# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Wong, W.-T.' 'Wong, J.S.-Y' _publ_contact_author_name 'Dr W.-T. Wong' _publ_contact_author_address ; Department of Chemistry The University of Hong Kong Pokfulam Road Hong Kong ; _publ_contact_author_email 'WTWONG@HKUCC.HKU.HK' _publ_section_title ; Synthesis, structural characterization and reactivity of troismium carbonyl clusters containing oxime ligands. ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; data_wt0243w-JW007-compound_1 _database_code_CSD 174851 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Sep 22 18:07:05 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 13.050(2) _cell_length_b 13.050(2) _cell_length_c 19.513(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3323.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' _symmetry_Int_Tables_number 92 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' '1/2-y,1/2+x,1/4+z' '1/2+y,1/2-x,3/4+z' ' +y, +x, -z' ' -y, -x,1/2-z' '1/2-x,1/2+y,1/4-z' '1/2+x,1/2-y,3/4-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.140 _exptl_crystal_density_diffrn 2.377 _exptl_crystal_density_meas ? _chemical_formula_weight 1189.11 _chemical_formula_analytical ? _chemical_formula_sum 'C32 H18 N4 O10 Os3 ' _chemical_formula_moiety 'C32 H18 N4 O10 Os3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2184.00 _exptl_absorpt_coefficient_mu 11.498 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 20864 _reflns_number_total 3699 _reflns_number_observed 3141 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 12 -1.216 7.603 'International Tables' N 0 16 0.006 0.003 'International Tables' O 0 40 0.011 0.006 'International Tables' C 0 128 0.003 0.002 'International Tables' H 0 72 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) -0.01404(3) 0.03427(3) 0.08947(2) 0.0314(1) Uij ? ? Os(2) 0.12956(3) 0.1296 0.0000 0.03248(9) Uij ? ? O(1) -0.0693(9) 0.2375(8) 0.1530(5) 0.077(4) Uij ? ? O(2) 0.1494(8) -0.0009(8) 0.1956(5) 0.069(3) Uij ? ? O(3) 0.2722(8) 0.2039(10) -0.1130(5) 0.088(4) Uij ? ? O(4) 0.2641(8) -0.0533(8) 0.0400(5) 0.061(3) Uij ? ? O(5) 0.0595(6) -0.1296(6) -0.0154(3) 0.037(2) Uij ? ? N(1) -0.1197(8) -0.0681(7) 0.1408(4) 0.040(3) Uij ? ? N(2) 0.0071(7) -0.1135(7) 0.0433(4) 0.038(3) Uij ? ? C(1) -0.046(1) 0.161(1) 0.1291(6) 0.049(4) Uij ? ? C(2) 0.0871(9) 0.0130(9) 0.1547(6) 0.042(3) Uij ? ? C(3) 0.2199(9) 0.177(1) -0.0710(7) 0.050(4) Uij ? ? C(4) 0.2129(9) 0.016(1) 0.0245(6) 0.045(4) Uij ? ? C(5) -0.193(1) -0.041(1) 0.1872(6) 0.050(4) Uij ? ? C(6) -0.248(1) -0.114(1) 0.2221(7) 0.054(4) Uij ? ? C(7) -0.230(1) -0.216(1) 0.2107(6) 0.056(4) Uij ? ? C(8) -0.1570(10) -0.2451(9) 0.1644(6) 0.044(4) Uij ? ? C(9) -0.1037(8) -0.1686(9) 0.1288(5) 0.036(3) Uij ? ? C(10) -0.0329(9) -0.1920(8) 0.0731(5) 0.034(3) Uij ? ? C(11) -0.0091(9) -0.2988(8) 0.0500(6) 0.037(3) Uij ? ? C(12) -0.055(1) -0.340(1) -0.0078(7) 0.059(4) Uij ? ? C(13) -0.031(1) -0.437(1) -0.0286(9) 0.074(5) Uij ? ? C(14) 0.041(1) -0.4944(9) 0.0050(9) 0.065(5) Uij ? ? C(15) 0.087(1) -0.452(1) 0.0621(8) 0.066(5) Uij ? ? C(16) 0.062(1) -0.355(1) 0.0853(7) 0.052(4) Uij ? ? H(1) -0.2056 0.0291 0.1956 0.0600 Uij ? ? H(3) -0.2682 -0.2662 0.2350 0.0667 Uij ? ? H(4) -0.1428 -0.3156 0.1566 0.0524 Uij ? ? H(5) -0.1032 -0.3009 -0.0331 0.0704 Uij ? ? H(6) -0.0651 -0.4649 -0.0673 0.0893 Uij ? ? H(7) 0.0581 -0.5612 -0.0104 0.0778 Uij ? ? H(8) 0.1376 -0.4907 0.0860 0.0790 Uij ? ? H(9) 0.0932 -0.3272 0.1252 0.0622 Uij ? ? H(10) -0.2987 -0.0930 0.2542 0.0651 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0338(2) 0.0306(2) 0.0300(2) -0.0040(2) 0.0034(2) -0.0047(2) Os(2) 0.0304(2) 0.0304 0.0367(3) -0.0050(3) 0.0009 -0.0009(2) O(1) 0.099(8) 0.046(6) 0.085(8) 0.020(6) -0.020(7) -0.033(6) O(2) 0.067(7) 0.086(8) 0.055(6) -0.003(6) -0.019(5) 0.002(6) O(3) 0.072(8) 0.12(1) 0.074(7) -0.019(7) 0.022(6) 0.024(7) O(4) 0.058(6) 0.053(6) 0.073(7) 0.007(5) -0.010(5) 0.000(5) O(5) 0.043(5) 0.032(4) 0.037(5) -0.004(4) 0.012(3) -0.005(3) N(1) 0.046(6) 0.042(6) 0.034(5) -0.010(5) 0.003(4) 0.001(4) N(2) 0.033(5) 0.047(6) 0.033(5) -0.008(5) 0.001(4) -0.001(4) C(1) 0.045(8) 0.056(9) 0.047(8) -0.009(7) -0.008(6) -0.005(6) C(2) 0.041(6) 0.040(7) 0.045(7) -0.009(6) 0.005(6) -0.001(6) C(3) 0.035(7) 0.049(8) 0.065(9) -0.003(6) 0.002(6) 0.017(7) C(4) 0.034(6) 0.051(8) 0.051(8) -0.011(6) 0.003(6) -0.002(6) C(5) 0.049(8) 0.049(8) 0.051(8) 0.003(7) 0.014(6) -0.013(6) C(6) 0.047(8) 0.066(10) 0.050(8) -0.007(7) 0.022(6) -0.010(7) C(7) 0.050(9) 0.064(10) 0.053(8) -0.014(7) 0.011(7) 0.007(7) C(8) 0.043(7) 0.044(7) 0.044(7) -0.007(6) 0.008(6) 0.005(6) C(9) 0.037(7) 0.041(7) 0.029(6) 0.005(5) 0.002(5) -0.003(5) C(10) 0.036(6) 0.036(6) 0.030(6) -0.002(5) 0.001(5) 0.002(5) C(11) 0.039(7) 0.030(6) 0.042(7) -0.003(6) 0.015(5) 0.005(5) C(12) 0.063(9) 0.052(8) 0.062(9) 0.007(7) -0.013(8) -0.019(7) C(13) 0.07(1) 0.057(9) 0.09(1) -0.008(9) -0.004(10) -0.026(9) C(14) 0.055(9) 0.030(7) 0.11(1) 0.001(7) 0.028(9) -0.013(9) C(15) 0.07(1) 0.051(9) 0.07(1) 0.014(8) -0.005(8) 0.003(8) C(16) 0.050(8) 0.050(8) 0.056(8) 0.014(7) 0.001(7) -0.003(7) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3141 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0351 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0378 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.166 _refine_ls_shift/esd_max 0.0006 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.61 _refine_diff_density_max 3.03 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Os(2) 2.8472(6) ? ? yes Os(1) O(5) 2.115(7) ? ? yes Os(1) N(1) 2.165(9) ? ? yes Os(1) N(2) 2.146(9) ? ? yes Os(1) C(1) 1.87(1) ? ? yes Os(1) C(2) 1.86(1) ? ? yes Os(2) C(3) 1.92(1) ? ? yes Os(2) C(3) 1.92(1) ? ? yes Os(2) C(4) 1.90(1) ? ? yes Os(2) C(4) 1.90(1) ? ? yes O(1) C(1) 1.15(2) ? ? yes O(2) C(2) 1.15(1) ? ? yes O(3) C(3) 1.12(1) ? ? yes O(4) C(4) 1.16(1) ? ? yes O(5) N(2) 1.35(1) ? ? yes N(1) C(5) 1.36(1) ? ? yes N(1) C(9) 1.35(1) ? ? yes N(2) C(10) 1.29(1) ? ? yes C(5) C(6) 1.37(2) ? ? yes C(6) C(7) 1.37(2) ? ? yes C(7) C(8) 1.37(2) ? ? yes C(8) C(9) 1.40(2) ? ? yes C(9) C(10) 1.46(1) ? ? yes C(10) C(11) 1.50(1) ? ? yes C(11) C(12) 1.39(2) ? ? yes C(11) C(16) 1.36(2) ? ? yes C(12) C(13) 1.36(2) ? ? yes C(13) C(14) 1.37(2) ? ? yes C(14) C(15) 1.38(2) ? ? yes C(15) C(16) 1.39(2) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Os(2) Os(1) O(5) 89.0(2) ? ? ? yes Os(2) Os(1) N(1) 166.5(2) ? ? ? yes Os(2) Os(1) N(2) 92.9(2) ? ? ? yes Os(2) Os(1) C(1) 90.8(4) ? ? ? yes Os(2) Os(1) C(2) 91.0(3) ? ? ? yes O(5) Os(1) N(1) 87.6(3) ? ? ? yes O(5) Os(1) N(2) 86.8(3) ? ? ? yes O(5) Os(1) C(1) 89.3(4) ? ? ? yes O(5) Os(1) C(2) 179.6(4) ? ? ? yes N(1) Os(1) N(2) 73.9(3) ? ? ? yes N(1) Os(1) C(1) 102.2(5) ? ? ? yes N(1) Os(1) C(2) 92.5(4) ? ? ? yes N(2) Os(1) C(1) 174.6(5) ? ? ? yes N(2) Os(1) C(2) 93.6(4) ? ? ? yes C(1) Os(1) C(2) 90.3(5) ? ? ? yes Os(1) Os(2) Os(1) 78.52(2) ? ? ? yes Os(1) Os(2) C(3) 170.6(4) ? ? ? yes Os(1) Os(2) C(3) 92.2(4) ? ? ? yes Os(1) Os(2) C(4) 83.2(3) ? ? ? yes Os(1) Os(2) C(4) 83.7(4) ? ? ? yes Os(1) Os(2) C(3) 92.2(4) ? ? ? yes Os(1) Os(2) C(3) 170.6(4) ? ? ? yes Os(1) Os(2) C(4) 83.7(4) ? ? ? yes Os(1) Os(2) C(4) 83.2(3) ? ? ? yes C(3) Os(2) C(3) 97.1(8) ? ? ? yes C(3) Os(2) C(4) 94.7(5) ? ? ? yes C(3) Os(2) C(4) 96.5(5) ? ? ? yes C(3) Os(2) C(4) 96.5(5) ? ? ? yes C(3) Os(2) C(4) 94.7(5) ? ? ? yes C(4) Os(2) C(4) 163.0(7) ? ? ? yes Os(1) O(5) N(2) 113.0(6) ? ? ? yes Os(1) N(1) C(5) 126.6(9) ? ? ? yes Os(1) N(1) C(9) 114.9(7) ? ? ? yes C(5) N(1) C(9) 118(1) ? ? ? yes Os(1) N(2) O(5) 124.2(6) ? ? ? yes Os(1) N(2) C(10) 118.2(7) ? ? ? yes O(5) N(2) C(10) 117.6(9) ? ? ? yes Os(1) C(1) O(1) 177(1) ? ? ? yes Os(1) C(2) O(2) 179(1) ? ? ? yes Os(2) C(3) O(3) 179(1) ? ? ? yes Os(2) C(4) O(4) 179(1) ? ? ? yes N(1) C(5) C(6) 121(1) ? ? ? yes C(5) C(6) C(7) 119(1) ? ? ? yes C(6) C(7) C(8) 119(1) ? ? ? yes C(7) C(8) C(9) 118(1) ? ? ? yes N(1) C(9) C(8) 122(1) ? ? ? yes N(1) C(9) C(10) 115.5(10) ? ? ? yes C(8) C(9) C(10) 122(1) ? ? ? yes N(2) C(10) C(9) 115.2(10) ? ? ? yes N(2) C(10) C(11) 121.3(10) ? ? ? yes C(9) C(10) C(11) 123.4(10) ? ? ? yes C(10) C(11) C(12) 121(1) ? ? ? yes C(10) C(11) C(16) 118(1) ? ? ? yes C(12) C(11) C(16) 119(1) ? ? ? yes C(11) C(12) C(13) 120(1) ? ? ? yes C(12) C(13) C(14) 121(1) ? ? ? yes C(13) C(14) C(15) 117(1) ? ? ? yes C(14) C(15) C(16) 121(1) ? ? ? yes C(11) C(16) C(15) 118(1) ? ? ? yes #------------------------------------------------------------------------------ #===============================end of file================================ data_wong930-JW003-compound 2 _database_code_CSD 174852 #------------------------------------------------------------------------------ _audit_creation_date 'Sun Sep 21 16:34:08 1997' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.982(2) _cell_length_b 16.596(6) _cell_length_c 8.586(4) _cell_angle_alpha 102.17(3) _cell_angle_beta 101.34(3) _cell_angle_gamma 92.27(2) _cell_volume 1358.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.4 _cell_measurement_theta_max 16.6 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.130 _exptl_crystal_density_diffrn 2.633 _exptl_crystal_density_meas ? _chemical_formula_weight 1076.94 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H10 N2 O12 Os3 ' _chemical_formula_moiety 'C23 H10 N2 O12 Os3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 972.00 _exptl_absorpt_coefficient_mu 14.052 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.414 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 250 _diffrn_standards_decay_% -3.27 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -2 3 -1 3 2 2 1 2 _diffrn_reflns_number 5075 _reflns_number_total 4776 _reflns_number_observed 3064 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 3.25 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.09472 _diffrn_orient_matrix_UB_12 -0.01764 _diffrn_orient_matrix_UB_13 0.02816 _diffrn_orient_matrix_UB_21 0.03907 _diffrn_orient_matrix_UB_22 0.05786 _diffrn_orient_matrix_UB_23 0.01120 _diffrn_orient_matrix_UB_31 -0.00409 _diffrn_orient_matrix_UB_32 0.01297 _diffrn_orient_matrix_UB_33 0.11803 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 6 -1.216 7.603 'International Tables' C 0 46 0.003 0.002 'International Tables' O 0 24 0.011 0.006 'International Tables' N 0 4 0.006 0.003 'International Tables' H 0 20 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) 0.25798(5) 0.79100(3) 0.60258(6) 0.0358(1) Uij ? ? Os(2) 0.54613(5) 0.81110(3) 0.76123(7) 0.0377(1) Uij ? ? Os(3) 0.83054(5) 0.82361(3) 0.93610(7) 0.0422(2) Uij ? ? O(1) -0.043(1) 0.7936(8) 0.442(1) 0.078(4) Uij ? ? O(2) 0.342(1) 0.9273(7) 0.442(1) 0.067(4) Uij ? ? O(3) 0.217(1) 0.9154(7) 0.901(1) 0.064(4) Uij ? ? O(4) 0.629(1) 0.811(1) 0.434(1) 0.101(5) Uij ? ? O(5) 0.548(1) 1.0017(7) 0.833(1) 0.074(4) Uij ? ? O(6) 0.459(1) 0.8040(8) 1.082(1) 0.080(4) Uij ? ? O(7) 0.561(1) 0.6246(8) 0.689(2) 0.104(5) Uij ? ? O(8) 0.866(1) 0.6780(8) 0.660(2) 0.085(5) Uij ? ? O(9) 0.896(1) 0.9647(9) 0.773(2) 0.091(5) Uij ? ? O(10) 0.742(1) 0.9306(8) 1.231(1) 0.077(4) Uij ? ? O(11) 1.112(1) 0.8201(8) 1.145(1) 0.080(4) Uij ? ? O(12) 0.1958(9) 0.7030(6) 0.851(1) 0.049(3) Uij ? ? N(1) 0.2882(10) 0.6868(7) 0.427(1) 0.040(3) Uij ? ? N(2) 0.2265(10) 0.6913(6) 0.710(1) 0.036(3) Uij ? ? C(1) 0.070(1) 0.7908(9) 0.502(2) 0.052(5) Uij ? ? C(2) 0.313(1) 0.877(1) 0.500(2) 0.057(5) Uij ? ? C(3) 0.235(1) 0.8694(8) 0.788(2) 0.042(4) Uij ? ? C(4) 0.600(1) 0.8132(10) 0.555(2) 0.056(5) Uij ? ? C(5) 0.547(1) 0.933(1) 0.811(2) 0.048(5) Uij ? ? C(6) 0.492(1) 0.8078(10) 0.967(2) 0.052(5) Uij ? ? C(7) 0.553(1) 0.6929(9) 0.715(2) 0.064(5) Uij ? ? C(8) 0.854(1) 0.7322(10) 0.760(2) 0.051(5) Uij ? ? C(9) 0.872(1) 0.912(1) 0.831(2) 0.056(5) Uij ? ? C(10) 0.772(2) 0.892(1) 1.119(2) 0.064(5) Uij ? ? C(11) 1.008(1) 0.8204(10) 1.062(2) 0.052(5) Uij ? ? C(12) 0.312(1) 0.6890(10) 0.276(2) 0.052(5) Uij ? ? C(13) 0.320(1) 0.617(1) 0.163(2) 0.056(5) Uij ? ? C(14) 0.301(2) 0.543(1) 0.202(2) 0.061(5) Uij ? ? C(15) 0.276(1) 0.5395(9) 0.350(2) 0.054(4) Uij ? ? C(16) 0.269(1) 0.6126(8) 0.465(2) 0.038(4) Uij ? ? C(17) 0.235(1) 0.6152(8) 0.623(1) 0.037(4) Uij ? ? C(18) 0.219(1) 0.5395(8) 0.687(2) 0.043(4) Uij ? ? C(19) 0.097(2) 0.523(1) 0.733(2) 0.072(6) Uij ? ? C(20) 0.083(2) 0.451(1) 0.792(2) 0.067(6) Uij ? ? C(21) 0.181(2) 0.398(1) 0.802(2) 0.072(6) Uij ? ? C(22) 0.299(2) 0.415(1) 0.751(2) 0.075(6) Uij ? ? C(23) 0.319(2) 0.4854(10) 0.698(2) 0.058(5) Uij ? ? H(1) 0.7959 0.7575 0.9968 0.0643 Uij ? ? H(2) 0.3241 0.7409 0.2484 0.0627 Uij ? ? H(3) 0.3380 0.6189 0.0593 0.0677 Uij ? ? H(4) 0.3046 0.4934 0.1245 0.0730 Uij ? ? H(5) 0.2639 0.4874 0.3768 0.0646 Uij ? ? H(6) 0.0256 0.5596 0.7258 0.0858 Uij ? ? H(7) 0.0009 0.4394 0.8259 0.0809 Uij ? ? H(8) 0.1684 0.3499 0.8429 0.0860 Uij ? ? H(9) 0.3678 0.3764 0.7525 0.0906 Uij ? ? H(10) 0.4038 0.4974 0.6694 0.0691 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0306(3) 0.0350(3) 0.0407(3) 0.0015(2) 