2 Os3 85.7(2) 7_565 . ? C23 Os2 Os3 85.7(2) . . ? C22 Os2 Os3 96.7(3) . . ? C31 Os3 C31 95.4(4) . 7_565 ? C31 Os3 C32 96.7(3) . . ? C31 Os3 C32 96.7(3) 7_565 . ? C31 Os3 Te4 171.3(2) . 7_565 ? C31 Os3 Te4 90.9(2) 7_565 7_565 ? C32 Os3 Te4 88.6(2) . 7_565 ? C31 Os3 Te4 90.9(2) . . ? C31 Os3 Te4 171.3(2) 7_565 . ? C32 Os3 Te4 88.6(2) . . ? Te4 Os3 Te4 82.331(18) 7_565 . ? C31 Os3 Os2 86.4(2) . . ? C31 Os3 Os2 86.4(2) 7_565 . ? C32 Os3 Os2 175.4(3) . . ? Te4 Os3 Os2 87.944(13) 7_565 . ? Te4 Os3 Os2 87.944(13) . . ? C411 Te4 Os1 107.32(17) . . ? C411 Te4 Os3 102.03(16) . . ? Os1 Te4 Os3 97.095(13) . . ? O11 C11 Os1 177.9(7) . . ? O12 C12 Os1 178.6(8) . . ? O21 C21 Os2 175.1(11) . . ? O22 C22 Os2 179.9(11) . . ? O23 C23 Os2 177.6(7) . . ? O31 C31 Os3 178.4(7) . . ? O32 C32 Os3 179.2(10) . . ? C416 C411 C412 119.6(6) . . ? C416 C411 Te4 125.0(5) . . ? C412 C411 Te4 115.3(5) . . ? C413 C412 C411 119.4(7) . . ? C414 C413 C412 120.6(8) . . ? C415 C414 C413 119.7(8) . . ? C414 C415 C416 121.0(8) . . ? C411 C416 C415 119.5(7) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 29.26 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 1.335 _refine_diff_density_min -1.770 _refine_diff_density_rms 0.234 #==================================================================== # CRYSTAL DATA FOR COMPOUND 6 #========================================================================= data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H12 O6 Os2 Te2' _chemical_formula_weight 959.88 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' 'Te' 'Te' -0.5308 1.6751 '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 9.3686(4) _cell_length_b 6.2656(3) _cell_length_c 19.0147(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.4480(10) _cell_angle_gamma 90.00 _cell_volume 1116.13(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 'PLATE' _exptl_crystal_colour 'PALE YELLOW' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.856 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 13.964 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.261783 _exptl_absorpt_correction_T_max 0.404935 _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 7115 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 29.25 _reflns_number_total 2715 _reflns_number_gt 2261 _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^)+(0.0293P)^2^+2.1199P] 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 2715 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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 0.65414(3) 0.97376(4) 0.075016(12) 0.03906(9) Uani 1 1 d . . . Te2 Te 0.42383(4) 1.22915(6) 0.04651(2) 0.03747(11) Uani 1 1 d . . . O11 O 0.6795(7) 1.1627(11) 0.2221(3) 0.0818(19) Uani 1 1 d . . . O12 O 0.8739(8) 0.6293(12) 0.1075(3) 0.092(2) Uani 1 1 d . . . O13 O 0.8643(8) 1.2733(11) -0.0026(4) 0.089(2) Uani 1 1 d . . . C11 C 0.6711(8) 1.0960(14) 0.1667(4) 0.0535(18) Uani 1 1 d . . . C12 C 0.7940(8) 0.7618(13) 0.0942(4) 0.0555(19) Uani 1 1 d . . . C13 