0.0029(2) 0.0105(2) Os(2) 0.0305(3) 0.0374(3) 0.0433(3) -0.0001(2) 0.0015(2) 0.0112(2) Os(3) 0.0336(3) 0.0425(3) 0.0485(3) 0.0019(2) -0.0011(2) 0.0150(3) O(1) 0.035(6) 0.086(9) 0.105(9) 0.011(6) -0.001(6) 0.020(8) O(2) 0.064(7) 0.068(8) 0.077(8) -0.006(6) 0.010(6) 0.041(7) O(3) 0.060(7) 0.051(7) 0.074(8) 0.001(5) 0.014(6) -0.004(6) O(4) 0.083(9) 0.17(2) 0.058(8) 0.030(9) 0.032(7) 0.031(9) O(5) 0.083(8) 0.040(7) 0.092(9) 0.001(6) 0.010(7) 0.009(7) O(6) 0.077(8) 0.11(1) 0.062(8) -0.017(7) 0.014(6) 0.034(7) O(7) 0.058(8) 0.053(8) 0.18(2) 0.006(6) 0.012(8) 0.004(9) O(8) 0.062(8) 0.081(10) 0.098(10) 0.018(7) 0.006(7) -0.003(8) O(9) 0.088(9) 0.088(10) 0.12(1) 0.003(7) 0.031(8) 0.063(9) O(10) 0.092(9) 0.073(9) 0.059(7) 0.004(7) 0.017(7) -0.005(7) O(11) 0.061(7) 0.11(1) 0.062(7) 0.019(7) -0.012(6) 0.027(7) O(12) 0.063(6) 0.049(6) 0.033(5) -0.011(5) 0.016(4) 0.003(4) N(1) 0.033(6) 0.047(7) 0.038(6) 0.002(5) 0.003(5) 0.012(5) N(2) 0.033(6) 0.031(6) 0.043(6) 0.001(4) 0.010(5) 0.004(5) C(1) 0.040(8) 0.038(8) 0.08(1) 0.002(6) 0.021(8) 0.007(8) C(2) 0.045(9) 0.06(1) 0.07(1) 0.004(7) -0.006(7) 0.024(9) C(3) 0.044(8) 0.030(8) 0.044(8) 0.001(6) -0.001(6) 0.000(7) C(4) 0.040(8) 0.06(1) 0.059(10) 0.009(7) -0.005(7) 0.018(9) C(5) 0.043(8) 0.06(1) 0.046(9) -0.003(7) 0.012(6) 0.013(8) C(6) 0.037(8) 0.07(1) 0.054(9) 0.009(7) 0.011(7) 0.031(9) C(7) 0.040(8) 0.028(8) 0.12(1) -0.005(6) -0.011(8) 0.023(9) C(8) 0.032(7) 0.047(10) 0.08(1) 0.005(7) 0.001(7) 0.027(9) C(9) 0.040(8) 0.06(1) 0.059(10) -0.003(7) -0.008(7) 0.014(9) C(10) 0.055(10) 0.07(1) 0.06(1) -0.004(8) -0.006(8) 0.021(10) C(11) 0.041(8) 0.07(1) 0.044(8) 0.006(7) 0.000(7) 0.010(8) C(12) 0.043(8) 0.07(1) 0.050(9) 0.007(7) 0.007(7) 0.019(8) C(13) 0.061(10) 0.08(1) 0.026(7) 0.010(8) 0.009(6) 0.004(8) C(14) 0.06(1) 0.07(1) 0.037(9) 0.016(9) 0.003(7) -0.005(8) C(15) 0.058(9) 0.040(9) 0.048(9) 0.008(7) -0.010(7) -0.003(7) C(16) 0.023(6) 0.038(8) 0.047(8) 0.003(5) -0.004(5) 0.006(7) C(17) 0.045(7) 0.033(7) 0.026(6) -0.001(6) -0.007(5) 0.007(6) C(18) 0.036(7) 0.042(8) 0.048(8) -0.009(6) -0.003(6) 0.017(7) C(19) 0.057(10) 0.07(1) 0.09(1) -0.006(8) -0.005(9) 0.03(1) C(20) 0.048(9) 0.06(1) 0.09(1) -0.013(8) 0.006(8) 0.02(1) C(21) 0.09(1) 0.05(1) 0.07(1) -0.014(9) -0.020(9) 0.028(9) C(22) 0.09(1) 0.04(1) 0.09(1) 0.013(9) 0.00(1) 0.025(10) C(23) 0.063(10) 0.05(1) 0.056(9) 0.004(8) 0.011(8) 0.014(8) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3064 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0391 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0419 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.058 _refine_ls_shift/esd_max 0.0020 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.24 _refine_diff_density_max 0.90 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Os(2) 2.9038(8) ? ? yes Os(1) N(1) 2.11(1) ? ? yes Os(1) N(2) 2.10(1) ? ? yes Os(1) C(1) 1.90(1) ? ? yes Os(1) C(2) 1.94(2) ? ? yes Os(1) C(3) 1.89(1) ? ? yes Os(2) Os(3) 2.9159(8) ? ? yes Os(2) C(4) 1.96(2) ? ? yes Os(2) C(5) 1.98(2) ? ? yes Os(2) C(6) 1.96(1) ? ? yes Os(2) C(7) 1.92(2) ? ? yes Os(3) C(8) 1.96(2) ? ? yes Os(3) C(9) 1.95(2) ? ? yes Os(3) C(10) 1.94(2) ? ? yes Os(3) C(11) 1.90(1) ? ? yes Os(3) H(1) 1.370 ? ? no O(1) C(1) 1.16(2) ? ? yes O(2) C(2) 1.12(2) ? ? yes O(3) C(3) 1.15(2) ? ? yes O(4) C(4) 1.13(2) ? ? yes O(5) C(5) 1.11(2) ? ? yes O(6) C(6) 1.11(1) ? ? yes O(7) C(7) 1.12(2) ? ? yes O(8) C(8) 1.13(2) ? ? yes O(9) C(9) 1.13(2) ? ? yes O(10) C(10) 1.14(2) ? ? yes O(11) C(11) 1.14(1) ? ? yes O(12) N(2) 1.28(1) ? ? yes N(1) C(12) 1.37(2) ? ? yes N(1) C(16) 1.35(2) ? ? yes N(2) C(17) 1.34(2) ? ? yes C(12) C(13) 1.39(2) ? ? yes C(12) H(2) 0.950 ? ? no C(13) C(14) 1.34(2) ? ? yes C(13) H(3) 0.950 ? ? no C(14) C(15) 1.36(2) ? ? yes C(14) H(4) 0.950 ? ? no C(15) C(16) 1.41(2) ? ? yes C(15) H(5) 0.950 ? ? no C(16) C(17) 1.45(2) ? ? yes C(17) C(18) 1.49(2) ? ? yes C(18) C(19) 1.39(2) ? ? yes C(18) C(23) 1.37(2) ? ? yes C(19) C(20) 1.41(2) ? ? yes C(19) H(6) 0.950 ? ? no C(20) C(21) 1.35(2) ? ? yes C(20) H(7) 0.950 ? ? no C(21) C(22) 1.37(2) ? ? yes C(21) H(8) 0.950 ? ? no C(22) C(23) 1.37(2) ? ? yes C(22) H(9) 0.950 ? ? no C(23) H(10) 0.950 ? ? no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Os(2) Os(1) N(1) 91.8(3) ? ? ? yes Os(2) Os(1) N(2) 90.3(3) ? ? ? yes Os(2) Os(1) C(1) 173.7(4) ? ? ? yes Os(2) Os(1) C(2) 82.8(4) ? ? ? yes Os(2) Os(1) C(3) 84.9(4) ? ? ? yes N(1) Os(1) N(2) 76.5(4) ? ? ? yes N(1) Os(1) C(1) 92.9(5) ? ? ? yes N(1) Os(1) C(2) 98.5(6) ? ? ? yes N(1) Os(1) C(3) 168.4(5) ? ? ? yes N(2) Os(1) C(1) 94.9(5) ? ? ? yes N(2) Os(1) C(2) 171.4(5) ? ? ? yes N(2) Os(1) C(3) 92.4(5) ? ? ? yes C(1) Os(1) C(2) 92.3(6) ? ? ? yes C(1) Os(1) C(3) 91.2(6) ? ? ? yes C(2) Os(1) C(3) 92.2(6) ? ? ? yes Os(1) Os(2) Os(3) 175.79(2) ? ? ? yes Os(1) Os(2) C(4) 91.0(4) ? ? ? yes Os(1) Os(2) C(5) 92.0(4) ? ? ? yes Os(1) Os(2) C(6) 88.7(4) ? ? ? yes Os(1) Os(2) C(7) 90.3(4) ? ? ? yes Os(3) Os(2) C(4) 92.4(4) ? ? ? yes Os(3) Os(2) C(5) 90.4(4) ? ? ? yes Os(3) Os(2) C(6) 87.8(4) ? ? ? yes Os(3) Os(2) C(7) 87.3(4) ? ? ? yes C(4) Os(2) C(5) 90.1(6) ? ? ? yes C(4) Os(2) C(6) 179.4(7) ? ? ? yes C(4) Os(2) C(7) 89.1(7) ? ? ? yes C(5) Os(2) C(6) 90.5(6) ? ? ? yes C(5) Os(2) C(7) 177.6(6) ? ? ? yes C(6) Os(2) C(7) 90.3(7) ? ? ? yes Os(2) Os(3) C(8) 85.8(4) ? ? ? yes Os(2) Os(3) C(9) 89.2(4) ? ? ? yes Os(2) Os(3) C(10) 86.7(4) ? ? ? yes Os(2) Os(3) C(11) 172.5(5) ? ? ? yes Os(2) Os(3) H(1) 87.6 ? ? ? no C(8) Os(3) C(9) 96.2(6) ? ? ? yes C(8) Os(3) C(10) 164.7(6) ? ? ? yes C(8) Os(3) C(11) 93.4(6) ? ? ? yes C(8) Os(3) H(1) 79.9 ? ? ? no C(9) Os(3) C(10) 97.0(7) ? ? ? yes C(9) Os(3) C(11) 98.3(6) ? ? ? yes C(9) Os(3) H(1) 175.1 ? ? ? no C(10) Os(3) C(11) 92.3(6) ? ? ? yes C(10) Os(3) H(1) 86.5 ? ? ? no C(11) Os(3) H(1) 84.9 ? ? ? no Os(1) N(1) C(12) 125.0(10) ? ? ? yes Os(1) N(1) C(16) 115.6(8) ? ? ? yes C(12) N(1) C(16) 119(1) ? ? ? yes Os(1) N(2) O(12) 121.1(8) ? ? ? yes Os(1) N(2) C(17) 117.2(8) ? ? ? yes O(12) N(2) C(17) 121(1) ? ? ? yes Os(1) C(1) O(1) 177(1) ? ? ? yes Os(1) C(2) O(2) 177(1) ? ? ? yes Os(1) C(3) O(3) 177(1) ? ? ? yes Os(2) C(4) O(4) 177(1) ? ? ? yes Os(2) C(5) O(5) 177(1) ? ? ? yes Os(2) C(6) O(6) 178(1) ? ? ? yes Os(2) C(7) O(7) 178(1) ? ? ? yes Os(3) C(8) O(8) 177(1) ? ? ? yes Os(3) C(9) O(9) 178(1) ? ? ? yes Os(3) C(10) O(10) 176(1) ? ? ? yes Os(3) C(11) O(11) 176(1) ? ? ? yes N(1) C(12) C(13) 121(1) ? ? ? yes N(1) C(12) H(2) 119.4 ? ? ? no C(13) C(12) H(2) 119.4 ? ? ? no C(12) C(13) C(14) 119(1) ? ? ? yes C(12) C(13) H(3) 120.4 ? ? ? no C(14) C(13) H(3) 120.4 ? ? ? no C(13) C(14) C(15) 120(1) ? ? ? yes C(13) C(14) H(4) 119.8 ? ? ? no C(15) C(14) H(4) 119.8 ? ? ? no C(14) C(15) C(16) 120(1) ? ? ? yes C(14) C(15) H(5) 119.8 ? ? ? no C(16) C(15) H(5) 119.8 ? ? ? no N(1) C(16) C(15) 119(1) ? ? ? yes N(1) C(16) C(17) 115(1) ? ? ? yes C(15) C(16) C(17) 124(1) ? ? ? yes N(2) C(17) C(16) 114(1) ? ? ? yes N(2) C(17) C(18) 122(1) ? ? ? yes C(16) C(17) C(18) 122(1) ? ? ? yes C(17) C(18) C(19) 117(1) ? ? ? yes C(17) C(18) C(23) 122(1) ? ? ? yes C(19) C(18) C(23) 119(1) ? ? ? yes C(18) C(19) C(20) 117(1) ? ? ? yes C(18) C(19) H(6) 121.4 ? ? ? no C(20) C(19) H(6) 121.4 ? ? ? no C(19) C(20) C(21) 123(1) ? ? ? yes C(19) C(20) H(7) 118.5 ? ? ? no C(21) C(20) H(7) 118.5 ? ? ? no C(20) C(21) C(22) 118(1) ? ? ? yes C(20) C(21) H(8) 120.8 ? ? ? no C(22) C(21) H(8) 120.8 ? ? ? no C(21) C(22) C(23) 120(1) ? ? ? yes C(21) C(22) H(9) 119.7 ? ? ? no C(23) C(22) H(9) 119.7 ? ? ? no C(18) C(23) C(22) 120(1) ? ? ? yes C(18) C(23) H(10) 119.5 ? ? ? no C(22) C(23) H(10) 119.5 ? ? ? no #------------------------------------------------------------------------------ #==============================End of file============================= data_wt0214w-JW001-compound 3 _database_code_CSD 174853 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Sep 23 16:11:47 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 8.803(2) _cell_length_b 12.235(1) _cell_length_c 12.380(2) _cell_angle_alpha 81.46(2) _cell_angle_beta 71.34(1) _cell_angle_gamma 77.51(2) _cell_volume 1228.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.220 _exptl_crystal_density_diffrn 2.759 _exptl_crystal_density_meas ? _chemical_formula_weight 1020.92 _chemical_formula_analytical ? _chemical_formula_sum 'C21 H10 N2 O10 Os3 ' _chemical_formula_moiety 'C21 H10 N2 O10 Os3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 916.00 _exptl_absorpt_coefficient_mu 15.519 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 7606 _reflns_number_total 5278 _reflns_number_observed 4794 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 3.15 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 6 -1.216 7.603 'International Tables' N 0 4 0.006 0.003 'International Tables' C 0 42 0.003 0.002 'International Tables' O 0 20 0.011 0.006 'International Tables' H 0 20 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) 0.19466(4) 0.32425(3) 0.22191(3) 0.02826(10) Uij ? ? Os(2) 0.17732(5) 0.09677(3) 0.19909(3) 0.0337(1) Uij ? ? Os(3) -0.04341(4) 0.28012(3) 0.13150(3) 0.0304(1) Uij ? ? O(1) 0.152(1) 0.5762(7) 0.2078(8) 0.065(3) Uij ? ? O(2) 0.5308(10) 0.3174(9) 0.0471(8) 0.071(3) Uij ? ? O(3) -0.110(1) 0.0808(8) 0.4174(8) 0.070(3) Uij ? ? O(4) 0.434(1) 0.0051(9) 0.3228(10) 0.077(4) Uij ? ? O(5) 0.429(1) 0.1285(9) -0.0357(8) 0.084(3) Uij ? ? O(6) 0.106(2) -0.1071(10) 0.125(1) 0.095(4) Uij ? ? O(7) -0.263(1) 0.1117(9) 0.1565(9) 0.077(4) Uij ? ? O(8) -0.263(1) 0.4910(8) 0.0648(8) 0.069(3) Uij ? ? O(9) 0.133(1) 0.2394(10) -0.1154(7) 0.074(3) Uij ? ? O(10) -0.1532(8) 0.3217(6) 0.3071(5) 0.034(2) Uij ? ? N(1) 0.2539(9) 0.2881(7) 0.3757(7) 0.032(2) Uij ? ? N(2) -0.0247(9) 0.3215(6) 0.3439(6) 0.029(2) Uij ? ? C(1) 0.173(1) 0.4810(9) 0.2175(8) 0.039(3) Uij ? ? C(2) 0.403(1) 0.318(1) 0.1124(9) 0.045(3) Uij ? ? C(3) -0.003(1) 0.0898(9) 0.3380(9) 0.041(3) Uij ? ? C(4) 0.339(1) 0.0393(10) 0.273(1) 0.051(3) Uij ? ? C(5) 0.336(2) 0.1195(10) 0.0531(10) 0.053(3) Uij ? ? C(6) 0.129(2) -0.032(1) 0.152(1) 0.052(4) Uij ? ? C(7) -0.185(1) 0.1772(10) 0.1471(9) 0.044(3) Uij ? ? C(8) -0.181(1) 0.4124(10) 0.0916(9) 0.044(3) Uij ? ? C(9) 0.066(1) 0.2543(10) -0.0232(9) 0.042(3) Uij ? ? C(10) 0.404(1) 0.2623(10) 0.3870(9) 0.042(3) Uij ? ? C(11) 0.432(1) 0.239(1) 0.493(1) 0.053(4) Uij ? ? C(12) 0.297(2) 0.246(1) 0.5909(10) 0.051(3) Uij ? ? C(13) 0.145(1) 0.2736(9) 0.5808(9) 0.043(3) Uij ? ? C(14) 0.122(1) 0.2944(8) 0.4723(8) 0.033(2) Uij ? ? C(15) -0.035(1) 0.3166(8) 0.4515(8) 0.031(2) Uij ? ? C(16) -0.192(1) 0.3289(8) 0.5448(8) 0.033(2) Uij ? ? C(17) -0.231(1) 0.2442(9) 0.6304(8) 0.041(3) Uij ? ? C(18) -0.375(1) 0.260(1) 0.7199(10) 0.049(3) Uij ? ? C(19) -0.480(1) 0.361(1) 0.7232(10) 0.050(3) Uij ? ? C(20) -0.446(1) 0.4446(9) 0.637(1) 0.049(3) Uij ? ? C(21) -0.303(1) 0.4305(9) 0.5481(9) 0.040(3) Uij ? ? H(1) 0.4952 0.2597 0.3199 0.0498 Uij ? ? H(2) 0.5403 0.2194 0.4987 0.0638 Uij ? ? H(3) 0.3128 0.2313 0.6646 0.0617 Uij ? ? H(4) 0.0528 0.2789 0.6473 0.0514 Uij ? ? H(5) -0.1588 0.1741 0.6279 0.0493 Uij ? ? H(6) -0.4011 0.2006 0.7780 0.0590 Uij ? ? H(7) -0.5760 0.3738 0.7859 0.0602 Uij ? ? H(8) -0.5215 0.5130 0.6381 0.0593 Uij ? ? H(9) -0.2797 0.4894 0.4893 0.0480 Uij ? ? H(10) 0.0750 0.3574 0.1398 0.0515 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0272(2) 0.0352(2) 0.0222(2) -0.0091(1) -0.0061(1) 0.0001(1) Os(2) 0.0363(2) 0.0325(2) 0.0280(2) -0.0054(2) -0.0048(2) -0.0013(1) Os(3) 0.0312(2) 0.0392(2) 0.0221(2) -0.0090(2) -0.0087(1) -0.0011(1) O(1) 0.096(7) 0.036(4) 0.063(6) -0.006(4) -0.029(5) -0.006(4) O(2) 0.032(4) 0.108(8) 0.060(6) -0.017(5) -0.001(4) 0.007(5) O(3) 0.080(7) 0.065(6) 0.050(5) -0.027(5) 0.008(5) -0.003(4) O(4) 0.078(7) 0.070(6) 0.092(8) -0.008(5) -0.045(6) -0.001(6) O(5) 0.083(7) 0.072(6) 0.055(6) -0.004(5) 0.029(5) 0.003(5) O(6) 0.15(1) 0.076(7) 0.089(8) -0.049(7) -0.046(8) -0.020(6) O(7) 0.073(6) 0.084(7) 0.084(8) -0.036(6) -0.025(6) -0.004(6) O(8) 0.084(7) 0.057(5) 0.053(5) 0.008(5) -0.024(5) 0.007(4) O(9) 0.085(7) 0.115(8) 0.028(4) -0.038(6) -0.006(4) -0.015(5) O(10) 0.032(3) 0.048(4) 0.022(3) -0.003(3) -0.011(3) -0.003(3) N(1) 0.029(4) 0.042(4) 0.029(4) -0.005(3) -0.015(3) -0.004(3) N(2) 0.029(4) 0.037(4) 0.019(3) -0.006(3) -0.004(3) -0.001(3) C(1) 0.049(6) 0.047(6) 0.026(5) -0.013(5) -0.015(4) -0.003(4) C(2) 0.038(6) 0.064(7) 0.034(6) -0.016(5) -0.013(5) 0.007(5) C(3) 0.045(6) 0.043(6) 0.031(5) -0.013(5) -0.005(4) 0.006(4) C(4) 0.043(6) 0.041(6) 0.064(8) -0.004(5) -0.011(6) 0.000(5) C(5) 0.063(8) 0.046(6) 0.034(6) 0.000(5) 0.002(5) -0.006(5) C(6) 0.058(7) 0.056(7) 0.046(7) -0.019(6) -0.017(5) -0.003(5) C(7) 0.041(6) 0.057(7) 0.039(6) -0.021(5) -0.010(4) -0.009(5) C(8) 0.046(6) 0.053(6) 0.032(5) 0.000(5) -0.019(5) -0.003(5) C(9) 0.040(6) 0.060(7) 0.027(5) -0.021(5) -0.005(4) -0.002(5) C(10) 0.034(5) 0.061(7) 0.032(5) -0.013(5) -0.009(4) -0.004(5) C(11) 0.038(6) 0.084(9) 0.044(6) -0.013(6) -0.022(5) 0.000(6) C(12) 0.056(7) 0.072(8) 0.032(6) -0.016(6) -0.020(5) -0.001(5) C(13) 0.051(6) 0.051(6) 0.029(5) -0.012(5) -0.014(4) -0.002(4) C(14) 0.038(5) 0.034(5) 0.029(5) -0.005(4) -0.011(4) -0.005(4) C(15) 0.033(5) 0.035(5) 0.024(4) -0.003(4) -0.008(4) -0.002(4) C(16) 0.034(5) 0.039(5) 0.024(4) -0.012(4) -0.003(4) -0.005(4) C(17) 0.051(6) 0.044(6) 0.023(5) -0.012(5) -0.004(4) 0.002(4) C(18) 0.050(7) 0.054(7) 0.039(6) -0.018(6) -0.003(5) -0.002(5) C(19) 0.042(6) 0.063(7) 0.040(6) -0.015(5) 0.005(5) -0.016(5) C(20) 0.038(6) 0.041(6) 0.060(7) 0.005(5) -0.006(5) -0.012(5) C(21) 0.040(6) 0.039(5) 0.037(5) -0.008(4) -0.008(4) 0.001(4) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4794 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0433 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0549 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.813 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -3.23 _refine_diff_density_max 2.25 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Os(2) 2.8800(6) ? ? yes Os(1) Os(3) 2.8473(7) ? ? yes Os(1) N(1) 2.092(9) ? ? yes Os(1) N(2) 2.039(7) ? ? yes Os(1) C(1) 1.88(1) ? ? yes Os(1) C(2) 1.896(10) ? ? yes Os(2) Os(3) 2.8470(5) ? ? yes Os(2) C(3) 1.939(9) ? ? yes Os(2) C(4) 1.89(1) ? ? yes Os(2) C(5) 1.92(1) ? ? yes Os(2) C(6) 1.92(2) ? ? yes Os(3) O(10) 2.166(6) ? ? yes Os(3) C(7) 1.90(1) ? ? yes Os(3) C(8) 1.90(1) ? ? yes Os(3) C(9) 1.887(10) ? ? yes O(1) C(1) 1.13(1) ? ? yes O(2) C(2) 1.15(1) ? ? yes O(3) C(3) 1.13(1) ? ? yes O(4) C(4) 1.17(2) ? ? yes O(5) C(5) 1.15(1) ? ? yes O(6) C(6) 1.11(2) ? ? yes O(7) C(7) 1.13(2) ? ? yes O(8) C(8) 1.15(1) ? ? yes O(9) C(9) 1.13(1) ? ? yes O(10) N(2) 1.35(1) ? ? yes N(1) C(10) 1.34(1) ? ? yes N(1) C(14) 1.37(1) ? ? yes N(2) C(15) 1.30(1) ? ? yes C(10) C(11) 1.39(2) ? ? yes C(11) C(12) 1.40(1) ? ? yes C(12) C(13) 1.36(2) ? ? yes C(13) C(14) 1.40(2) ? ? yes C(14) C(15) 1.45(2) ? ? yes C(15) C(16) 1.48(1) ? ? yes C(16) C(17) 1.38(1) ? ? yes C(16) C(21) 1.40(1) ? ? yes C(17) C(18) 1.39(1) ? ? yes C(18) C(19) 1.38(2) ? ? yes C(19) C(20) 1.37(2) ? ? yes C(20) C(21) 1.38(1) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Os(2) Os(1) Os(3) 59.61(1) ? ? ? yes Os(2) Os(1) N(1) 95.6(2) ? ? ? yes Os(2) Os(1) N(2) 84.1(2) ? ? ? yes Os(2) Os(1) C(1) 167.2(4) ? ? ? yes Os(2) Os(1) C(2) 93.3(4) ? ? ? yes Os(3) Os(1) N(1) 137.4(2) ? ? ? yes Os(3) Os(1) N(2) 68.0(3) ? ? ? yes Os(3) Os(1) C(1) 107.8(4) ? ? ? yes Os(3) Os(1) C(2) 112.8(4) ? ? ? yes N(1) Os(1) N(2) 76.0(3) ? ? ? yes N(1) Os(1) C(1) 95.8(4) ? ? ? yes N(1) Os(1) C(2) 101.8(4) ? ? ? yes N(2) Os(1) C(1) 93.1(4) ? ? ? yes N(2) Os(1) C(2) 176.4(4) ? ? ? yes C(1) Os(1) C(2) 90.0(5) ? ? ? yes Os(1) Os(2) Os(3) 59.62(1) ? ? ? yes Os(1) Os(2) C(3) 93.1(3) ? ? ? yes Os(1) Os(2) C(4) 91.4(4) ? ? ? yes Os(1) Os(2) C(5) 83.5(4) ? ? ? yes Os(1) Os(2) C(6) 162.3(4) ? ? ? yes Os(3) Os(2) C(3) 83.1(3) ? ? ? yes Os(3) Os(2) C(4) 150.6(4) ? ? ? yes Os(3) Os(2) C(5) 89.1(4) ? ? ? yes Os(3) Os(2) C(6) 103.5(4) ? ? ? yes C(3) Os(2) C(4) 94.6(5) ? ? ? yes C(3) Os(2) C(5) 172.1(5) ? ? ? yes C(3) Os(2) C(6) 89.7(5) ? ? ? yes C(4) Os(2) C(5) 92.6(5) ? ? ? yes C(4) Os(2) C(6) 105.8(6) ? ? ? yes C(5) Os(2) C(6) 91.4(5) ? ? ? yes Os(1) Os(3) Os(2) 60.76(1) ? ? ? yes Os(1) Os(3) O(10) 69.4(2) ? ? ? yes Os(1) Os(3) C(7) 142.5(4) ? ? ? yes Os(1) Os(3) C(8) 113.4(4) ? ? ? yes Os(1) Os(3) C(9) 106.0(4) ? ? ? yes Os(2) Os(3) O(10) 90.8(2) ? ? ? yes Os(2) Os(3) C(7) 87.8(3) ? ? ? yes Os(2) Os(3) C(8) 174.2(4) ? ? ? yes Os(2) Os(3) C(9) 89.6(3) ? ? ? yes O(10) Os(3) C(7) 92.9(4) ? ? ? yes O(10) Os(3) C(8) 86.6(4) ? ? ? yes O(10) Os(3) C(9) 174.3(4) ? ? ? yes C(7) Os(3) C(8) 97.5(5) ? ? ? yes C(7) Os(3) C(9) 92.7(5) ? ? ? yes C(8) Os(3) C(9) 92.5(4) ? ? ? yes Os(3) O(10) N(2) 103.9(4) ? ? ? yes Os(1) N(1) C(10) 126.5(6) ? ? ? yes Os(1) N(1) C(14) 114.6(7) ? ? ? yes C(10) N(1) C(14) 118.9(9) ? ? ? yes Os(1) N(2) O(10) 116.8(5) ? ? ? yes Os(1) N(2) C(15) 120.3(7) ? ? ? yes O(10) N(2) C(15) 122.8(7) ? ? ? yes Os(1) C(1) O(1) 173(1) ? ? ? yes Os(1) C(2) O(2) 177(1) ? ? ? yes Os(2) C(3) O(3) 176(1) ? ? ? yes Os(2) C(4) O(4) 176(1) ? ? ? yes Os(2) C(5) O(5) 176(1) ? ? ? yes Os(2) C(6) O(6) 177(1) ? ? ? yes Os(3) C(7) O(7) 176(1) ? ? ? yes Os(3) C(8) O(8) 178(1) ? ? ? yes Os(3) C(9) O(9) 178(1) ? ? ? yes N(1) C(10) C(11) 122.6(9) ? ? ? yes C(10) C(11) C(12) 117(1) ? ? ? yes C(11) C(12) C(13) 120(1) ? ? ? yes C(12) C(13) C(14) 119.8(9) ? ? ? yes N(1) C(14) C(13) 120.6(10) ? ? ? yes N(1) C(14) C(15) 114.9(9) ? ? ? yes C(13) C(14) C(15) 124.4(8) ? ? ? yes N(2) C(15) C(14) 113.2(7) ? ? ? yes N(2) C(15) C(16) 123.9(9) ? ? ? yes C(14) C(15) C(16) 122.9(9) ? ? ? yes C(15) C(16) C(17) 122.3(8) ? ? ? yes C(15) C(16) C(21) 119.1(8) ? ? ? yes C(17) C(16) C(21) 118.6(8) ? ? ? yes C(16) C(17) C(18) 121.2(9) ? ? ? yes C(17) C(18) C(19) 119(1) ? ? ? yes C(18) C(19) C(20) 120.4(9) ? ? ? yes C(19) C(20) C(21) 120.8(10) ? ? ? yes C(16) C(21) C(20) 119.7(9) ? ? ? yes #------------------------------------------------------------------------------ #===============================end of file=============================== data_wt0265w-JW009-compound_4 _database_code_CSD 174854 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Sep 22 19:10:45 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 12.417(1) _cell_length_b 15.469(2) _cell_length_c 21.601(2) _cell_angle_alpha 77.57(1) _cell_angle_beta 82.77(2) _cell_angle_gamma 82.51(1) _cell_volume 3996.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.210 _exptl_crystal_density_diffrn 2.250 _exptl_crystal_density_meas ? _chemical_formula_weight 1354.20 _chemical_formula_analytical ? _chemical_formula_sum 'C33.50 H21.50 Cl4.50 N4 O9 Os3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2508.00 _exptl_absorpt_coefficient_mu 9.864 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 25032 _reflns_number_total 17331 _reflns_number_observed 10105 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 3.01 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.52 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 12 -1.216 7.603 'International Tables' N 0 16 0.006 0.003 'International Tables' C 0 134 0.003 0.002 'International Tables' O 0 36 0.011 0.006 'International Tables' Cl 0 18 0.148 0.159 'International Tables' H 0 86 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) 0.83773(4) 0.32155(4) 0.80210(3) 0.0434(2) Uij ? ? Os(2) 1.00540(4) 0.23759(4) 0.72511(3) 0.0468(2) Uij ? ? Os(3) 0.94096(4) 0.11019(4) 0.83319(3) 0.0428(2) Uij ? ? Os(4) 0.71416(4) 0.12853(4) 0.43927(3) 0.0450(2) Uij ? ? Os(5) 0.64127(5) 0.20732(4) 0.31714(3) 0.0541(2) Uij ? ? Os(6) 0.65258(5) 0.34486(4) 0.38217(3) 0.0492(2) Uij ? ? Cl(1) 0.4979(5) 0.7053(4) 0.9639(3) 0.145(3) Uij ? ? Cl(2) 0.4883(9) 0.8476(6) 0.8606(4) 0.257(5) Uij ? ? Cl(3) 0.6453(7) 0.8349(7) 0.9427(5) 0.238(5) Uij ? ? Cl(4) 0.7268(5) 0.6405(5) 0.7416(3) 0.161(3) Uij ? ? Cl(5) 0.8316(6) 0.7846(4) 0.7663(3) 0.160(3) Uij ? ? Cl(6) 0.8287(5) 0.6210(4) 0.8540(3) 0.133(3) Uij ? ? Cl(7) 1.086(1) 0.4555(10) 0.9293(5) 0.374(9) Uij ? ? Cl(8) 1.1655(8) 0.5970(5) 0.8622(3) 0.205(4) Uij ? ? Cl(9) 1.290(1) 0.438(1) 0.8857(10) 0.52(1) Uij ? ? O(1) 0.7025(9) 0.3828(8) 0.6923(5) 0.092(4) Uij ? ? O(2) 0.9624(10) 0.4829(8) 0.7619(6) 0.105(5) Uij ? ? O(3) 1.1524(8) 0.2878(9) 0.8142(6) 0.090(5) Uij ? ? O(4) 0.8145(9) 0.1857(7) 0.6679(5) 0.081(4) Uij ? ? O(5) 1.1755(9) 0.1048(8) 0.6710(6) 0.097(5) Uij ? ? O(6) 1.0340(10) 0.4034(8) 0.6219(6) 0.100(5) Uij ? ? O(7) 0.8989(10) -0.0180(8) 0.7565(5) 0.088(5) Uij ? ? O(8) 1.1734(8) 0.0207(7) 0.8368(5) 0.075(4) Uij ? ? O(9) 0.9720(6) 0.1920(6) 0.8956(4) 0.052(3) Uij ? ? O(10) 0.5929(10) -0.0275(8) 0.4367(6) 0.097(5) Uij ? ? O(11) 0.9220(9) 0.0367(9) 0.3873(6) 0.110(5) Uij ? ? O(12) 0.6382(10) 0.0364(9) 0.2718(6) 0.097(5) Uij ? ? O(13) 0.4130(9) 0.1917(9) 0.3909(6) 0.091(5) Uij ? ? O(14) 0.8863(10) 0.226(1) 0.2825(6) 0.115(6) Uij ? ? O(15) 0.560(1) 0.3382(9) 0.2009(6) 0.114(6) Uij ? ? O(16) 0.803(1) 0.4483(10) 0.2821(6) 0.125(6) Uij ? ? O(17) 0.461(1) 0.4538(8) 0.3205(6) 0.103(5) Uij ? ? O(18) 0.5462(6) 0.2831(6) 0.4572(4) 0.046(3) Uij ? ? N(1) 0.7309(8) 0.3804(7) 0.8721(5) 0.046(3) Uij ? ? N(2) 0.9040(8) 0.2674(7) 0.8896(5) 0.047(4) Uij ? ? N(3) 0.8497(8) 0.0497(7) 0.9186(5) 0.044(3) Uij ? ? N(4) 0.7851(7) 0.1894(6) 0.8270(4) 0.037(3) Uij ? ? N(5) 0.7302(8) 0.0790(7) 0.5382(5) 0.048(3) Uij ? ? N(6) 0.5923(7) 0.2035(7) 0.4874(5) 0.036(3) Uij ? ? N(7) 0.6812(9) 0.4118(8) 0.4535(5) 0.057(4) Uij ? ? N(8) 0.7790(8) 0.2548(7) 0.4276(5) 0.049(4) Uij ? ? C(1) 0.756(1) 0.3610(10) 0.7328(6) 0.058(5) Uij ? ? C(2) 0.912(1) 0.422(1) 0.7781(7) 0.064(5) Uij ? ? C(3) 1.097(1) 0.2690(10) 0.7826(8) 0.062(5) Uij ? ? C(4) 0.885(1) 0.2042(9) 0.6889(7) 0.057(5) Uij ? ? C(5) 1.113(1) 0.152(1) 0.6917(7) 0.059(5) Uij ? ? C(6) 1.024(1) 0.341(1) 0.6593(8) 0.064(5) Uij ? ? C(7) 0.914(1) 0.0346(10) 0.7868(7) 0.058(5) Uij ? ? C(8) 1.084(1) 0.0535(9) 0.8380(5) 0.044(4) Uij ? ? C(9) 0.643(1) 0.4397(9) 0.8625(7) 0.053(5) Uij ? ? C(10) 0.596(1) 0.491(1) 0.9036(8) 0.068(5) Uij ? ? C(11) 0.640(1) 0.479(1) 0.9608(7) 0.066(5) Uij ? ? C(12) 0.729(1) 0.4180(10) 0.9734(7) 0.060(5) Uij ? ? C(13) 0.7719(10) 0.3678(8) 0.9300(6) 0.039(4) Uij ? ? C(14) 0.860(1) 0.2980(9) 0.9405(6) 0.048(4) Uij ? ? C(15) 0.893(1) 0.2568(9) 1.0060(6) 0.051(5) Uij ? ? C(16) 0.999(1) 0.253(1) 1.0205(8) 0.072(6) Uij ? ? C(17) 1.025(2) 0.218(1) 1.0825(9) 0.087(7) Uij ? ? C(18) 0.944(2) 0.187(1) 1.1284(8) 0.083(7) Uij ? ? C(19) 0.841(1) 0.189(1) 1.1137(8) 0.081(6) Uij ? ? C(20) 0.815(1) 0.226(1) 1.0525(7) 0.061(5) Uij ? ? C(21) 0.889(1) -0.0209(9) 0.9616(7) 0.051(4) Uij ? ? C(22) 0.831(1) -0.056(1) 1.0162(7) 0.068(5) Uij ? ? C(23) 0.728(1) -0.021(1) 1.0292(7) 0.068(6) Uij ? ? C(24) 0.681(1) 0.053(1) 0.9862(7) 0.065(5) Uij ? ? C(25) 0.748(1) 0.0855(9) 0.9302(6) 0.047(4) Uij ? ? C(26) 0.7020(10) 0.1673(8) 0.8852(6) 0.044(4) Uij ? ? C(27) 0.5959(10) 0.1554(10) 0.8628(6) 0.048(4) Uij ? ? C(28) 0.511(1) 0.221(1) 0.8652(7) 0.068(6) Uij ? ? C(29) 0.413(1) 0.214(1) 0.841(1) 0.106(8) Uij ? ? C(30) 0.405(1) 0.145(1) 0.8115(8) 0.081(7) Uij ? ? C(31) 0.490(1) 0.081(1) 0.8096(7) 0.077(6) Uij ? ? C(32) 0.585(1) 0.087(1) 0.8344(7) 0.068(6) Uij ? ? C(33) 0.639(1) 0.031(1) 0.4391(7) 0.058(5) Uij ? ? C(34) 0.840(1) 0.0727(10) 0.4044(7) 0.059(5) Uij ? ? C(35) 0.641(1) 0.102(1) 0.2896(8) 0.077(6) Uij ? ? C(36) 0.499(1) 0.201(1) 0.3615(8) 0.070(6) Uij ? ? C(37) 0.793(2) 0.218(1) 0.2939(7) 0.082(6) Uij ? ? C(38) 0.590(1) 0.289(1) 0.2442(8) 0.079(7) Uij ? ? C(39) 0.743(2) 0.407(1) 0.3204(8) 0.079(7) Uij ? ? C(40) 0.531(1) 0.4129(10) 0.3452(8) 0.069(6) Uij ? ? C(41) 0.801(1) 0.0132(10) 0.5633(7) 0.060(5) Uij ? ? C(42) 0.790(2) -0.031(1) 0.6268(10) 0.090(7) Uij ? ? C(43) 0.699(1) -0.010(1) 0.6651(8) 0.077(6) Uij ? ? C(44) 0.627(1) 0.0618(10) 0.6410(7) 0.058(5) Uij ? ? C(45) 0.6451(10) 0.1048(8) 0.5773(6) 0.040(4) Uij ? ? C(46) 0.5723(10) 0.1815(8) 0.5499(6) 0.043(4) Uij ? ? C(47) 0.493(1) 0.2340(8) 0.5881(6) 0.042(4) Uij ? ? C(48) 0.385(1) 0.243(1) 0.5777(7) 0.061(5) Uij ? ? C(49) 0.311(1) 0.293(1) 0.6143(10) 0.088(7) Uij ? ? C(50) 0.343(2) 0.329(1) 0.6588(10) 0.088(7) Uij ? ? C(51) 0.453(2) 0.318(1) 0.6691(7) 0.083(7) Uij ? ? C(52) 0.526(1) 0.272(1) 0.6322(7) 0.063(5) Uij ? ? C(53) 0.629(1) 0.491(1) 0.4636(7) 0.070(6) Uij ? ? C(54) 0.646(1) 0.5316(10) 0.5111(7) 0.068(6) Uij ? ? C(55) 0.723(2) 0.488(1) 0.5522(8) 0.077(6) Uij ? ? C(56) 0.779(1) 0.408(1) 0.5421(7) 0.062(5) Uij ? ? C(57) 0.756(1) 0.3711(10) 0.4930(7) 0.054(5) Uij ? ? C(58) 0.814(1) 0.2804(10) 0.4851(6) 0.055(5) Uij ? ? C(59) 0.937(1) 0.278(1) 0.4801(7) 0.054(5) Uij ? ? C(60) 0.987(1) 0.343(1) 0.4355(9) 0.094(7) Uij ? ? C(61) 1.104(2) 0.340(2) 0.427(1) 0.14(1) Uij ? ? C(62) 1.160(2) 0.266(2) 0.460(2) 0.15(2) Uij ? ? C(63) 1.110(2) 0.200(2) 0.506(1) 0.13(1) Uij ? ? C(64) 1.000(1) 0.210(1) 0.5142(8) 0.076(6) Uij ? ? C(65) 0.5692 0.7728 0.9079 0.1018 Uij ? ? C(66) 0.8314 0.6737 0.7762 0.0876 Uij ? ? C(67) 1.1726 0.4851 0.8711 0.1035 Uij ? ? H(1) 0.6100 0.4459 0.8223 0.0641 Uij ? ? H(2) 0.5337 0.5347 0.8932 0.0799 Uij ? ? H(3) 0.6073 0.5146 0.9928 0.0762 Uij ? ? H(4) 0.7628 0.4104 1.0134 0.0728 Uij ? ? H(5) 1.0560 0.2756 0.9871 0.0871 Uij ? ? H(6) 1.1002 0.2138 1.0934 0.1017 Uij ? ? H(7) 0.9608 0.1638 1.1722 0.0987 Uij ? ? H(8) 0.7843 0.1645 1.1471 0.0970 Uij ? ? H(9) 0.7398 0.2278 1.0426 0.0728 Uij ? ? H(10) 0.9633 -0.0471 0.9528 0.0595 Uij ? ? H(11) 0.8627 -0.1068 1.0460 0.0770 Uij ? ? H(12) 0.6852 -0.0459 1.0690 0.0782 Uij ? ? H(13) 0.6048 0.0784 0.9948 0.0796 Uij ? ? H(14) 0.5172 0.2713 0.8852 0.0843 Uij ? ? H(15) 0.3500 0.2599 0.8431 0.1244 Uij ? ? H(16) 0.3393 0.1409 0.7919 0.0958 Uij ? ? H(17) 0.4844 0.0284 0.7913 0.0900 Uij ? ? H(18) 0.6474 0.0401 0.8317 0.0812 Uij ? ? H(19) 0.8652 -0.0057 0.5356 0.0712 Uij ? ? H(20) 0.8454 -0.0764 0.6451 0.1021 Uij ? ? H(21) 0.6852 -0.0447 0.7094 0.0916 Uij ? ? H(22) 0.5639 0.0828 0.6678 0.0679 Uij ? ? H(23) 0.3605 0.2162 0.5453 0.0743 Uij ? ? H(24) 0.2328 0.3004 0.6075 0.1045 Uij ? ? H(25) 0.2892 0.3627 0.6834 0.1048 Uij ? ? H(26) 0.4754 0.3450 0.7021 0.0992 Uij ? ? H(27) 0.6040 0.2656 0.6378 0.0754 Uij ? ? H(28) 0.5738 0.5229 0.4347 0.0816 Uij ? ? H(29) 0.6048 0.5881 0.5176 0.0803 Uij ? ? H(30) 0.7361 0.5131 0.5888 0.0932 Uij ? ? H(31) 0.8366 0.3783 0.5693 0.0725 Uij ? ? H(32) 0.9416 0.3910 0.4090 0.1097 Uij ? ? H(33) 1.1404 0.3905 0.3999 0.1567 Uij ? ? H(34) 1.2383 0.2606 0.4508 0.1740 Uij ? ? H(35) 1.1518 0.1491 0.5321 0.1535 Uij ? ? H(36) 0.9616 0.1642 0.5468 0.0904 Uij ? ? H(38) 0.6906 0.2181 0.9070 0.0552 Uij ? ? H(40) 0.7915 0.2354 0.5222 0.0662 Uij ? ? H(41) 0.6174 0.7383 0.8826 0.1221 Uij ? ? H(42) 0.8985 0.6523 0.7555 0.1051 Uij ? ? H(43) 1.1528 0.4706 0.8337 0.1242 Uij ? ? H(44) 0.7576 0.1804 0.7946 0.0449 Uij ? ? H(45) 0.8352 0.2544 0.4000 0.0590 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0379(3) 0.0448(4) 0.0445(3) 0.0009(2) -0.0051(2) -0.0055(3) Os(2) 0.0383(3) 0.0516(4) 0.0472(3) -0.0015(3) -0.0003(3) -0.0070(3) Os(3) 0.0402(3) 0.0447(4) 0.0428(3) 0.0003(2) -0.0093(2) -0.0072(3) Os(4) 0.0390(3) 0.0494(4) 0.0498(3) 0.0005(2) -0.0097(3) -0.0173(3) Os(5) 0.0510(3) 0.0716(5) 0.0452(4) -0.0052(3) -0.0105(3) -0.0215(3) Os(6) 0.0574(4) 0.0525(4) 0.0389(3) -0.0097(3) -0.0097(3) -0.0066(3) Cl(1) 0.133(5) 0.104(5) 0.183(6) -0.002(4) 0.005(4) -0.015(4) Cl(2) 0.37(1) 0.185(9) 0.228(9) -0.088(9) -0.137(9) 0.036(8) Cl(3) 0.185(8) 0.29(1) 0.29(1) -0.112(8) -0.024(7) -0.120(10) Cl(4) 0.139(5) 0.199(7) 0.143(6) -0.044(5) -0.049(4) 0.003(5) Cl(5) 0.184(7) 0.092(5) 0.190(7) -0.021(4) -0.043(5) 0.021(4) Cl(6) 0.164(6) 0.104(5) 0.127(5) -0.013(4) -0.031(4) -0.006(4) Cl(7) 0.55(2) 0.38(2) 0.21(1) -0.29(2) 0.05(1) 0.00(1) Cl(8) 0.37(1) 0.154(7) 0.110(5) -0.078(7) -0.015(6) -0.037(5) Cl(9) 0.32(1) 0.46(2) 0.98(4) 0.27(1) -0.44(2) -0.55(2) O(1) 0.109(9) 0.099(10) 0.064(8) 0.038(7) -0.049(7) -0.011(7) O(2) 0.097(10) 0.061(9) 0.14(1) -0.022(7) 0.023(8) -0.004(8) O(3) 0.051(7) 0.14(1) 0.095(9) -0.023(7) -0.023(6) -0.037(8) O(4) 0.081(8) 0.090(9) 0.080(8) -0.030(7) -0.031(7) -0.010(7) O(5) 0.090(9) 0.086(10) 0.11(1) 0.031(7) 0.011(7) -0.042(8) O(6) 0.096(9) 0.079(10) 0.10(1) -0.011(7) -0.014(7) 0.031(8) O(7) 0.13(1) 0.064(8) 0.075(8) -0.003(7) -0.023(7) -0.026(7) O(8) 0.058(7) 0.084(9) 0.077(8) 0.016(6) -0.012(6) -0.013(6) O(9) 0.043(5) 0.056(6) 0.060(6) 0.006(5) -0.019(4) -0.016(5) O(10) 0.103(10) 0.085(10) 0.12(1) -0.040(8) -0.024(8) -0.027(8) O(11) 0.061(8) 0.14(1) 0.14(1) 0.006(8) 0.022(8) -0.079(10) O(12) 0.104(10) 0.10(1) 0.11(1) -0.001(8) -0.030(8) -0.060(9) O(13) 0.051(7) 0.13(1) 0.095(9) -0.013(7) -0.004(6) -0.040(8) O(14) 0.061(8) 0.19(2) 0.096(10) -0.021(9) 0.012(7) -0.049(10) O(15) 0.14(1) 0.12(1) 0.078(9) -0.008(9) -0.036(9) 0.011(8) O(16) 0.16(1) 0.14(1) 0.082(10) -0.08(1) 0.027(9) -0.004(9) O(17) 0.13(1) 0.081(9) 0.095(10) 0.031(8) -0.059(8) -0.003(7) O(18) 0.053(5) 0.048(6) 0.039(5) 0.005(4) -0.014(4) -0.010(4) N(1) 0.039(6) 0.050(8) 0.048(7) 0.001(5) 0.002(5) -0.015(6) N(2) 0.037(6) 0.051(8) 0.055(8) 0.001(5) -0.009(5) -0.019(6) N(3) 0.043(6) 0.049(7) 0.040(6) -0.003(5) -0.010(5) -0.003(5) N(4) 0.041(6) 0.047(7) 0.026(5) -0.007(5) -0.006(4) -0.008(5) N(5) 0.051(7) 0.035(7) 0.055(7) 0.006(5) -0.019(6) -0.003(6) N(6) 0.023(5) 0.039(7) 0.048(7) -0.001(4) -0.016(5) -0.004(5) N(7) 0.064(8) 0.049(8) 0.052(8) -0.008(6) -0.012(6) 0.007(6) N(8) 0.046(6) 0.055(8) 0.052(7) -0.005(5) -0.006(5) -0.023(6) C(1) 0.054(9) 0.07(1) 0.037(8) 0.009(8) 0.001(7) 0.001(8) C(2) 0.08(1) 0.05(1) 0.06(1) 0.006(8) -0.008(9) -0.010(8) C(3) 0.046(9) 0.06(1) 0.08(1) -0.006(7) 0.010(8) -0.023(9) C(4) 0.061(10) 0.045(10) 0.06(1) 0.003(8) -0.008(8) -0.013(8) C(5) 0.059(10) 0.05(1) 0.06(1) -0.011(8) -0.009(8) 0.002(8) C(6) 0.039(8) 0.05(1) 0.11(1) -0.010(7) 0.000(9) -0.023(10) C(7) 0.058(9) 0.05(1) 0.054(10) 0.024(8) -0.007(7) 0.004(8) C(8) 0.058(9) 0.054(9) 0.022(7) -0.003(7) -0.003(6) -0.015(6) C(9) 0.046(8) 0.054(10) 0.057(10) -0.002(7) -0.003(7) -0.011(8) C(10) 0.060(10) 0.07(1) 0.06(1) 0.022(8) 0.004(8) -0.011(9) C(11) 0.07(1) 0.06(1) 0.07(1) 0.011(8) -0.004(9) -0.015(8) C(12) 0.07(1) 0.051(10) 0.059(10) 0.008(8) -0.001(8) -0.024(8) C(13) 0.045(7) 0.032(8) 0.039(8) -0.012(6) -0.004(6) -0.003(6) C(14) 0.046(8) 0.059(10) 0.046(9) -0.013(7) -0.011(7) -0.014(7) C(15) 0.053(9) 0.058(10) 0.049(9) -0.003(7) -0.022(7) -0.020(7) C(16) 0.07(1) 0.06(1) 0.09(1) -0.013(8) -0.011(10) -0.024(10) C(17) 0.10(1) 0.10(2) 0.07(1) 0.01(1) -0.06(1) -0.03(1) C(18) 0.11(2) 0.08(1) 0.05(1) 0.02(1) -0.01(1) -0.015(10) C(19) 0.08(1) 0.08(1) 0.07(1) 0.02(1) -0.01(1) -0.01(1) C(20) 0.060(10) 0.07(1) 0.048(9) -0.002(8) 0.000(8) -0.010(8) C(21) 0.047(8) 0.049(9) 0.052(9) -0.001(7) -0.006(7) -0.002(7) C(22) 0.08(1) 0.06(1) 0.045(10) 0.011(9) -0.020(9) 0.016(8) C(23) 0.10(1) 0.06(1) 0.039(9) -0.023(10) -0.005(9) 0.012(8) C(24) 0.060(10) 0.09(1) 0.044(9) -0.011(9) -0.002(8) -0.015(9) C(25) 0.048(8) 0.060(10) 0.034(8) -0.009(7) -0.007(6) -0.006(7) C(26) 0.044(8) 0.043(8) 0.045(8) -0.001(6) -0.016(6) 0.000(6) C(27) 0.034(7) 0.058(10) 0.045(9) -0.004(7) -0.008(6) 0.006(7) C(28) 0.06(1) 0.07(1) 0.08(1) -0.020(9) -0.022(9) -0.006(9) C(29) 0.04(1) 0.13(2) 0.14(2) 0.01(1) -0.03(1) -0.01(2) C(30) 0.042(9) 0.11(2) 0.07(1) -0.03(1) -0.025(9) 0.03(1) C(31) 0.09(1) 0.10(1) 0.06(1) -0.06(1) -0.011(10) -0.011(10) C(32) 0.07(1) 0.08(1) 0.07(1) -0.020(9) -0.021(9) -0.020(9) C(33) 0.06(1) 0.06(1) 0.045(9) 0.005(8) -0.002(7) -0.018(8) C(34) 0.050(9) 0.06(1) 0.07(1) -0.006(8) -0.009(8) -0.030(9) C(35) 0.051(9) 0.12(2) 0.06(1) 0.00(1) -0.013(8) -0.03(1) C(36) 0.07(1) 0.08(1) 0.07(1) -0.002(9) -0.034(9) -0.034(10) C(37) 0.09(1) 0.12(2) 0.034(9) 0.01(1) -0.003(9) -0.023(9) C(38) 0.11(1) 0.07(1) 0.06(1) -0.01(1) -0.02(1) -0.013(10) C(39) 0.11(1) 0.08(1) 0.05(1) -0.01(1) -0.03(1) -0.022(10) C(40) 0.10(1) 0.029(9) 0.07(1) -0.004(9) -0.023(10) -0.006(8) C(41) 0.068(10) 0.044(10) 0.07(1) 0.005(8) -0.012(8) -0.014(8) C(42) 0.10(1) 0.06(1) 0.10(2) 0.01(1) -0.06(1) 0.00(1) C(43) 0.09(1) 0.06(1) 0.08(1) 0.004(10) -0.03(1) -0.005(10) C(44) 0.046(8) 0.06(1) 0.057(10) 0.003(7) -0.005(7) -0.006(8) C(45) 0.047(8) 0.034(8) 0.038(8) 0.002(6) -0.009(6) -0.009(6) C(46) 0.043(7) 0.042(9) 0.049(9) -0.008(6) -0.012(7) -0.013(7) C(47) 0.049(8) 0.025(7) 0.049(9) -0.005(6) 0.005(7) -0.006(6) C(48) 0.041(8) 0.07(1) 0.07(1) -0.015(8) 0.016(8) -0.014(9) C(49) 0.05(1) 0.09(2) 0.11(2) -0.010(10) 0.01(1) -0.01(1) C(50) 0.08(1) 0.06(1) 0.10(2) 0.01(1) 0.04(1) 0.00(1) C(51) 0.13(2) 0.08(1) 0.043(10) -0.01(1) 0.01(1) -0.026(9) C(52) 0.07(1) 0.07(1) 0.06(1) 0.004(8) -0.016(8) -0.018(9) C(53) 0.10(1) 0.04(1) 0.06(1) -0.014(9) -0.029(9) 0.011(8) C(54) 0.11(1) 0.040(10) 0.05(1) 0.004(9) -0.010(9) -0.012(8) C(55) 0.12(2) 0.05(1) 0.06(1) -0.02(1) -0.01(1) -0.007(9) C(56) 0.07(1) 0.07(1) 0.06(1) 0.002(8) -0.020(8) -0.025(9) C(57) 0.058(9) 0.051(10) 0.056(10) -0.018(7) -0.015(7) -0.007(8) C(58) 0.059(9) 0.06(1) 0.053(9) -0.025(8) -0.006(7) -0.008(8) C(59) 0.039(8) 0.07(1) 0.06(1) -0.017(8) -0.018(7) -0.020(8) C(60) 0.05(1) 0.13(2) 0.10(1) -0.03(1) -0.022(10) 0.00(1) C(61) 0.10(2) 0.23(3) 0.11(2) -0.10(2) 0.01(1) -0.03(2) C(62) 0.08(2) 0.20(4) 0.19(3) 0.03(2) -0.05(2) -0.08(3) C(63) 0.08(2) 0.18(3) 0.15(3) 0.05(2) -0.06(2) -0.09(2) C(64) 0.06(1) 0.10(1) 0.08(1) 0.002(10) -0.014(9) -0.05(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 10105 _refine_ls_number_parameters 946 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0484 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0447 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.932 _refine_ls_shift/esd_max 0.0030 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.46 _refine_diff_density_max 0.80 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Os(2) 2.8531(8) ? ? yes Os(1) N(1) 2.16(1) ? ? yes Os(1) N(2) 2.12(1) ? ? yes Os(1) N(4) 2.16(1) ? ? yes Os(1) C(1) 1.87(1) ? ? yes Os(1) C(2) 1.86(2) ? ? yes Os(2) Os(3) 2.8170(8) ? ? yes Os(2) C(3) 1.96(2) ? ? yes Os(2) C(4) 1.95(2) ? ? yes Os(2) C(5) 1.94(1) ? ? yes Os(2) C(6) 1.91(2) ? ? yes Os(3) O(9) 2.14(1) ? ? yes Os(3) N(3) 2.138(9) ? ? yes Os(3) N(4) 2.155(9) ? ? yes Os(3) C(7) 1.78(2) ? ? yes Os(3) C(8) 1.88(1) ? ? yes Os(4) Os(5) 2.8624(8) ? ? yes Os(4) N(5) 2.13(1) ? ? yes Os(4) N(6) 2.093(9) ? ? yes Os(4) N(8) 2.16(1) ? ? yes Os(4) C(33) 1.88(2) ? ? yes Os(4) C(34) 1.84(1) ? ? yes Os(5) Os(6) 2.817(1) ? ? yes Os(5) C(35) 1.86(2) ? ? yes Os(5) C(36) 1.90(2) ? ? yes Os(5) C(37) 1.91(2) ? ? yes Os(5) C(38) 1.91(2) ? ? yes Os(6) O(18) 2.099(8) ? ? yes Os(6) N(7) 2.12(1) ? ? yes Os(6) N(8) 2.144(10) ? ? yes Os(6) C(39) 1.82(2) ? ? yes Os(6) C(40) 1.88(2) ? ? yes Cl(1) C(65) 1.663(6) ? ? yes Cl(2) C(65) 1.685(10) ? ? yes Cl(3) C(65) 1.76(1) ? ? yes Cl(4) C(66) 1.758(8) ? ? yes Cl(5) C(66) 1.683(6) ? ? yes Cl(6) C(66) 1.701(6) ? ? yes Cl(7) C(67) 1.58(1) ? ? yes Cl(8) C(67) 1.692(8) ? ? yes Cl(9) C(67) 1.58(1) ? ? yes O(1) C(1) 1.13(2) ? ? yes O(2) C(2) 1.16(2) ? ? yes O(3) C(3) 1.13(2) ? ? yes O(4) C(4) 1.12(2) ? ? yes O(5) C(5) 1.11(2) ? ? yes O(6) C(6) 1.13(2) ? ? yes O(7) C(7) 1.19(2) ? ? yes O(8) C(8) 1.16(2) ? ? yes O(9) N(2) 1.34(1) ? ? yes O(10) C(33) 1.15(2) ? ? yes O(11) C(34) 1.15(2) ? ? yes O(12) C(35) 1.16(3) ? ? yes O(13) C(36) 1.18(2) ? ? yes O(14) C(37) 1.17(2) ? ? yes O(15) C(38) 1.14(2) ? ? yes O(16) C(39) 1.18(2) ? ? yes O(17) C(40) 1.12(2) ? ? yes O(18) N(6) 1.35(1) ? ? yes N(1) C(9) 1.34(2) ? ? yes N(1) C(13) 1.38(2) ? ? yes N(2) C(14) 1.32(2) ? ? yes N(3) C(21) 1.35(2) ? ? yes N(3) C(25) 1.33(2) ? ? yes N(4) C(26) 1.53(1) ? ? yes N(5) C(41) 1.32(2) ? ? yes N(5) C(45) 1.34(2) ? ? yes N(6) C(46) 1.32(2) ? ? yes N(7) C(53) 1.36(2) ? ? yes N(7) C(57) 1.35(2) ? ? yes N(8) C(58) 1.51(2) ? ? yes C(9) C(10) 1.34(2) ? ? yes C(10) C(11) 1.38(2) ? ? yes C(11) C(12) 1.38(2) ? ? yes C(12) C(13) 1.36(2) ? ? yes C(13) C(14) 1.44(2) ? ? yes C(14) C(15) 1.50(2) ? ? yes C(15) C(16) 1.39(2) ? ? yes C(15) C(20) 1.35(2) ? ? yes C(16) C(17) 1.39(3) ? ? yes C(17) C(18) 1.37(3) ? ? yes C(18) C(19) 1.34(3) ? ? yes C(19) C(20) 1.38(2) ? ? yes C(21) C(22) 1.34(2) ? ? yes C(22) C(23) 1.35(2) ? ? yes C(23) C(24) 1.41(2) ? ? yes C(24) C(25) 1.42(2) ? ? yes C(25) C(26) 1.52(2) ? ? yes C(26) C(27) 1.51(2) ? ? yes C(27) C(28) 1.37(2) ? ? yes C(27) C(32) 1.36(2) ? ? yes C(28) C(29) 1.40(3) ? ? yes C(29) C(30) 1.37(3) ? ? yes C(30) C(31) 1.35(3) ? ? yes C(31) C(32) 1.38(3) ? ? yes C(41) C(42) 1.39(2) ? ? yes C(42) C(43) 1.36(3) ? ? yes C(43) C(44) 1.39(2) ? ? yes C(44) C(45) 1.40(2) ? ? yes C(45) C(46) 1.46(2) ? ? yes C(46) C(47) 1.48(2) ? ? yes C(47) C(48) 1.37(2) ? ? yes C(47) C(52) 1.35(2) ? ? yes C(48) C(49) 1.40(2) ? ? yes C(49) C(50) 1.33(3) ? ? yes C(50) C(51) 1.39(3) ? ? yes C(51) C(52) 1.37(2) ? ? yes C(53) C(54) 1.36(3) ? ? yes C(54) C(55) 1.39(2) ? ? yes C(55) C(56) 1.39(2) ? ? yes C(56) C(57) 1.38(2) ? ? yes C(57) C(58) 1.52(2) ? ? yes C(58) C(59) 1.52(2) ? ? yes C(59) C(60) 1.38(2) ? ? yes C(59) C(64) 1.36(2) ? ? yes C(60) C(61) 1.43(3) ? ? yes C(61) C(62) 1.36(4) ? ? yes C(62) C(63) 1.41(4) ? ? yes C(63) C(64) 1.35(3) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Os(2) Os(1) N(1) 170.2(3) ? ? ? yes Os(2) Os(1) N(2) 95.8(3) ? ? ? yes Os(2) Os(1) N(4) 82.4(2) ? ? ? yes Os(2) Os(1) C(1) 90.7(4) ? ? ? yes Os(2) Os(1) C(2) 86.9(5) ? ? ? yes N(1) Os(1) N(2) 75.0(4) ? ? ? yes N(1) Os(1) N(4) 98.4(4) ? ? ? yes N(1) Os(1) C(1) 98.9(5) ? ? ? yes N(1) Os(1) C(2) 91.1(6) ? ? ? yes N(2) Os(1) N(4) 77.2(4) ? ? ? yes N(2) Os(1) C(1) 169.4(5) ? ? ? yes N(2) Os(1) C(2) 98.3(6) ? ? ? yes N(4) Os(1) C(1) 95.4(5) ? ? ? yes N(4) Os(1) C(2) 167.9(5) ? ? ? yes C(1) Os(1) C(2) 90.4(7) ? ? ? yes Os(1) Os(2) Os(3) 71.45(2) ? ? ? yes Os(1) Os(2) C(3) 81.5(4) ? ? ? yes Os(1) Os(2) C(4) 84.6(4) ? ? ? yes Os(1) Os(2) C(5) 164.0(4) ? ? ? yes Os(1) Os(2) C(6) 96.1(5) ? ? ? yes Os(3) Os(2) C(3) 83.6(4) ? ? ? yes Os(3) Os(2) C(4) 84.3(4) ? ? ? yes Os(3) Os(2) C(5) 92.6(4) ? ? ? yes Os(3) Os(2) C(6) 167.5(5) ? ? ? yes C(3) Os(2) C(4) 163.9(6) ? ? ? yes C(3) Os(2) C(5) 96.8(6) ? ? ? yes C(3) Os(2) C(6) 95.6(7) ? ? ? yes C(4) Os(2) C(5) 94.3(7) ? ? ? yes C(4) Os(2) C(6) 93.9(6) ? ? ? yes C(5) Os(2) C(6) 99.9(6) ? ? ? yes Os(2) Os(3) O(9) 91.5(2) ? ? ? yes Os(2) Os(3) N(3) 160.5(3) ? ? ? yes Os(2) Os(3) N(4) 83.5(2) ? ? ? yes Os(2) Os(3) C(7) 93.2(4) ? ? ? yes Os(2) Os(3) C(8) 92.3(3) ? ? ? yes O(9) Os(3) N(3) 80.4(4) ? ? ? yes O(9) Os(3) N(4) 85.6(4) ? ? ? yes O(9) Os(3) C(7) 175.2(5) ? ? ? yes O(9) Os(3) C(8) 89.3(5) ? ? ? yes N(3) Os(3) N(4) 78.2(3) ? ? ? yes N(3) Os(3) C(7) 95.3(5) ? ? ? yes N(3) Os(3) C(8) 105.3(4) ? ? ? yes N(4) Os(3) C(7) 95.7(5) ? ? ? yes N(4) Os(3) C(8) 173.3(5) ? ? ? yes C(7) Os(3) C(8) 89.6(6) ? ? ? yes Os(5) Os(4) N(5) 166.6(3) ? ? ? yes Os(5) Os(4) N(6) 93.2(3) ? ? ? yes Os(5) Os(4) N(8) 82.6(3) ? ? ? yes Os(5) Os(4) C(33) 87.8(4) ? ? ? yes Os(5) Os(4) C(34) 93.0(5) ? ? ? yes N(5) Os(4) N(6) 74.5(4) ? ? ? yes N(5) Os(4) N(8) 99.4(4) ? ? ? yes N(5) Os(4) C(33) 88.9(5) ? ? ? yes N(5) Os(4) C(34) 