C 0.7852(9) 1.1682(12) 0.0265(4) 0.0551(18) Uani 1 1 d . . . C21 C 0.2637(7) 1.1377(10) 0.1206(3) 0.0365(13) Uani 1 1 d . . . C22 C 0.1590(8) 1.2874(12) 0.1340(4) 0.0504(16) Uani 1 1 d . . . H22A H 0.1598 1.4177 0.1105 0.060 Uiso 1 1 calc R . . C23 C 0.0535(8) 1.2437(13) 0.1820(4) 0.063(2) Uani 1 1 d . . . H23A H -0.0167 1.3448 0.1910 0.075 Uiso 1 1 calc R . . C24 C 0.0518(8) 1.0496(13) 0.2169(4) 0.0551(18) Uani 1 1 d . . . H24A H -0.0188 1.0206 0.2497 0.066 Uiso 1 1 calc R . . C25 C 0.1555(8) 0.8998(13) 0.2026(4) 0.0556(18) Uani 1 1 d . . . H25A H 0.1534 0.7685 0.2254 0.067 Uiso 1 1 calc R . . C26 C 0.2619(8) 0.9418(11) 0.1553(4) 0.0478(16) Uani 1 1 d . . . H26A H 0.3321 0.8404 0.1464 0.057 Uiso 1 1 calc R . . H1 H 0.545(9) 0.795(14) 0.107(5) 0.09(3) 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 0.03808(15) 0.04837(16) 0.03076(13) 0.00169(10) 0.00170(9) 0.00380(11) Te2 0.0418(2) 0.0365(2) 0.0341(2) 0.00252(15) 0.00389(16) 0.00090(16) O11 0.085(4) 0.118(5) 0.043(3) -0.025(3) 0.001(3) 0.026(4) O12 0.102(5) 0.094(5) 0.079(4) -0.001(4) -0.018(4) 0.053(4) O13 0.096(5) 0.093(5) 0.078(4) 0.003(4) 0.017(4) -0.044(4) C11 0.042(4) 0.073(5) 0.046(4) -0.003(3) 0.002(3) 0.013(4) C12 0.055(4) 0.071(5) 0.040(4) 0.002(3) -0.005(3) 0.009(4) C13 0.062(5) 0.053(4) 0.050(4) -0.002(3) -0.003(4) -0.004(4) C21 0.040(3) 0.041(3) 0.028(3) 0.003(2) 0.003(2) -0.003(3) C22 0.051(4) 0.047(4) 0.053(4) 0.006(3) 0.009(3) 0.005(3) C23 0.044(4) 0.068(5) 0.076(5) 0.010(4) 0.018(4) 0.014(4) C24 0.040(4) 0.074(5) 0.052(4) 0.005(4) 0.015(3) -0.002(4) C25 0.057(5) 0.058(4) 0.051(4) 0.009(3) 0.005(3) 0.002(4) C26 0.053(4) 0.048(4) 0.042(4) 0.007(3) 0.010(3) 0.009(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 1.899(8) . ? Os1 C11 1.909(7) . ? Os1 C13 1.965(8) . ? Os1 Te2 2.7318(5) 3_675 ? Os1 Te2 2.7372(5) . ? Te2 C21 2.144(6) . ? Te2 Os1 2.7318(5) 3_675 ? O11 C11 1.136(8) . ? O12 C12 1.145(9) . ? O13 C13 1.139(9) . ? C21 C22 1.382(9) . ? C21 C26 1.393(9) . ? C22 C23 1.379(10) . ? C23 C24 1.385(11) . ? C24 C25 1.380(11) . ? C25 C26 1.374(10) . ? 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 93.0(3) . . ? C12 Os1 C13 95.2(3) . . ? C11 Os1 C13 97.6(3) . . ? C12 Os1 Te2 90.9(2) . 3_675 ? C11 Os1 Te2 168.1(2) . 3_675 ? C13 Os1 Te2 93.2(2) . 3_675 ? C12 Os1 Te2 171.3(2) . . ? C11 Os1 Te2 90.4(2) . . ? C13 Os1 Te2 92.2(2) . . ? Te2 Os1 Te2 84.226(14) 3_675 . ? C21 Te2 Os1 104.34(15) . 3_675 ? C21 Te2 Os1 105.55(16) . . ? Os1 Te2 Os1 95.774(14) 3_675 . ? O11 C11 Os1 177.8(8) . . ? O12 C12 Os1 177.0(8) . . ? O13 C13 Os1 177.0(8) . . ? C22 C21 C26 120.0(6) . . ? C22 C21 Te2 116.1(5) . . ? C26 C21 Te2 123.9(5) . . ? C23 C22 C21 120.0(7) . . ? C22 C23 C24 120.2(7) . . ? C25 C24 C23 119.5(7) . . ? C26 C25 C24 121.0(7) . . ? C25 C26 C21 119.3(7) . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 29.25 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 2.034 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.172 #======END========================