100.0(5) ? ? ? yes N(6) Os(4) N(8) 76.6(4) ? ? ? yes N(6) Os(4) C(33) 99.5(5) ? ? ? yes N(6) Os(4) C(34) 168.5(6) ? ? ? yes N(8) Os(4) C(33) 169.4(5) ? ? ? yes N(8) Os(4) C(34) 94.7(6) ? ? ? yes C(33) Os(4) C(34) 90.3(7) ? ? ? yes Os(4) Os(5) Os(6) 71.83(2) ? ? ? yes Os(4) Os(5) C(35) 96.6(5) ? ? ? yes Os(4) Os(5) C(36) 84.3(5) ? ? ? yes Os(4) Os(5) C(37) 82.6(4) ? ? ? yes Os(4) Os(5) C(38) 164.5(6) ? ? ? yes Os(6) Os(5) C(35) 168.4(5) ? ? ? yes Os(6) Os(5) C(36) 84.4(6) ? ? ? yes Os(6) Os(5) C(37) 83.9(6) ? ? ? yes Os(6) Os(5) C(38) 92.7(6) ? ? ? yes C(35) Os(5) C(36) 93.9(7) ? ? ? yes C(35) Os(5) C(37) 95.6(7) ? ? ? yes C(35) Os(5) C(38) 98.8(8) ? ? ? yes C(36) Os(5) C(37) 164.6(7) ? ? ? yes C(36) Os(5) C(38) 93.7(7) ? ? ? yes C(37) Os(5) C(38) 96.8(7) ? ? ? yes Os(5) Os(6) O(18) 89.3(3) ? ? ? yes Os(5) Os(6) N(7) 160.9(3) ? ? ? yes Os(5) Os(6) N(8) 84.0(3) ? ? ? yes Os(5) Os(6) C(39) 95.6(6) ? ? ? yes Os(5) Os(6) C(40) 91.9(5) ? ? ? yes O(18) Os(6) N(7) 81.2(4) ? ? ? yes O(18) Os(6) N(8) 85.4(3) ? ? ? yes O(18) Os(6) C(39) 175.0(7) ? ? ? yes O(18) Os(6) C(40) 89.2(5) ? ? ? yes N(7) Os(6) N(8) 78.8(4) ? ? ? yes N(7) Os(6) C(39) 94.4(7) ? ? ? yes N(7) Os(6) C(40) 104.3(6) ? ? ? yes N(8) Os(6) C(39) 96.1(6) ? ? ? yes N(8) Os(6) C(40) 173.3(6) ? ? ? yes C(39) Os(6) C(40) 89.6(7) ? ? ? yes Os(3) O(9) N(2) 111.5(7) ? ? ? yes Os(6) O(18) N(6) 112.0(6) ? ? ? yes Os(1) N(1) C(9) 127.8(9) ? ? ? yes Os(1) N(1) C(13) 113.9(7) ? ? ? yes C(9) N(1) C(13) 117(1) ? ? ? yes Os(1) N(2) O(9) 120.0(8) ? ? ? yes Os(1) N(2) C(14) 118.2(8) ? ? ? yes O(9) N(2) C(14) 120(1) ? ? ? yes Os(3) N(3) C(21) 124.8(8) ? ? ? yes Os(3) N(3) C(25) 117.0(8) ? ? ? yes C(21) N(3) C(25) 118.1(10) ? ? ? yes Os(1) N(4) Os(3) 100.1(4) ? ? ? yes Os(1) N(4) C(26) 118.6(8) ? ? ? yes Os(3) N(4) C(26) 114.8(6) ? ? ? yes Os(4) N(5) C(41) 126.8(10) ? ? ? yes Os(4) N(5) C(45) 114.5(8) ? ? ? yes C(41) N(5) C(45) 117(1) ? ? ? yes Os(4) N(6) O(18) 120.7(7) ? ? ? yes Os(4) N(6) C(46) 120.1(7) ? ? ? yes O(18) N(6) C(46) 118.2(10) ? ? ? yes Os(6) N(7) C(53) 125(1) ? ? ? yes Os(6) N(7) C(57) 117.0(10) ? ? ? yes C(53) N(7) C(57) 117(1) ? ? ? yes Os(4) N(8) Os(6) 101.4(5) ? ? ? yes Os(4) N(8) C(58) 118.9(7) ? ? ? yes Os(6) N(8) C(58) 115.0(8) ? ? ? yes Os(1) C(1) O(1) 177(1) ? ? ? yes Os(1) C(2) O(2) 176(1) ? ? ? yes Os(2) C(3) O(3) 177(1) ? ? ? yes Os(2) C(4) O(4) 179(1) ? ? ? yes Os(2) C(5) O(5) 177(1) ? ? ? yes Os(2) C(6) O(6) 177(1) ? ? ? yes Os(3) C(7) O(7) 177(1) ? ? ? yes Os(3) C(8) O(8) 175(1) ? ? ? yes N(1) C(9) C(10) 124(1) ? ? ? yes C(9) C(10) C(11) 117(1) ? ? ? yes C(10) C(11) C(12) 119(1) ? ? ? yes C(11) C(12) C(13) 119(1) ? ? ? yes N(1) C(13) C(12) 120(1) ? ? ? yes N(1) C(13) C(14) 115(1) ? ? ? yes C(12) C(13) C(14) 123(1) ? ? ? yes N(2) C(14) C(13) 115(1) ? ? ? yes N(2) C(14) C(15) 122(1) ? ? ? yes C(13) C(14) C(15) 122(1) ? ? ? yes C(14) C(15) C(16) 121(1) ? ? ? yes C(14) C(15) C(20) 119(1) ? ? ? yes C(16) C(15) C(20) 119(1) ? ? ? yes C(15) C(16) C(17) 119(1) ? ? ? yes C(16) C(17) C(18) 119(1) ? ? ? yes C(17) C(18) C(19) 120(1) ? ? ? yes C(18) C(19) C(20) 120(1) ? ? ? yes C(15) C(20) C(19) 120(1) ? ? ? yes N(3) C(21) C(22) 124(1) ? ? ? yes C(21) C(22) C(23) 118(1) ? ? ? yes C(22) C(23) C(24) 120(1) ? ? ? yes C(23) C(24) C(25) 116(1) ? ? ? yes N(3) C(25) C(24) 122(1) ? ? ? yes N(3) C(25) C(26) 120(1) ? ? ? yes C(24) C(25) C(26) 117(1) ? ? ? yes N(4) C(26) C(25) 109.1(9) ? ? ? yes N(4) C(26) C(27) 108.6(10) ? ? ? yes C(25) C(26) C(27) 112(1) ? ? ? yes C(26) C(27) C(28) 118(1) ? ? ? yes C(26) C(27) C(32) 122(1) ? ? ? yes C(28) C(27) C(32) 118(1) ? ? ? yes C(27) C(28) C(29) 119(1) ? ? ? yes C(28) C(29) C(30) 120(1) ? ? ? yes C(29) C(30) C(31) 119(1) ? ? ? yes C(30) C(31) C(32) 120(1) ? ? ? yes C(27) C(32) C(31) 121(1) ? ? ? yes Os(4) C(33) O(10) 177(1) ? ? ? yes Os(4) C(34) O(11) 174(1) ? ? ? yes Os(5) C(35) O(12) 177(1) ? ? ? yes Os(5) C(36) O(13) 175(1) ? ? ? yes Os(5) C(37) O(14) 176(1) ? ? ? yes Os(5) C(38) O(15) 179(1) ? ? ? yes Os(6) C(39) O(16) 177(1) ? ? ? yes Os(6) C(40) O(17) 176(1) ? ? ? yes N(5) C(41) C(42) 123(1) ? ? ? yes C(41) C(42) C(43) 119(1) ? ? ? yes C(42) C(43) C(44) 117(1) ? ? ? yes C(43) C(44) C(45) 119(1) ? ? ? yes N(5) C(45) C(44) 122(1) ? ? ? yes N(5) C(45) C(46) 116(1) ? ? ? yes C(44) C(45) C(46) 121(1) ? ? ? yes N(6) C(46) C(45) 112(1) ? ? ? yes N(6) C(46) C(47) 123(1) ? ? ? yes C(45) C(46) C(47) 123(1) ? ? ? yes C(46) C(47) C(48) 118(1) ? ? ? yes C(46) C(47) C(52) 120(1) ? ? ? yes C(48) C(47) C(52) 120(1) ? ? ? yes C(47) C(48) C(49) 117(1) ? ? ? yes C(48) C(49) C(50) 121(1) ? ? ? yes C(49) C(50) C(51) 120(1) ? ? ? yes C(50) C(51) C(52) 118(1) ? ? ? yes C(47) C(52) C(51) 121(1) ? ? ? yes N(7) C(53) C(54) 124(1) ? ? ? yes C(53) C(54) C(55) 117(1) ? ? ? yes C(54) C(55) C(56) 119(1) ? ? ? yes C(55) C(56) C(57) 119(1) ? ? ? yes N(7) C(57) C(56) 121(1) ? ? ? yes N(7) C(57) C(58) 119(1) ? ? ? yes C(56) C(57) C(58) 118(1) ? ? ? yes N(8) C(58) C(57) 109(1) ? ? ? yes N(8) C(58) C(59) 110(1) ? ? ? yes C(57) C(58) C(59) 112(1) ? ? ? yes C(58) C(59) C(60) 118(1) ? ? ? yes C(58) C(59) C(64) 121(1) ? ? ? yes C(60) C(59) C(64) 119(1) ? ? ? yes C(59) C(60) C(61) 119(1) ? ? ? yes C(60) C(61) C(62) 116(2) ? ? ? yes C(61) C(62) C(63) 123(2) ? ? ? yes C(62) C(63) C(64) 116(2) ? ? ? yes C(59) C(64) C(63) 123(1) ? ? ? yes Cl(1) C(65) Cl(2) 112.2(4) ? ? ? yes Cl(1) C(65) Cl(3) 110.5(4) ? ? ? yes Cl(2) C(65) Cl(3) 106.3(5) ? ? ? yes Cl(4) C(66) Cl(5) 114.6(3) ? ? ? yes Cl(4) C(66) Cl(6) 109.1(3) ? ? ? yes Cl(5) C(66) Cl(6) 112.7(3) ? ? ? yes Cl(7) C(67) Cl(8) 104.7(6) ? ? ? yes Cl(7) C(67) Cl(9) 110.2(8) ? ? ? yes Cl(8) C(67) Cl(9) 112.3(7) ? ? ? yes #------------------------------------------------------------------------------ #================================end of file============================== data_wt0294w-JW011-compound 5 _database_code_CSD 174855 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 10 12:09:53 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 25.233(1) _cell_length_b 20.658(1) _cell_length_c 10.131(1) _cell_angle_alpha 90.00 _cell_angle_beta 91.60(1) _cell_angle_gamma 90.00 _cell_volume 5278.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.190 _exptl_crystal_density_diffrn 2.637 _exptl_crystal_density_meas ? _chemical_formula_weight 1047.94 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H11 N O11 Os3 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3776.00 _exptl_absorpt_coefficient_mu 14.456 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 32757 _reflns_number_total 12240 _reflns_number_observed 7842 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 4.92 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.55 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 24 -1.216 7.603 'International Tables' O 0 88 0.011 0.006 'International Tables' N 0 8 0.006 0.003 'International Tables' C 0 184 0.003 0.002 'International Tables' H 0 88 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) 0.92161(2) 0.01847(3) 0.24096(6) 0.0353(2) Uij ? ? Os(2) 0.87107(2) 0.09589(3) 0.43670(6) 0.0417(2) Uij ? ? Os(3) 0.84544(2) 0.11333(3) 0.16080(7) 0.0458(2) Uij ? ? Os(4) 0.57001(2) 0.00231(3) 0.78262(6) 0.0374(2) Uij ? ? Os(5) 0.59991(2) 0.12184(3) 0.66344(7) 0.0504(2) Uij ? ? Os(6) 0.62835(2) 0.09747(3) 0.93419(6) 0.0438(2) Uij ? ? O(1) 0.9624(4) -0.0660(6) 0.468(1) 0.063(4) Uij ? ? O(2) 0.9728(5) -0.0629(6) 0.029(1) 0.082(5) Uij ? ? O(3) 1.0187(4) 0.1036(6) 0.258(1) 0.066(4) Uij ? ? O(4) 0.9242(5) 0.0464(8) 0.692(1) 0.093(5) Uij ? ? O(5) 0.7847(5) -0.0089(6) 0.446(1) 0.077(4) Uij ? ? O(6) 0.7935(5) 0.1926(7) 0.555(1) 0.093(5) Uij ? ? O(7) 0.9592(5) 0.1984(6) 0.416(1) 0.079(5) Uij ? ? O(8) 0.7434(5) 0.1740(8) 0.255(2) 0.106(6) Uij ? ? O(9) 0.9003(6) 0.2425(7) 0.164(2) 0.119(7) Uij ? ? O(10) 0.8255(6) 0.1266(7) -0.136(1) 0.101(6) Uij ? ? O(11) 0.8116(4) 0.0209(4) 0.1540(9) 0.043(3) Uij ? ? O(12) 0.5479(4) -0.0461(6) 0.503(1) 0.069(4) Uij ? ? O(13) 0.5389(6) -0.1184(7) 0.933(1) 0.088(5) Uij ? ? O(14) 0.4540(4) 0.0425(6) 0.795(1) 0.074(4) Uij ? ? O(15) 0.5571(6) 0.1129(10) 0.379(1) 0.123(7) Uij ? ? O(16) 0.7070(5) 0.0614(8) 0.593(1) 0.103(6) Uij ? ? O(17) 0.6489(6) 0.2556(7) 0.666(2) 0.129(7) Uij ? ? O(18) 0.4929(5) 0.1805(8) 0.744(2) 0.102(6) Uij ? ? O(19) 0.7180(4) 0.1965(7) 0.912(1) 0.086(5) Uij ? ? O(20) 0.6528(6) 0.0659(8) 1.224(1) 0.093(6) Uij ? ? O(21) 0.5518(5) 0.2028(6) 1.012(1) 0.090(5) Uij ? ? O(22) 0.6780(3) 0.0229(5) 0.8775(9) 0.043(3) Uij ? ? N(1) 0.8449(4) -0.0248(5) 0.2038(9) 0.027(3) Uij ? ? N(2) 0.6538(4) -0.0211(6) 0.798(1) 0.037(3) Uij ? ? C(1) 0.9459(6) -0.0350(7) 0.381(2) 0.044(5) Uij ? ? C(2) 0.9518(7) -0.0321(8) 0.103(2) 0.057(5) Uij ? ? C(3) 0.9829(6) 0.0726(8) 0.256(1) 0.048(5) Uij ? ? C(4) 0.9037(6) 0.0635(10) 0.595(2) 0.067(6) Uij ? ? C(5) 0.8161(6) 0.0295(7) 0.435(2) 0.048(5) Uij ? ? C(6) 0.8243(6) 0.1567(9) 0.511(2) 0.063(6) Uij ? ? C(7) 0.9263(6) 0.1599(8) 0.422(2) 0.055(5) Uij ? ? C(8) 0.7817(6) 0.1520(8) 0.221(2) 0.065(6) Uij ? ? C(9) 0.8809(7) 0.1931(8) 0.164(2) 0.066(6) Uij ? ? C(10) 0.8325(7) 0.1220(9) -0.025(2) 0.062(6) Uij ? ? C(11) 0.8282(5) -0.0848(7) 0.204(1) 0.041(4) Uij ? ? C(12) 0.7735(5) -0.1059(7) 0.160(1) 0.035(4) Uij ? ? C(13) 0.7296(7) -0.0648(9) 0.154(2) 0.070(6) Uij ? ? C(14) 0.6808(6) -0.0907(8) 0.113(2) 0.058(5) Uij ? ? C(15) 0.6754(6) -0.1537(9) 0.079(2) 0.056(5) Uij ? ? C(16) 0.7190(7) -0.1923(9) 0.083(2) 0.073(7) Uij ? ? C(17) 0.7678(6) -0.1705(8) 0.123(2) 0.059(5) Uij ? ? C(18) 0.8643(5) -0.1344(6) 0.264(1) 0.038(4) Uij ? ? C(19) 0.8577(6) -0.1515(7) 0.397(2) 0.048(5) Uij ? ? C(20) 0.8904(8) -0.1973(8) 0.455(2) 0.066(6) Uij ? ? C(21) 0.9284(6) -0.2271(8) 0.384(2) 0.060(6) Uij ? ? C(22) 0.9343(6) -0.2116(7) 0.255(2) 0.047(5) Uij ? ? C(23) 0.9022(7) -0.1640(8) 0.196(1) 0.055(5) Uij ? ? C(24) 0.5582(5) -0.0288(8) 0.609(2) 0.053(5) Uij ? ? C(25) 0.5538(6) -0.0736(8) 0.873(2) 0.054(5) Uij ? ? C(26) 0.4976(6) 0.0307(7) 0.789(1) 0.047(5) Uij ? ? C(27) 0.5739(7) 0.1151(10) 0.483(2) 0.070(7) Uij ? ? C(28) 0.6671(8) 0.0820(9) 0.623(2) 0.073(7) Uij ? ? C(29) 0.6308(6) 0.2048(9) 0.663(2) 0.069(6) Uij ? ? C(30) 0.5325(7) 0.1567(8) 0.721(2) 0.071(6) Uij ? ? C(31) 0.6847(6) 0.1593(8) 0.923(2) 0.055(5) Uij ? ? C(32) 0.6434(6) 0.0778(9) 1.115(2) 0.062(6) Uij ? ? C(33) 0.5815(7) 0.1633(8) 0.982(2) 0.061(6) Uij ? ? C(34) 0.6816(5) -0.0696(7) 0.751(1) 0.040(4) Uij ? ? C(35) 0.7391(5) -0.0800(8) 0.776(1) 0.044(4) Uij ? ? C(36) 0.7755(6) -0.0315(8) 0.817(2) 0.060(5) Uij ? ? C(37) 0.8287(6) -0.0463(10) 0.837(2) 0.069(6) Uij ? ? C(38) 0.8465(6) -0.109(1) 0.820(2) 0.073(7) Uij ? ? C(39) 0.8117(7) -0.1563(9) 0.783(2) 0.071(6) Uij ? ? C(40) 0.7587(7) -0.1409(8) 0.757(2) 0.060(6) Uij ? ? C(41) 0.6547(6) -0.1151(7) 0.658(1) 0.041(4) Uij ? ? C(42) 0.6616(6) -0.1125(8) 0.526(1) 0.053(5) Uij ? ? C(43) 0.6364(9) -0.156(1) 0.440(2) 0.083(8) Uij ? ? C(44) 0.6016(8) -0.2009(9) 0.489(2) 0.072(7) Uij ? ? C(45) 0.5942(6) -0.2045(8) 0.618(2) 0.059(6) Uij ? ? C(46) 0.6215(6) -0.1632(7) 0.704(2) 0.049(5) Uij ? ? H(1) 0.7328 -0.0204 0.1770 0.0844 Uij ? ? H(2) 0.6505 -0.0633 0.1085 0.0693 Uij ? ? H(3) 0.6418 -0.1707 0.0524 0.0676 Uij ? ? H(4) 0.7153 -0.2363 0.0578 0.0876 Uij ? ? H(5) 0.7974 -0.1988 0.1251 0.0709 Uij ? ? H(6) 0.8308 -0.1315 0.4465 0.0581 Uij ? ? H(7) 0.8864 -0.2082 0.5452 0.0790 Uij ? ? H(8) 0.9508 -0.2587 0.4250 0.0716 Uij ? ? H(9) 0.9603 -0.2331 0.2049 0.0568 Uij ? ? H(10) 0.9073 -0.1524 0.1063 0.0657 Uij ? ? H(11) 0.7634 0.0114 0.8318 0.0714 Uij ? ? H(12) 0.8530 -0.0131 0.8613 0.0831 Uij ? ? H(13) 0.8829 -0.1188 0.8352 0.0875 Uij ? ? H(14) 0.8235 -0.1997 0.7747 0.0855 Uij ? ? H(15) 0.7354 -0.1739 0.7253 0.0723 Uij ? ? H(16) 0.6842 -0.0803 0.4919 0.0633 Uij ? ? H(17) 0.6432 -0.1544 0.3481 0.1000 Uij ? ? H(18) 0.5830 -0.2292 0.4301 0.0867 Uij ? ? H(19) 0.5702 -0.2354 0.6518 0.0712 Uij ? ? H(20) 0.6174 -0.1680 0.7960 0.0587 Uij ? ? H(21) 0.8880 0.0551 0.1158 0.0608 Uij ? ? H(22) 0.5989 0.0237 0.9294 0.0608 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0287(3) 0.0412(3) 0.0360(3) -0.0019(2) 0.0025(2) 0.0020(3) Os(2) 0.0357(3) 0.0420(4) 0.0477(4) -0.0016(3) 0.0040(3) -0.0060(3) Os(3) 0.0425(3) 0.0369(4) 0.0573(4) -0.0040(3) -0.0108(3) 0.0101(3) Os(4) 0.0295(3) 0.0403(3) 0.0425(3) -0.0028(2) 0.0038(2) -0.0066(3) Os(5) 0.0402(3) 0.0469(4) 0.0642(4) 0.0024(3) 0.0020(3) 0.0103(3) Os(6) 0.0359(3) 0.0388(4) 0.0565(4) -0.0027(3) -0.0007(3) -0.0107(3) O(1) 0.061(7) 0.069(9) 0.058(8) -0.004(6) -0.024(6) 0.010(6) O(2) 0.11(1) 0.060(8) 0.083(9) -0.030(7) 0.054(8) -0.037(7) O(3) 0.042(6) 0.087(9) 0.067(8) -0.036(6) 0.002(6) 0.001(7) O(4) 0.065(8) 0.16(2) 0.052(8) 0.008(9) -0.003(7) 0.016(9) O(5) 0.074(8) 0.077(10) 0.081(9) -0.025(7) 0.031(7) -0.028(7) O(6) 0.079(9) 0.08(1) 0.12(1) 0.026(8) 0.017(9) -0.024(9) O(7) 0.069(8) 0.081(10) 0.086(10) -0.037(7) 0.004(7) -0.022(8) O(8) 0.051(8) 0.12(1) 0.14(1) 0.045(8) -0.027(8) -0.03(1) O(9) 0.14(1) 0.08(1) 0.13(1) -0.06(1) -0.06(1) 0.05(1) O(10) 0.10(1) 0.12(1) 0.08(1) 0.007(9) -0.046(9) 0.022(9) O(11) 0.042(5) 0.032(6) 0.054(6) 0.002(4) -0.007(5) 0.000(5) O(12) 0.052(7) 0.10(1) 0.053(8) 0.025(7) -0.010(6) -0.027(7) O(13) 0.10(1) 0.08(1) 0.09(1) -0.025(8) 0.034(8) 0.011(8) O(14) 0.031(6) 0.11(1) 0.079(9) 0.017(6) 0.004(6) -0.021(8) O(15) 0.10(1) 0.20(2) 0.062(10) 0.00(1) -0.004(9) 0.01(1) O(16) 0.056(8) 0.13(1) 0.13(1) 0.031(8) 0.051(8) 0.05(1) O(17) 0.11(1) 0.07(1) 0.20(2) -0.035(9) -0.08(1) 0.06(1) O(18) 0.043(7) 0.13(1) 0.13(1) 0.045(8) 0.004(8) -0.01(1) O(19) 0.053(7) 0.09(1) 0.12(1) -0.029(7) -0.008(7) 0.014(9) O(20) 0.09(1) 0.12(1) 0.068(10) 0.008(9) -0.008(8) -0.011(9) O(21) 0.050(7) 0.060(9) 0.16(1) 0.010(6) -0.015(8) -0.041(9) O(22) 0.037(5) 0.036(6) 0.057(6) 0.001(4) -0.008(5) -0.007(5) N(1) 0.034(6) 0.023(6) 0.025(6) -0.004(5) 0.006(4) 0.003(5) N(2) 0.025(5) 0.041(7) 0.043(7) 0.003(5) 0.001(5) -0.002(6) C(1) 0.040(8) 0.040(9) 0.052(10) -0.015(7) 0.008(7) -0.006(8) C(2) 0.09(1) 0.04(1) 0.045(10) -0.001(9) 0.014(9) -0.009(8) C(3) 0.047(9) 0.06(1) 0.031(8) 0.001(8) 0.000(7) 0.001(8) C(4) 0.042(9) 0.10(2) 0.06(1) -0.009(10) 0.018(9) 0.02(1) C(5) 0.047(9) 0.035(9) 0.06(1) -0.008(7) 0.015(8) -0.018(8) C(6) 0.042(9) 0.07(1) 0.07(1) -0.002(9) 0.006(9) -0.03(1) C(7) 0.054(10) 0.06(1) 0.05(1) -0.013(9) 0.002(8) -0.023(9) C(8) 0.043(9) 0.05(1) 0.10(2) 0.008(8) -0.014(10) -0.02(1) C(9) 0.08(1) 0.04(1) 0.08(1) -0.021(9) -0.01(1) 0.021(9) C(10) 0.050(10) 0.06(1) 0.07(1) -0.005(8) -0.010(9) 0.02(1) C(11) 0.029(7) 0.046(10) 0.049(9) 0.006(6) -0.011(6) -0.015(7) C(12) 0.027(7) 0.040(9) 0.036(8) 0.001(6) -0.002(6) 0.002(7) C(13) 0.06(1) 0.06(1) 0.09(1) -0.012(9) -0.01(1) 0.00(1) C(14) 0.052(10) 0.05(1) 0.07(1) 0.000(8) -0.010(9) 0.006(9) C(15) 0.040(9) 0.07(1) 0.06(1) -0.018(8) -0.010(8) 0.008(9) C(16) 0.07(1) 0.05(1) 0.10(2) -0.028(10) -0.01(1) 0.00(1) C(17) 0.054(10) 0.037(10) 0.08(1) -0.001(8) -0.024(9) -0.020(9) C(18) 0.038(8) 0.025(8) 0.050(9) -0.010(6) -0.007(7) -0.002(7) C(19) 0.052(9) 0.045(10) 0.048(10) 0.005(7) 0.003(8) 0.008(8) C(20) 0.10(1) 0.05(1) 0.05(1) 0.003(10) -0.02(1) 0.018(9) C(21) 0.048(10) 0.04(1) 0.09(1) 0.017(8) -0.010(9) -0.002(10) C(22) 0.044(9) 0.032(9) 0.07(1) 0.016(7) -0.004(8) -0.008(8) C(23) 0.08(1) 0.05(1) 0.038(9) 0.002(9) 0.000(8) -0.013(8) C(24) 0.018(6) 0.08(1) 0.06(1) 0.020(7) 0.001(7) -0.020(9) C(25) 0.046(9) 0.039(10) 0.08(1) -0.008(8) -0.003(9) -0.004(9) C(26) 0.057(10) 0.034(9) 0.051(10) -0.010(7) 0.001(8) -0.012(7) C(27) 0.06(1) 0.08(1) 0.08(1) 0.009(10) 0.01(1) 0.02(1) C(28) 0.09(1) 0.05(1) 0.09(1) 0.00(1) 0.03(1) 0.04(1) C(29) 0.038(9) 0.05(1) 0.12(2) -0.005(8) -0.027(10) 0.03(1) C(30) 0.06(1) 0.05(1) 0.10(2) 0.012(9) -0.01(1) -0.02(1) C(31) 0.051(10) 0.036(10) 0.08(1) -0.006(8) 0.002(9) -0.008(9) C(32) 0.032(8) 0.06(1) 0.09(2) 0.004(8) 0.002(9) 0.01(1) C(33) 0.06(1) 0.04(1) 0.08(1) -0.002(8) -0.010(10) -0.023(9) C(34) 0.029(7) 0.048(9) 0.044(9) 0.005(7) 0.004(6) 0.008(7) C(35) 0.028(7) 0.06(1) 0.044(9) 0.001(7) 0.007(6) -0.007(8) C(36) 0.032(8) 0.05(1) 0.10(1) 0.002(7) -0.003(8) -0.011(10) C(37) 0.026(8) 0.09(1) 0.10(1) -0.008(9) -0.001(9) -0.01(1) C(38) 0.035(9) 0.09(2) 0.10(2) 0.011(9) -0.001(9) -0.01(1) C(39) 0.045(10) 0.07(1) 0.10(2) 0.012(9) -0.02(1) -0.02(1) C(40) 0.06(1) 0.05(1) 0.07(1) 0.005(9) -0.016(9) -0.013(9) C(41) 0.048(8) 0.034(9) 0.041(9) 0.000(7) 0.002(7) 0.006(7) C(42) 0.06(1) 0.06(1) 0.036(9) 0.005(8) 0.015(8) -0.003(8) C(43) 0.12(2) 0.08(2) 0.04(1) 0.05(1) 0.01(1) -0.03(1) C(44) 0.08(1) 0.05(1) 0.09(2) 0.004(10) -0.04(1) -0.02(1) C(45) 0.06(1) 0.04(1) 0.08(1) -0.013(8) -0.018(9) -0.002(9) C(46) 0.058(10) 0.036(9) 0.05(1) -0.011(7) 0.001(8) -0.010(8) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 7842 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0519 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0499 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.183 _refine_ls_shift/esd_max 0.0040 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.56 _refine_diff_density_max 2.12 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Os(2) 2.8736(8) ? ? yes Os(1) Os(3) 2.8471(8) ? ? yes Os(1) N(1) 2.155(10) ? ? yes Os(1) C(1) 1.89(2) ? ? yes Os(1) C(2) 1.92(2) ? ? yes Os(1) C(3) 1.91(2) ? ? yes Os(2) Os(3) 2.8740(9) ? ? yes Os(2) C(4) 1.90(2) ? ? yes Os(2) C(5) 1.95(1) ? ? yes Os(2) C(6) 1.90(2) ? ? yes Os(2) C(7) 1.93(2) ? ? yes Os(3) O(11) 2.091(9) ? ? yes Os(3) C(8) 1.91(2) ? ? yes Os(3) C(9) 1.87(2) ? ? yes Os(3) C(10) 1.91(2) ? ? yes Os(4) Os(5) 2.8594(9) ? ? yes Os(4) Os(6) 2.8747(8) ? ? yes Os(4) N(2) 2.170(10) ? ? yes Os(4) C(24) 1.89(2) ? ? yes Os(4) C(25) 1.87(2) ? ? yes Os(4) C(26) 1.92(2) ? ? yes Os(5) Os(6) 2.8605(9) ? ? yes Os(5) C(27) 1.93(2) ? ? yes Os(5) C(28) 1.94(2) ? ? yes Os(5) C(29) 1.88(2) ? ? yes Os(5) C(30) 1.95(2) ? ? yes Os(6) O(22) 2.077(9) ? ? yes Os(6) C(31) 1.92(2) ? ? yes Os(6) C(32) 1.91(2) ? ? yes Os(6) C(33) 1.88(2) ? ? yes O(1) C(1) 1.16(2) ? ? yes O(2) C(2) 1.13(2) ? ? yes O(3) C(3) 1.11(2) ? ? yes O(4) C(4) 1.16(2) ? ? yes O(5) C(5) 1.13(2) ? ? yes O(6) C(6) 1.17(2) ? ? yes O(7) C(7) 1.15(2) ? ? yes O(8) C(8) 1.13(2) ? ? yes O(9) C(9) 1.13(2) ? ? yes O(10) C(10) 1.14(2) ? ? yes O(11) N(1) 1.35(1) ? ? yes O(12) C(24) 1.15(2) ? ? yes O(13) C(25) 1.18(2) ? ? yes O(14) C(26) 1.13(2) ? ? yes O(15) C(27) 1.13(2) ? ? yes O(16) C(28) 1.14(2) ? ? yes O(17) C(29) 1.14(2) ? ? yes O(18) C(30) 1.14(2) ? ? yes O(19) C(31) 1.15(2) ? ? yes O(20) C(32) 1.15(2) ? ? yes O(21) C(33) 1.15(2) ? ? yes O(22) N(2) 1.35(1) ? ? yes N(1) C(11) 1.31(2) ? ? yes N(2) C(34) 1.32(2) ? ? yes C(11) C(12) 1.50(2) ? ? yes C(11) C(18) 1.49(2) ? ? yes C(12) C(13) 1.40(2) ? ? yes C(12) C(17) 1.39(2) ? ? yes C(13) C(14) 1.40(2) ? ? yes C(14) C(15) 1.35(2) ? ? yes C(15) C(16) 1.36(2) ? ? yes C(16) C(17) 1.36(2) ? ? yes C(18) C(19) 1.41(2) ? ? yes C(18) C(23) 1.34(2) ? ? yes C(19) C(20) 1.38(2) ? ? yes C(20) C(21) 1.36(2) ? ? yes C(21) C(22) 1.36(2) ? ? yes C(22) C(23) 1.40(2) ? ? yes C(34) C(35) 1.48(2) ? ? yes C(34) C(41) 1.48(2) ? ? yes C(35) C(36) 1.41(2) ? ? yes C(35) C(40) 1.37(2) ? ? yes C(36) C(37) 1.38(2) ? ? yes C(37) C(38) 1.38(2) ? ? yes C(38) C(39) 1.36(2) ? ? yes C(39) C(40) 1.39(2) ? ? yes C(41) C(42) 1.35(2) ? ? yes C(41) C(46) 1.39(2) ? ? yes C(42) C(43) 1.39(2) ? ? yes C(43) C(44) 1.38(3) ? ? yes C(44) C(45) 1.33(3) ? ? yes C(45) C(46) 1.39(2) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Os(2) Os(1) Os(3) 60.31(2) ? ? ? yes Os(2) Os(1) N(1) 86.4(3) ? ? ? yes Os(2) Os(1) C(1) 87.0(4) ? ? ? yes Os(2) Os(1) C(2) 176.5(5) ? ? ? yes Os(2) Os(1) C(3) 89.5(4) ? ? ? yes Os(3) Os(1) N(1) 68.9(3) ? ? ? yes Os(3) Os(1) C(1) 145.1(4) ? ? ? yes Os(3) Os(1) C(2) 116.5(5) ? ? ? yes Os(3) Os(1) C(3) 99.1(5) ? ? ? yes N(1) Os(1) C(1) 99.2(5) ? ? ? yes N(1) Os(1) C(2) 91.1(6) ? ? ? yes N(1) Os(1) C(3) 167.8(5) ? ? ? yes C(1) Os(1) C(2) 95.8(7) ? ? ? yes C(1) Os(1) C(3) 92.1(6) ? ? ? yes C(2) Os(1) C(3) 92.3(7) ? ? ? yes Os(1) Os(2) Os(3) 59.39(2) ? ? ? yes Os(1) Os(2) C(4) 101.3(6) ? ? ? yes Os(1) Os(2) C(5) 86.2(4) ? ? ? yes Os(1) Os(2) C(6) 159.7(6) ? ? ? yes Os(1) Os(2) C(7) 89.6(5) ? ? ? yes Os(3) Os(2) C(4) 160.7(6) ? ? ? yes Os(3) Os(2) C(5) 86.6(5) ? ? ? yes Os(3) Os(2) C(6) 100.4(6) ? ? ? yes Os(3) Os(2) C(7) 89.1(5) ? ? ? yes C(4) Os(2) C(5) 92.9(7) ? ? ? yes C(4) Os(2) C(6) 99.0(8) ? ? ? yes C(4) Os(2) C(7) 90.5(7) ? ? ? yes C(5) Os(2) C(6) 91.0(7) ? ? ? yes C(5) Os(2) C(7) 175.1(6) ? ? ? yes C(6) Os(2) C(7) 92.0(7) ? ? ? yes Os(1) Os(3) Os(2) 60.30(2) ? ? ? yes Os(1) Os(3) O(11) 69.7(2) ? ? ? yes Os(1) Os(3) C(8) 139.7(6) ? ? ? yes Os(1) Os(3) C(9) 106.4(5) ? ? ? yes Os(1) Os(3) C(10) 116.2(5) ? ? ? yes Os(2) Os(3) O(11) 89.9(3) ? ? ? yes Os(2) Os(3) C(8) 84.8(6) ? ? ? yes Os(2) Os(3) C(9) 90.0(5) ? ? ? yes Os(2) Os(3) C(10) 176.3(5) ? ? ? yes O(11) Os(3) C(8) 92.6(6) ? ? ? yes O(11) Os(3) C(9) 175.5(6) ? ? ? yes O(11) Os(3) C(10) 89.7(6) ? ? ? yes C(8) Os(3) C(9) 91.9(8) ? ? ? yes C(8) Os(3) C(10) 98.9(8) ? ? ? yes C(9) Os(3) C(10) 90.2(7) ? ? ? yes Os(5) Os(4) Os(6) 59.85(2) ? ? ? yes Os(5) Os(4) N(2) 87.4(3) ? ? ? yes Os(5) Os(4) C(24) 86.4(5) ? ? ? yes Os(5) Os(4) C(25) 175.1(5) ? ? ? yes Os(5) Os(4) C(26) 90.7(4) ? ? ? yes Os(6) Os(4) N(2) 68.4(3) ? ? ? yes Os(6) Os(4) C(24) 142.6(5) ? ? ? yes Os(6) Os(4) C(25) 115.3(5) ? ? ? yes Os(6) Os(4) C(26) 104.3(4) ? ? ? yes N(2) Os(4) C(24) 96.8(5) ? ? ? yes N(2) Os(4) C(25) 90.2(6) ? ? ? yes N(2) Os(4) C(26) 172.3(5) ? ? ? yes C(24) Os(4) C(25) 98.2(7) ? ? ? yes C(24) Os(4) C(26) 90.6(6) ? ? ? yes C(25) Os(4) C(26) 91.1(6) ? ? ? yes Os(4) Os(5) Os(6) 60.34(2) ? ? ? yes Os(4) Os(5) C(27) 104.5(6) ? ? ? yes Os(4) Os(5) C(28) 88.1(5) ? ? ? yes Os(4) Os(5) C(29) 154.2(6) ? ? ? yes Os(4) Os(5) C(30) 87.1(6) ? ? ? yes Os(6) Os(5) C(27) 164.8(6) ? ? ? yes Os(6) Os(5) C(28) 86.1(6) ? ? ? yes Os(6) Os(5) C(29) 93.9(6) ? ? ? yes Os(6) Os(5) C(30) 88.5(6) ? ? ? yes C(27) Os(5) C(28) 92.5(8) ? ? ? yes C(27) Os(5) C(29) 101.2(8) ? ? ? yes C(27) Os(5) C(30) 92.0(8) ? ? ? yes C(28) Os(5) C(29) 91.3(7) ? ? ? yes C(28) Os(5) C(30) 174.1(8) ? ? ? yes C(29) Os(5) C(30) 91.6(8) ? ? ? yes Os(4) Os(6) Os(5) 59.81(2) ? ? ? yes Os(4) Os(6) O(22) 69.4(2) ? ? ? yes Os(4) Os(6) C(31) 142.5(5) ? ? ? yes Os(4) Os(6) C(32) 117.0(5) ? ? ? yes Os(4) Os(6) C(33) 108.5(5) ? ? ? yes Os(5) Os(6) O(22) 90.1(3) ? ? ? yes Os(5) Os(6) C(31) 89.5(5) ? ? ? yes Os(5) Os(6) C(32) 176.3(5) ? ? ? yes Os(5) Os(6) C(33) 88.7(6) ? ? ? yes O(22) Os(6) C(31) 91.4(5) ? ? ? yes O(22) Os(6) C(32) 90.2(6) ? ? ? yes O(22) Os(6) C(33) 177.9(5) ? ? ? yes C(31) Os(6) C(32) 94.1(7) ? ? ? yes C(31) Os(6) C(33) 90.4(7) ? ? ? yes C(32) Os(6) C(33) 90.8(8) ? ? ? yes Os(3) O(11) N(1) 112.1(7) ? ? ? yes Os(6) O(22) N(2) 113.5(7) ? ? ? yes Os(1) N(1) O(11) 108.7(7) ? ? ? yes Os(1) N(1) C(11) 132.8(9) ? ? ? yes O(11) N(1) C(11) 117(1) ? ? ? yes Os(4) N(2) O(22) 108.4(7) ? ? ? yes Os(4) N(2) C(34) 132.1(9) ? ? ? yes O(22) N(2) C(34) 119(1) ? ? ? yes Os(1) C(1) O(1) 177(1) ? ? ? yes Os(1) C(2) O(2) 174(1) ? ? ? yes Os(1) C(3) O(3) 175(1) ? ? ? yes Os(2) C(4) O(4) 177(1) ? ? ? yes Os(2) C(5) O(5) 174(1) ? ? ? yes Os(2) C(6) O(6) 176(1) ? ? ? yes Os(2) C(7) O(7) 178(1) ? ? ? yes Os(3) C(8) O(8) 178(1) ? ? ? yes Os(3) C(9) O(9) 177(1) ? ? ? yes Os(3) C(10) O(10) 178(1) ? ? ? yes N(1) C(11) C(12) 124(1) ? ? ? yes N(1) C(11) C(18) 117(1) ? ? ? yes C(12) C(11) C(18) 117(1) ? ? ? yes C(11) C(12) C(13) 123(1) ? ? ? yes C(11) C(12) C(17) 116(1) ? ? ? yes C(13) C(12) C(17) 119(1) ? ? ? yes C(12) C(13) C(14) 118(1) ? ? ? yes C(13) C(14) C(15) 121(1) ? ? ? yes C(14) C(15) C(16) 118(1) ? ? ? yes C(15) C(16) C(17) 122(1) ? ? ? yes C(12) C(17) C(16) 118(1) ? ? ? yes C(11) C(18) C(19) 118(1) ? ? ? yes C(11) C(18) C(23) 122(1) ? ? ? yes C(19) C(18) C(23) 118(1) ? ? ? yes C(18) C(19) C(20) 119(1) ? ? ? yes C(19) C(20) C(21) 120(1) ? ? ? yes C(20) C(21) C(22) 119(1) ? ? ? yes C(21) C(22) C(23) 119(1) ? ? ? yes C(18) C(23) C(22) 120(1) ? ? ? yes Os(4) C(24) O(12) 175(1) ? ? ? yes Os(4) C(25) O(13) 173(1) ? ? ? yes Os(4) C(26) O(14) 174(1) ? ? ? yes Os(5) C(27) O(15) 177(1) ? ? ? yes Os(5) C(28) O(16) 176(1) ? ? ? yes Os(5) C(29) O(17) 178(2) ? ? ? yes Os(5) C(30) O(18) 173(1) ? ? ? yes Os(6) C(31) O(19) 177(1) ? ? ? yes Os(6) C(32) O(20) 179(1) ? ? ? yes Os(6) C(33) O(21) 178(1) ? ? ? yes N(2) C(34) C(35) 125(1) ? ? ? yes N(2) C(34) C(41) 118(1) ? ? ? yes C(35) C(34) C(41) 116(1) ? ? ? yes C(34) C(35) C(36) 124(1) ? ? ? yes C(34) C(35) C(40) 117(1) ? ? ? yes C(36) C(35) C(40) 117(1) ? ? ? yes C(35) C(36) C(37) 120(1) ? ? ? yes C(36) C(37) C(38) 120(1) ? ? ? yes C(37) C(38) C(39) 119(1) ? ? ? yes C(38) C(39) C(40) 119(1) ? ? ? yes C(35) C(40) C(39) 122(1) ? ? ? yes C(34) C(41) C(42) 122(1) ? ? ? yes C(34) C(41) C(46) 120(1) ? ? ? yes C(42) C(41) C(46) 116(1) ? ? ? yes C(41) C(42) C(43) 121(1) ? ? ? yes C(42) C(43) C(44) 119(1) ? ? ? yes C(43) C(44) C(45) 119(1) ? ? ? yes C(44) C(45) C(46) 119(1) ? ? ? yes C(41) C(46) C(45) 121(1) ? ? ? yes #------------------------------------------------------------------------------ #=================end of file====================== data_wt0337w-JW015-compound 6 _database_code_CSD 174856 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Sep 23 16:21:19 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 12.084(1) _cell_length_b 12.075(1) _cell_length_c 18.003(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.82(2) _cell_angle_gamma 90.00 _cell_volume 2514.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 2.694 _exptl_crystal_density_meas ? _chemical_formula_weight 1019.93 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H11 N O10 Os3 ' _chemical_formula_moiety 'C22 H11 N O10 Os3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1832.00 _exptl_absorpt_coefficient_mu 15.167 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 15646 _reflns_number_total 5891 _reflns_number_observed 4053 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 3.97 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.52 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 12 -1.216 7.603 'International Tables' O 0 40 0.011 0.006 'International Tables' N 0 4 0.006 0.003 'International Tables' C 0 88 0.003 0.002 'International Tables' H 0 44 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) 0.19406(3) -0.33070(3) 0.47371(3) 0.0488(1) Uij ? ? Os(2) 0.28958(4) -0.27772(3) 0.64506(3) 0.0517(1) Uij ? ? Os(3) 0.06389(3) -0.19856(3) 0.55815(3) 0.0496(1) Uij ? ? O(1) 0.2130(9) -0.5784(7) 0.4993(6) 0.106(4) Uij ? ? O(2) 0.0428(8) -0.3730(8) 0.3109(5) 0.092(3) Uij ? ? O(3) 0.5366(8) -0.3612(8) 0.7202(6) 0.100(3) Uij ? ? O(4) 0.3627(8) -0.0376(7) 0.6265(5) 0.084(3) Uij ? ? O(5) 0.246(1) -0.2097(9) 0.7971(7) 0.112(4) Uij ? ? O(6) 0.1707(9) -0.4995(7) 0.6576(7) 0.118(4) Uij ? ? O(7) 0.0710(9) -0.0050(8) 0.6693(6) 0.099(4) Uij ? ? O(8) -0.1720(7) -0.1509(7) 0.4437(6) 0.091(3) Uij ? ? O(9) -0.0363(8) -0.3475(7) 0.6583(6) 0.088(3) Uij ? ? O(10) 0.1382(6) -0.0954(5) 0.4877(4) 0.052(2) Uij ? ? N(1) 0.2058(7) -0.1613(6) 0.4590(4) 0.044(2) Uij ? ? C(1) 0.203(1) -0.4868(9) 0.4893(7) 0.069(4) Uij ? ? C(2) 0.0976(9) -0.3545(9) 0.3730(7) 0.061(3) Uij ? ? C(3) 0.447(1) -0.3306(10) 0.6906(7) 0.069(4) Uij ? ? C(4) 0.335(1) -0.1258(9) 0.6318(6) 0.062(3) Uij ? ? C(5) 0.261(1) -0.235(1) 0.7388(9) 0.079(5) Uij ? ? C(6) 0.214(1) -0.4201(10) 0.6498(7) 0.070(4) Uij ? ? C(7) 0.0691(10) -0.075(1) 0.6274(7) 0.066(4) Uij ? ? C(8) -0.0852(10) -0.1649(9) 0.4857(7) 0.063(4) Uij ? ? C(9) 0.0005(10) -0.2902(10) 0.6196(7) 0.063(3) Uij ? ? C(10) 0.2754(8) -0.1219(8) 0.4218(6) 0.049(3) Uij ? ? C(11) 0.2835(8) -0.0009(9) 0.4035(6) 0.055(3) Uij ? ? C(12) 0.348(1) 0.072(1) 0.4555(7) 0.098(5) Uij ? ? C(13) 0.360(2) 0.181(1) 0.4357(9) 0.107(6) Uij ? ? C(14) 0.299(1) 0.218(1) 0.3653(9) 0.086(5) Uij ? ? C(15) 0.236(2) 0.148(1) 0.3130(9) 0.125(6) Uij ? ? C(16) 0.230(1) 0.038(1) 0.3327(8) 0.107(5) Uij ? ? C(17) 0.3487(9) -0.2070(9) 0.4034(6) 0.054(3) Uij ? ? C(18) 0.4356(9) -0.180(1) 0.3687(7) 0.072(4) Uij ? ? C(19) 0.507(1) -0.264(1) 0.3590(9) 0.092(5) Uij ? ? C(20) 0.494(1) -0.371(1) 0.3819(9) 0.093(5) Uij ? ? C(21) 0.408(1) -0.396(1) 0.4140(8) 0.078(4) Uij ? ? C(22) 0.3338(8) -0.3157(9) 0.4260(6) 0.058(3) Uij ? ? H(1) 0.3852 0.0479 0.5068 0.1174 Uij ? ? H(2) 0.4115 0.2287 0.4714 0.1284 Uij ? ? H(3) 0.3002 0.2946 0.3531 0.1031 Uij ? ? H(4) 0.1953 0.1728 0.2624 0.1504 Uij ? ? H(5) 0.1860 -0.0116 0.2945 0.1288 Uij ? ? H(6) 0.4446 -0.1069 0.3525 0.0868 Uij ? ? H(7) 0.5666 -0.2483 0.3360 0.1099 Uij ? ? H(8) 0.5454 -0.4274 0.3754 0.1110 Uij ? ? H(9) 0.3989 -0.4707 0.4284 0.0932 Uij ? ? H(10) 0.0727 -0.2601 0.4706 0.0608 Uij ? ? H(11) 0.3061 -0.3423 0.5599 0.0608 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0488(2) 0.0398(2) 0.0544(3) -0.0002(2) 0.0093(2) -0.0059(2) Os(2) 0.0524(2) 0.0502(2) 0.0509(3) -0.0077(2) 0.0123(2) 0.0038(2) Os(3) 0.0476(2) 0.0450(2) 0.0602(3) -0.0034(2) 0.0217(2) -0.0016(2) O(1) 0.121(8) 0.043(5) 0.132(9) -0.003(5) 0.001(7) -0.006(5) O(2) 0.092(6) 0.104(7) 0.062(6) -0.030(5) -0.007(5) -0.003(5) O(3) 0.065(6) 0.098(6) 0.122(9) 0.006(5) 0.004(6) 0.043(6) O(4) 0.100(7) 0.064(5) 0.082(6) -0.021(5) 0.018(5) 0.002(4) O(5) 0.137(9) 0.131(8) 0.089(8) -0.038(7) 0.063(7) -0.010(7) O(6) 0.113(8) 0.063(6) 0.18(1) -0.030(5) 0.046(8) 0.024(6) O(7) 0.121(8) 0.080(6) 0.110(8) -0.012(5) 0.057(6) -0.044(6) O(8) 0.063(5) 0.085(6) 0.107(8) 0.018(5) -0.005(5) 0.001(5) O(9) 0.091(6) 0.091(6) 0.098(7) -0.020(5) 0.049(6) 0.009(5) O(10) 0.064(4) 0.044(3) 0.054(4) 0.002(3) 0.025(3) -0.004(3) N(1) 0.048(4) 0.041(4) 0.040(5) -0.005(3) 0.012(4) -0.010(3) C(1) 0.078(8) 0.051(7) 0.061(8) 0.000(5) -0.004(6) -0.009(5) C(2) 0.056(6) 0.060(6) 0.066(8) 0.004(5) 0.017(6) -0.011(5) C(3) 0.068(7) 0.070(7) 0.072(8) -0.001(6) 0.025(7) 0.017(6) C(4) 0.079(8) 0.056(6) 0.052(7) -0.013(6) 0.021(6) -0.002(5) C(5) 0.083(9) 0.087(9) 0.078(10) -0.034(7) 0.040(8) -0.002(7) C(6) 0.067(7) 0.062(7) 0.080(9) -0.009(6) 0.017(6) 0.012(6) C(7) 0.071(7) 0.081(8) 0.058(7) -0.001(6) 0.036(6) -0.002(6) C(8) 0.059(7) 0.058(6) 0.075(8) 0.000(5) 0.024(6) -0.004(6) C(9) 0.062(7) 0.068(7) 0.061(7) -0.005(6) 0.022(6) -0.010(6) C(10) 0.047(5) 0.047(5) 0.052(6) -0.008(4) 0.016(5) -0.011(4) C(11) 0.044(5) 0.074(7) 0.046(6) -0.009(5) 0.012(5) 0.004(5) C(12) 0.17(1) 0.069(8) 0.041(7) -0.035(8) 0.002(8) 0.010(6) C(13) 0.16(2) 0.078(9) 0.08(1) -0.044(10) 0.03(1) 0.001(8) C(14) 0.082(9) 0.072(8) 0.11(1) -0.002(7) 0.035(8) 0.035(8) C(15) 0.14(1) 0.11(1) 0.08(1) -0.05(1) -0.04(1) 0.038(9) C(16) 0.12(1) 0.082(9) 0.080(10) -0.037(8) -0.031(9) 0.025(8) C(17) 0.048(5) 0.071(7) 0.046(6) -0.009(5) 0.018(5) -0.014(5) C(18) 0.053(7) 0.092(9) 0.078(9) -0.009(6) 0.028(6) -0.015(7) C(19) 0.066(8) 0.12(1) 0.10(1) -0.007(8) 0.051(8) -0.042(9) C(20) 0.060(8) 0.11(1) 0.11(1) 0.022(7) 0.018(8) -0.047(9) C(21) 0.063(8) 0.085(9) 0.075(9) 0.007(6) 0.004(7) -0.026(7) C(22) 0.044(5) 0.067(7) 0.054(7) 0.007(5) 0.000(5) -0.019(5) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4053 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0369 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0394 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.995 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.03 _refine_diff_density_max 1.37 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Os(2) 3.0327(6) ? ? yes Os(1) Os(3) 2.9522(6) ? ? yes Os(1) N(1) 2.073(7) ? ? yes Os(1) C(1) 1.90(1) ? ? yes Os(1) C(2) 1.87(1) ? ? yes Os(1) C(22) 2.11(1) ? ? yes Os(2) Os(3) 2.8862(6) ? ? yes Os(2) C(3) 1.95(1) ? ? yes Os(2) C(4) 1.95(1) ? ? yes Os(2) C(5) 1.89(2) ? ? yes Os(2) C(6) 1.96(1) ? ? yes Os(3) O(10) 2.151(7) ? ? yes Os(3) C(7) 1.93(1) ? ? yes Os(3) C(8) 1.94(1) ? ? yes Os(3) C(9) 1.88(1) ? ? yes O(1) C(1) 1.12(1) ? ? yes O(2) C(2) 1.14(1) ? ? yes O(3) C(3) 1.12(1) ? ? yes O(4) C(4) 1.13(1) ? ? yes O(5) C(5) 1.16(2) ? ? yes O(6) C(6) 1.12(1) ? ? yes O(7) C(7) 1.13(1) ? ? yes O(8) C(8) 1.11(1) ? ? yes O(9) C(9) 1.16(1) ? ? yes O(10) N(1) 1.346(9) ? ? yes N(1) C(10) 1.31(1) ? ? yes C(10) C(11) 1.51(1) ? ? yes C(10) C(17) 1.46(1) ? ? yes C(11) C(12) 1.36(1) ? ? yes C(11) C(16) 1.34(2) ? ? yes C(12) C(13) 1.38(2) ? ? yes C(13) C(14) 1.35(2) ? ? yes C(14) C(15) 1.33(2) ? ? yes C(15) C(16) 1.38(2) ? ? yes C(17) C(18) 1.41(1) ? ? yes C(17) C(22) 1.40(1) ? ? yes C(18) C(19) 1.37(2) ? ? yes C(19) C(20) 1.38(2) ? ? yes C(20) C(21) 1.36(2) ? ? yes C(21) C(22) 1.38(1) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Os(2) Os(1) Os(3) 57.65(1) ? ? ? yes Os(2) Os(1) N(1) 84.4(2) ? ? ? yes Os(2) Os(1) C(1) 94.0(3) ? ? ? yes Os(2) Os(1) C(2) 164.7(3) ? ? ? yes Os(2) Os(1) C(22) 106.4(3) ? ? ? yes Os(3) Os(1) N(1) 66.3(2) ? ? ? yes Os(3) Os(1) C(1) 118.3(4) ? ? ? yes Os(3) Os(1) C(2) 107.8(3) ? ? ? yes Os(3) Os(1) C(22) 140.4(3) ? ? ? yes N(1) Os(1) C(1) 173.2(4) ? ? ? yes N(1) Os(1) C(2) 94.2(4) ? ? ? yes N(1) Os(1) C(22) 76.8(4) ? ? ? yes C(1) Os(1) C(2) 89.0(5) ? ? ? yes C(1) Os(1) C(22) 97.4(5) ? ? ? yes C(2) Os(1) C(22) 88.1(4) ? ? ? yes Os(1) Os(2) Os(3) 59.78(1) ? ? ? yes Os(1) Os(2) C(3) 113.4(4) ? ? ? yes Os(1) Os(2) C(4) 96.4(3) ? ? ? yes Os(1) Os(2) C(5) 148.4(4) ? ? ? yes Os(1) Os(2) C(6) 79.3(4) ? ? ? yes Os(3) Os(2) C(3) 172.3(4) ? ? ? yes Os(3) Os(2) C(4) 83.1(3) ? ? ? yes Os(3) Os(2) C(5) 90.3(4) ? ? ? yes Os(3) Os(2) C(6) 86.2(3) ? ? ? yes C(3) Os(2) C(4) 94.7(5) ? ? ? yes C(3) Os(2) C(5) 97.0(6) ? ? ? yes C(3) Os(2) C(6) 96.1(5) ? ? ? yes C(4) Os(2) C(5) 89.1(5) ? ? ? yes C(4) Os(2) C(6) 169.2(5) ? ? ? yes C(5) Os(2) C(6) 89.6(5) ? ? ? yes Os(1) Os(3) Os(2) 62.58(1) ? ? ? yes Os(1) Os(3) O(10) 68.5(2) ? ? ? yes Os(1) Os(3) C(7) 145.7(3) ? ? ? yes Os(1) Os(3) C(8) 107.3(4) ? ? ? yes Os(1) Os(3) C(9) 110.7(3) ? ? ? yes Os(2) Os(3) O(10) 91.2(2) ? ? ? yes Os(2) Os(3) C(7) 93.3(4) ? ? ? yes Os(2) Os(3) C(8) 169.5(3) ? ? ? yes Os(2) Os(3) C(9) 88.2(3) ? ? ? yes O(10) Os(3) C(7) 89.6(4) ? ? ? yes O(10) Os(3) C(8) 87.0(4) ? ? ? yes O(10) Os(3) C(9) 179.2(4) ? ? ? yes C(7) Os(3) C(8) 97.0(5) ? ? ? yes C(7) Os(3) C(9) 91.0(5) ? ? ? yes C(8) Os(3) C(9) 93.5(5) ? ? ? yes Os(3) O(10) N(1) 106.7(5) ? ? ? yes Os(1) N(1) O(10) 117.6(6) ? ? ? yes Os(1) N(1) C(10) 120.2(6) ? ? ? yes O(10) N(1) C(10) 122.2(7) ? ? ? yes Os(1) C(1) O(1) 176(1) ? ? ? yes Os(1) C(2) O(2) 176(1) ? ? ? yes Os(2) C(3) O(3) 176(1) ? ? ? yes Os(2) C(4) O(4) 177(1) ? ? ? yes Os(2) C(5) O(5) 178(1) ? ? ? yes Os(2) C(6) O(6) 175(1) ? ? ? yes Os(3) C(7) O(7) 177(1) ? ? ? yes Os(3) C(8) O(8) 176(1) ? ? ? yes Os(3) C(9) O(9) 178(1) ? ? ? yes N(1) C(10) C(11) 123.9(9) ? ? ? yes N(1) C(10) C(17) 112.5(8) ? ? ? yes C(11) C(10) C(17) 123.5(9) ? ? ? yes C(10) C(11) C(12) 122.8(10) ? ? ? yes C(10) C(11) C(16) 120.4(10) ? ? ? yes C(12) C(11) C(16) 116(1) ? ? ? yes C(11) C(12) C(13) 121(1) ? ? ? yes C(12) C(13) C(14) 119(1) ? ? ? yes C(13) C(14) C(15) 119(1) ? ? ? yes C(14) C(15) C(16) 119(1) ? ? ? yes C(11) C(16) C(15) 122(1) ? ? ? yes C(10) C(17) C(18) 121(1) ? ? ? yes C(10) C(17) C(22) 117.2(9) ? ? ? yes C(18) C(17) C(22) 121(1) ? ? ? yes C(17) C(18) C(19) 117(1) ? ? ? yes C(18) C(19) C(20) 121(1) ? ? ? yes C(19) C(20) C(21) 120(1) ? ? ? yes C(20) C(21) C(22) 121(1) ? ? ? yes Os(1) C(22) C(17) 112.6(7) ? ? ? yes Os(1) C(22) C(21) 129.4(9) ? ? ? yes C(17) C(22) C(21) 118(1) ? ? ? yes #------------------------------------------------------------------------------ #=================================end of file=============================== data_wt0300w-JW013-compound_7 _database_code_CSD 174857 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Sep 23 16:16:58 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.142(2) _cell_length_b 10.612(2) _cell_length_c 13.508(1) _cell_angle_alpha 97.08(1) _cell_angle_beta 99.07(1) _cell_angle_gamma 111.95(2) _cell_volume 1305.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 2.667 _exptl_crystal_density_meas ? _chemical_formula_weight 1047.94 _chemical_formula_analytical ? _chemical_formula_sum 'C23 H11 N O11 Os3 ' _chemical_formula_moiety 'C23 H11 N O11 Os3 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 944.00 _exptl_absorpt_coefficient_mu 14.620 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 8113 _reflns_number_total 5629 _reflns_number_observed 4613 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 2.12 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.52 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 6 -1.216 7.603 'International Tables' C 0 46 0.003 0.002 'International Tables' N 0 2 0.006 0.003 'International Tables' O 0 22 0.011 0.006 'International Tables' H 0 22 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) 0.18237(4) 0.41263(4) 0.83532(3) 0.0442(1) Uij ? ? Os(2) -0.00220(4) 0.48587(4) 0.69137(3) 0.0463(1) Uij ? ? Os(3) -0.15570(4) 0.28574(4) 0.80128(3) 0.0456(1) Uij ? ? O(1) 0.3744(10) 0.3410(9) 0.9978(7) 0.083(3) Uij ? ? O(2) 0.3599(9) 0.3958(9) 0.6798(7) 0.076(3) Uij ? ? O(3) 0.3713(10) 0.7217(9) 0.9074(8) 0.093(3) Uij ? ? O(4) 0.245(1) 0.6924(9) 0.6164(7) 0.083(3) Uij ? ? O(5) 0.0125(10) 0.6942(9) 0.8765(6) 0.077(3) Uij ? ? O(6) -0.275(1) 0.495(1) 0.5630(8) 0.111(4) Uij ? ? O(7) -0.0076(9) 0.2362(8) 0.5453(6) 0.069(2) Uij ? ? O(8) -0.345(1) 0.443(1) 0.8450(8) 0.093(4) Uij ? ? O(9) -0.3685(8) 0.1386(10) 0.5996(6) 0.075(3) Uij ? ? O(10) -0.3023(9) 0.074(1) 0.9266(6) 0.081(3) Uij ? ? O(11) 0.0243(7) 0.4104(7) 0.9247(5) 0.055(2) Uij ? ? N(1) 0.0095(8) 0.2146(7) 0.7836(5) 0.038(2) Uij ? ? C(1) 0.297(1) 0.365(1) 0.9363(9) 0.059(3) Uij ? ? C(2) 0.294(1) 0.402(1) 0.7404(8) 0.052(3) Uij ? ? C(3) 0.302(1) 0.607(1) 0.8803(8) 0.059(3) Uij ? ? C(4) 0.151(1) 0.617(1) 0.6439(8) 0.056(3) Uij ? ? C(5) 0.008(1) 0.617(1) 0.8051(8) 0.054(3) Uij ? ? C(6) -0.173(1) 0.493(1) 0.6098(9) 0.072(4) Uij ? ? C(7) -0.0069(10) 0.328(1) 0.5990(7) 0.044(3) Uij ? ? C(8) -0.273(1) 0.385(1) 0.8287(9) 0.063(4) Uij ? ? C(9) -0.290(1) 0.190(1) 0.6776(8) 0.052(3) Uij ? ? C(10) -0.241(1) 0.153(1) 0.8805(8) 0.056(3) Uij ? ? C(11) 0.0059(9) 0.0942(9) 0.7550(6) 0.040(2) Uij ? ? C(12) 0.1405(10) 0.0658(9) 0.7535(7) 0.045(3) Uij ? ? C(13) 0.215(1) 0.044(1) 0.8400(9) 0.059(3) Uij ? ? C(14) 0.333(1) 0.012(1) 0.8378(9) 0.062(3) Uij ? ? C(15) 0.378(1) 0.000(1) 0.749(1) 0.066(4) Uij ? ? C(16) 0.306(1) 0.022(1) 0.6621(9) 0.063(4) Uij ? ? C(17) 0.188(1) 0.054(1) 0.6633(8) 0.059(3) Uij ? ? C(18) -0.134(1) -0.0347(10) 0.7206(8) 0.046(3) Uij ? ? C(19) -0.211(1) -0.071(1) 0.6205(9) 0.074(4) Uij ? ? C(20) -0.339(1) -0.189(1) 0.588(1) 0.086(4) Uij ? ? C(21) -0.389(1) -0.274(1) 0.652(1) 0.080(4) Uij ? ? C(22) -0.313(2) -0.239(1) 0.753(1) 0.092(5) Uij ? ? C(23) -0.186(1) -0.122(1) 0.784(1) 0.077(4) Uij ? ? H(1) 0.1837 0.0515 0.9023 0.0712 Uij ? ? H(2) 0.3839 -0.0028 0.8979 0.0743 Uij ? ? H(3) 0.4597 -0.0224 0.7466 0.0792 Uij ? ? H(4) 0.3392 0.0140 0.6004 0.0760 Uij ? ? H(5) 0.1383 0.0679 0.6026 0.0705 Uij ? ? H(6) -0.1748 -0.0154 0.5730 0.0885 Uij ? ? H(7) -0.3934 -0.2101 0.5197 0.1032 Uij ? ? H(8) -0.4742 -0.3565 0.6284 0.0963 Uij ? ? H(9) -0.3493 -0.2952 0.8001 0.1106 Uij ? ? H(10) -0.1324 -0.1007 0.8530 0.0925 Uij ? ? H(11) 0.0208 0.3751 0.9810 0.0782 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0414(2) 0.0461(2) 0.0440(2) 0.0198(2) -0.0001(2) 0.0090(2) Os(2) 0.0513(2) 0.0528(2) 0.0401(2) 0.0277(2) 0.0048(2) 0.0124(2) Os(3) 0.0422(2) 0.0595(2) 0.0403(2) 0.0256(2) 0.0087(2) 0.0111(2) O(1) 0.083(6) 0.089(6) 0.076(6) 0.047(5) -0.016(5) 0.017(5) O(2) 0.067(5) 0.076(6) 0.084(6) 0.022(4) 0.027(5) 0.021(5) O(3) 0.072(6) 0.052(5) 0.130(8) 0.020(4) -0.026(5) 0.003(5) O(4) 0.090(6) 0.060(5) 0.092(7) 0.016(5) 0.033(5) 0.016(5) O(5) 0.102(7) 0.074(5) 0.064(5) 0.051(5) 0.014(5) 0.005(4) O(6) 0.110(8) 0.16(1) 0.086(7) 0.095(8) -0.019(6) 0.006(7) O(7) 0.084(6) 0.068(5) 0.056(5) 0.038(4) 0.003(4) 0.008(4) O(8) 0.092(7) 0.119(8) 0.103(7) 0.078(6) 0.032(6) 0.019(6) O(9) 0.055(4) 0.107(7) 0.053(5) 0.029(4) 0.000(4) 0.005(4) O(10) 0.075(5) 0.112(7) 0.062(5) 0.029(5) 0.030(4) 0.043(5) O(11) 0.060(4) 0.075(5) 0.034(3) 0.032(4) 0.008(3) 0.007(3) N(1) 0.040(4) 0.047(4) 0.031(4) 0.018(3) 0.006(3) 0.014(3) C(1) 0.050(6) 0.052(6) 0.067(7) 0.018(5) -0.005(5) 0.012(5) C(2) 0.043(5) 0.056(6) 0.058(6) 0.016(5) 0.019(5) 0.021(5) C(3) 0.056(6) 0.062(7) 0.057(6) 0.028(6) -0.003(5) 0.009(5) C(4) 0.073(7) 0.053(6) 0.047(6) 0.030(6) 0.010(5) 0.013(5) C(5) 0.059(6) 0.064(6) 0.047(6) 0.034(5) 0.011(5) 0.015(5) C(6) 0.077(8) 0.092(9) 0.056(7) 0.053(7) -0.005(6) 0.005(6) C(7) 0.045(5) 0.056(6) 0.037(5) 0.019(4) 0.020(4) 0.019(4) C(8) 0.061(7) 0.081(8) 0.057(7) 0.037(6) 0.011(5) 0.019(6) C(9) 0.043(5) 0.078(7) 0.043(5) 0.027(5) 0.018(5) 0.018(5) C(10) 0.053(6) 0.069(7) 0.047(6) 0.028(5) 0.008(5) 0.008(5) C(11) 0.041(5) 0.049(5) 0.031(4) 0.018(4) 0.009(4) 0.014(4) C(12) 0.039(5) 0.042(5) 0.052(6) 0.016(4) 0.010(4) 0.010(4) C(13) 0.063(6) 0.066(7) 0.065(7) 0.041(6) 0.014(5) 0.025(5) C(14) 0.062(7) 0.079(8) 0.058(7) 0.038(6) 0.014(6) 0.027(6) C(15) 0.048(6) 0.060(6) 0.093(9) 0.026(5) 0.011(6) 0.015(6) C(16) 0.063(7) 0.087(8) 0.054(6) 0.038(6) 0.029(6) 0.017(6) C(17) 0.062(6) 0.076(7) 0.047(6) 0.037(6) 0.010(5) 0.018(5) C(18) 0.045(5) 0.051(5) 0.051(6) 0.022(4) 0.022(4) 0.019(4) C(19) 0.073(8) 0.068(7) 0.054(7) 0.001(6) 0.008(6) 0.015(6) C(20) 0.060(7) 0.074(8) 0.09(1) 0.001(6) -0.002(7) 0.014(7) C(21) 0.055(7) 0.069(8) 0.10(1) 0.009(6) 0.006(7) 0.025(7) C(22) 0.075(9) 0.065(8) 0.15(1) 0.019(7) 0.044(9) 0.060(9) C(23) 0.074(8) 0.074(8) 0.080(9) 0.021(7) 0.011(7) 0.037(7) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4613 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0384 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0460 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.315 _refine_ls_shift/esd_max 0.0020 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.41 _refine_diff_density_max 1.98 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Os(2) 2.8639(5) ? ? yes Os(1) O(11) 2.149(7) ? ? yes Os(1) N(1) 2.116(7) ? ? yes Os(1) C(1) 1.90(1) ? ? yes Os(1) C(2) 1.86(1) ? ? yes Os(1) C(3) 1.92(1) ? ? yes Os(2) Os(3) 2.8587(6) ? ? yes Os(2) C(4) 1.92(1) ? ? yes Os(2) C(5) 1.90(1) ? ? yes Os(2) C(6) 1.93(1) ? ? yes Os(2) C(7) 1.94(1) ? ? yes Os(3) O(11) 2.134(6) ? ? yes Os(3) N(1) 2.112(7) ? ? yes Os(3) C(8) 1.91(1) ? ? yes Os(3) C(9) 1.87(1) ? ? yes Os(3) C(10) 1.91(1) ? ? yes O(1) C(1) 1.16(1) ? ? yes O(2) C(2) 1.15(1) ? ? yes O(3) C(3) 1.13(1) ? ? yes O(4) C(4) 1.14(1) ? ? yes O(5) C(5) 1.17(1) ? ? yes O(6) C(6) 1.13(1) ? ? yes O(7) C(7) 1.14(1) ? ? yes O(8) C(8) 1.14(1) ? ? yes O(9) C(9) 1.15(1) ? ? yes O(10) C(10) 1.15(1) ? ? yes N(1) C(11) 1.27(1) ? ? yes C(11) C(12) 1.51(1) ? ? yes C(11) C(18) 1.51(1) ? ? yes C(12) C(13) 1.38(1) ? ? yes C(12) C(17) 1.39(1) ? ? yes C(13) C(14) 1.37(1) ? ? yes C(14) C(15) 1.36(2) ? ? yes C(15) C(16) 1.37(2) ? ? yes C(16) C(17) 1.37(1) ? ? yes C(18) C(19) 1.38(1) ? ? yes C(18) C(23) 1.36(2) ? ? yes C(19) C(20) 1.39(2) ? ? yes C(20) C(21) 1.34(2) ? ? yes C(21) C(22) 1.38(2) ? ? yes C(22) C(23) 1.37(2) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Os(2) Os(1) O(11) 82.3(2) ? ? ? yes Os(2) Os(1) N(1) 81.8(2) ? ? ? yes Os(2) Os(1) C(1) 176.5(4) ? ? ? yes Os(2) Os(1) C(2) 90.6(3) ? ? ? yes Os(2) Os(1) C(3) 87.5(3) ? ? ? yes O(11) Os(1) N(1) 74.6(3) ? ? ? yes O(11) Os(1) C(1) 94.3(4) ? ? ? yes O(11) Os(1) C(2) 170.9(3) ? ? ? yes O(11) Os(1) C(3) 95.4(4) ? ? ? yes N(1) Os(1) C(1) 97.6(4) ? ? ? yes N(1) Os(1) C(2) 98.9(4) ? ? ? yes N(1) Os(1) C(3) 166.2(4) ? ? ? yes C(1) Os(1) C(2) 92.8(5) ? ? ? yes C(1) Os(1) C(3) 92.6(4) ? ? ? yes C(2) Os(1) C(3) 89.9(5) ? ? ? yes Os(1) Os(2) Os(3) 65.87(1) ? ? ? yes Os(1) Os(2) C(4) 96.5(3) ? ? ? yes Os(1) Os(2) C(5) 84.8(3) ? ? ? yes Os(1) Os(2) C(6) 162.1(4) ? ? ? yes Os(1) Os(2) C(7) 83.8(3) ? ? ? yes Os(3) Os(2) C(4) 162.4(3) ? ? ? yes Os(3) Os(2) C(5) 84.1(3) ? ? ? yes Os(3) Os(2) C(6) 96.3(4) ? ? ? yes Os(3) Os(2) C(7) 85.4(3) ? ? ? yes C(4) Os(2) C(5) 94.2(4) ? ? ? yes C(4) Os(2) C(6) 101.4(5) ? ? ? yes C(4) Os(2) C(7) 93.4(4) ? ? ? yes C(5) Os(2) C(6) 94.1(4) ? ? ? yes C(5) Os(2) C(7) 166.9(4) ? ? ? yes C(6) Os(2) C(7) 94.9(4) ? ? ? yes Os(2) Os(3) O(11) 82.7(2) ? ? ? yes Os(2) Os(3) N(1) 82.0(2) ? ? ? yes Os(2) Os(3) C(8) 91.1(4) ? ? ? yes Os(2) Os(3) C(9) 87.7(3) ? ? ? yes Os(2) Os(3) C(10) 174.7(3) ? ? ? yes O(11) Os(3) N(1) 75.0(3) ? ? ? yes O(11) Os(3) C(8) 95.1(4) ? ? ? yes O(11) Os(3) C(9) 169.5(3) ? ? ? yes O(11) Os(3) C(10) 93.3(4) ? ? ? yes N(1) Os(3) C(8) 168.4(4) ? ? ? yes N(1) Os(3) C(9) 99.5(4) ? ? ? yes N(1) Os(3) C(10) 93.7(4) ? ? ? yes C(8) Os(3) C(9) 89.4(5) ? ? ? yes C(8) Os(3) C(10) 92.7(5) ? ? ? yes C(9) Os(3) C(10) 96.0(4) ? ? ? yes Os(1) O(11) Os(3) 93.2(2) ? ? ? yes Os(1) N(1) Os(3) 94.8(3) ? ? ? yes Os(1) N(1) C(11) 132.8(6) ? ? ? yes Os(3) N(1) C(11) 132.4(6) ? ? ? yes Os(1) C(1) O(1) 176.5(10) ? ? ? yes Os(1) C(2) O(2) 178.0(9) ? ? ? yes Os(1) C(3) O(3) 179(1) ? ? ? yes Os(2) C(4) O(4) 177.7(10) ? ? ? yes Os(2) C(5) O(5) 177(1) ? ? ? yes Os(2) C(6) O(6) 178(1) ? ? ? yes Os(2) C(7) O(7) 179.0(8) ? ? ? yes Os(3) C(8) O(8) 178(1) ? ? ? yes Os(3) C(9) O(9) 175(1) ? ? ? yes Os(3) C(10) O(10) 174.8(9) ? ? ? yes N(1) C(11) C(12) 123.4(8) ? ? ? yes N(1) C(11) C(18) 123.1(8) ? ? ? yes C(12) C(11) C(18) 113.4(8) ? ? ? yes C(11) C(12) C(13) 121.1(9) ? ? ? yes C(11) C(12) C(17) 120.4(8) ? ? ? yes C(13) C(12) C(17) 118.4(9) ? ? ? yes C(12) C(13) C(14) 121(1) ? ? ? yes C(13) C(14) C(15) 119(1) ? ? ? yes C(14) C(15) C(16) 120.6(10) ? ? ? yes C(15) C(16) C(17) 120(1) ? ? ? yes C(12) C(17) C(16) 119.6(9) ? ? ? yes C(11) C(18) C(19) 120.3(9) ? ? ? yes C(11) C(18) C(23) 122.2(9) ? ? ? yes C(19) C(18) C(23) 117.5(10) ? ? ? yes C(18) C(19) C(20) 120(1) ? ? ? yes C(19) C(20) C(21) 120(1) ? ? ? yes C(20) C(21) C(22) 119(1) ? ? ? yes C(21) C(22) C(23) 119(1) ? ? ? yes C(18) C(23) C(22) 122(1) ? ? ? yes #------------------------------------------------------------------------------ #=================================end of file=============================== data_wt0350w-JW016-compound_8 _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Wong, W.-T.' 'Wong, J.S.-Y' _publ_contact_author_name 'Dr W.-T. Wong' _publ_contact_author_address ; Department of Chemistry The University of Hong Kong Pokfulam Road Hong Kong ; _publ_contact_author_email 'WTWONG@HKUCC.HKU.HK' _publ_section_title ; Synthesis, structural characterization and reactivity of troismium carbonyl clusters containing oxime ligands. ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _database_code_CSD 174858 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Aug 10 12:32:42 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 12.960(1) _cell_length_b 18.167(1) _cell_length_c 18.872(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.67(1) _cell_angle_gamma 90.00 _cell_volume 4443.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 2.936 _exptl_crystal_density_meas ? _chemical_formula_weight 1963.81 _chemical_formula_analytical ? _chemical_formula_sum 'C42 H18 N2 O17 Os6 ' _chemical_formula_moiety 'C42 H18 N2 O17 Os6 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3504.00 _exptl_absorpt_coefficient_mu 17.157 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l _diffrn_reflns_number 27603 _reflns_number_total 10322 _reflns_number_observed 5423 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 5.28 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 24 -1.216 7.603 'International Tables' O 0 68 0.011 0.006 'International Tables' C 0 168 0.003 0.002 'International Tables' N 0 8 0.006 0.003 'International Tables' H 0 72 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) 0.65044(6) 0.03305(5) 0.21405(5) 0.0451(2) Uij ? ? Os(2) 0.67579(6) 0.19107(4) 0.20860(4) 0.0403(2) Uij ? ? Os(3) 0.59704(6) 0.26550(5) 0.08815(5) 0.0479(3) Uij ? ? Os(4) 0.66395(6) 0.11404(4) 0.08562(4) 0.0412(2) Uij ? ? Os(5) 0.87944(5) 0.13299(4) 0.22791(4) 0.0357(2) Uij ? ? Os(6) 0.84029(6) 0.19913(4) 0.03727(4) 0.0397(2) Uij ? ? O(1) 0.660(1) -0.0196(9) 0.3669(10) 0.090(5) Uij ? ? O(2) 0.595(1) -0.1162(9) 0.1561(9) 0.084(5) Uij ? ? O(3) 0.420(1) 0.061(1) 0.2169(10) 0.103(6) Uij ? ? O(4) 0.736(1) 0.3454(9) 0.2532(9) 0.083(5) Uij ? ? O(5) 0.473(1) 0.2198(10) 0.280(1) 0.095(5) Uij ? ? O(6) 0.7240(8) 0.1463(6) 0.3519(6) 0.028(3) Uij ? ? O(7) 0.533(1) 0.4055(10) 0.1634(9) 0.090(5) Uij ? ? O(8) 0.527(1) 0.3178(10) -0.057(1) 0.094(5) Uij ? ? O(9) 0.381(1) 0.2069(9) 0.1156(9) 0.086(5) Uij ? ? O(10) 0.761(1) -0.0294(8) 0.0355(8) 0.067(4) Uij ? ? O(11) 0.453(1) 0.0544(9) 0.0522(9) 0.092(5) Uij ? ? O(12) 0.641(1) 0.1583(9) -0.0671(9) 0.075(5) Uij ? ? O(13) 0.975(1) 0.2847(8) 0.2299(8) 0.069(4) Uij ? ? O(14) 0.972(1) 0.0998(9) 0.3689(9) 0.079(5) Uij ? ? O(15) 0.991(1) 0.0751(8) 0.0140(8) 0.068(4) Uij ? ? O(16) 0.865(1) 0.2293(9) -0.1159(9) 0.077(5) Uij ? ? O(17) 0.7941(9) 0.1609(6) 0.1388(7) 0.040(4) Uij ? ? N(1) 0.8125(10) 0.0306(7) 0.2125(7) 0.033(4) Uij ? ? N(2) 0.752(1) 0.2906(8) 0.0657(7) 0.038(5) Uij ? ? C(1) 0.654(1) 0.000(1) 0.308(1) 0.050(5) Uij ? ? C(2) 0.621(2) -0.061(1) 0.178(1) 0.056(5) Uij ? ? C(3) 0.510(2) 0.050(1) 0.218(1) 0.071(6) Uij ? ? C(4) 0.709(2) 0.288(1) 0.234(1) 0.058(6) Uij ? ? C(5) 0.550(2) 0.207(1) 0.250(1) 0.067(6) Uij ? ? C(6) 0.721(1) 0.1537(9) 0.3118(10) 0.025(4) Uij ? ? C(7) 0.558(2) 0.352(1) 0.130(1) 0.075(7) Uij ? ? C(8) 0.552(2) 0.295(1) -0.001(1) 0.069(6) Uij ? ? C(9) 0.465(2) 0.231(1) 0.106(1) 0.069(6) Uij ? ? C(10) 0.726(2) 0.025(1) 0.059(1) 0.052(5) Uij ? ? C(11) 0.535(2) 0.082(2) 0.065(2) 0.101(8) Uij ? ? C(12) 0.645(2) 0.154(1) -0.009(2) 0.085(7) Uij ? ? C(13) 0.939(1) 0.226(1) 0.230(1) 0.052(5) Uij ? ? C(14) 0.934(2) 0.115(1) 0.311(1) 0.059(6) Uij ? ? C(15) 0.931(1) 0.120(1) 0.023(1) 0.049(5) Uij ? ? C(16) 0.856(1) 0.218(1) -0.056(1) 0.051(5) Uij ? ? C(17) 0.878(1) -0.0216(9) 0.1979(9) 0.032(5) Uij ? ? C(18) 0.847(1) -0.1019(10) 0.1951(10) 0.039(6) Uij ? ? C(19) 0.812(2) -0.1339(10) 0.255(1) 0.049(6) Uij ? ? C(20) 0.779(2) -0.207(1) 0.257(1) 0.064(8) Uij ? ? C(21) 0.789(2) -0.250(1) 0.198(2) 0.073(9) Uij ? ? C(22) 0.824(2) -0.219(1) 0.138(1) 0.066(8) Uij ? ? C(23) 0.857(2) -0.146(1) 0.135(1) 0.055(7) Uij ? ? C(24) 0.987(1) -0.002(1) 0.1826(9) 0.041(6) Uij ? ? C(25) 1.065(1) -0.048(1) 0.163(1) 0.047(6) Uij ? ? C(26) 1.159(2) -0.021(1) 0.147(1) 0.058(7) Uij ? ? C(27) 1.177(1) 0.053(1) 0.148(1) 0.050(7) Uij ? ? C(28) 1.103(2) 0.101(1) 0.172(1) 0.050(7) Uij ? ? C(29) 1.005(1) 0.0745(9) 0.1915(10) 0.035(5) Uij ? ? C(30) 0.803(1) 0.3518(10) 0.068(1) 0.045(6) Uij ? ? C(31) 0.757(2) 0.425(1) 0.083(1) 0.048(6) Uij ? ? C(32) 0.691(2) 0.459(1) 0.032(1) 0.063(8) Uij ? ? C(33) 0.648(2) 0.525(1) 0.043(1) 0.080(9) Uij ? ? C(34) 0.675(2) 0.562(1) 0.102(2) 0.079(10) Uij ? ? C(35) 0.740(2) 0.535(1) 0.150(1) 0.067(8) Uij ? ? C(36) 0.784(2) 0.465(1) 0.141(1) 0.058(7) Uij ? ? C(37) 0.918(1) 0.349(1) 0.061(1) 0.048(6) Uij ? ? C(38) 0.985(2) 0.406(1) 0.062(1) 0.050(7) Uij ? ? C(39) 1.089(2) 0.398(1) 0.054(1) 0.060(8) Uij ? ? C(40) 1.131(2) 0.327(2) 0.048(1) 0.075(9) Uij ? ? C(41) 1.063(2) 0.268(1) 0.046(1) 0.051(7) Uij ? ? C(42) 0.955(1) 0.274(1) 0.0505(10) 0.044(6) Uij ? ? H(1) 0.8087 -0.1052 0.2969 0.0593 Uij ? ? H(2) 0.7502 -0.2264 0.2994 0.0774 Uij ? ? H(3) 0.7721 -0.3007 0.1992 0.0878 Uij ? ? H(4) 0.8264 -0.2481 0.0957 0.0797 Uij ? ? H(5) 0.8855 -0.1265 0.0933 0.0662 Uij ? ? H(6) 1.0532 -0.1000 0.1610 0.0560 Uij ? ? H(7) 1.2135 -0.0534 0.1349 0.0694 Uij ? ? H(8) 1.2412 0.0723 0.1319 0.0598 Uij ? ? H(9) 1.1176 0.1519 0.1755 0.0602 Uij ? ? H(10) 0.6774 0.4334 -0.0111 0.0759 Uij ? ? H(11) 0.5994 0.5447 0.0101 0.0964 Uij ? ? H(12) 0.6464 0.6100 0.1086 0.0950 Uij ? ? H(13) 0.7571 0.5630 0.1914 0.0806 Uij ? ? H(14) 0.8310 0.4460 0.1750 0.0691 Uij ? ? H(15) 0.9587 0.4543 0.0684 0.0605 Uij ? ? H(16) 1.1325 0.4396 0.0533 0.0722 Uij ? ? H(17) 1.2032 0.3204 0.0453 0.0895 Uij ? ? H(18) 1.0917 0.2199 0.0404 0.0609 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0365(4) 0.0497(5) 0.0493(6) -0.0053(4) 0.0084(4) 0.0008(4) Os(2) 0.0379(4) 0.0455(5) 0.0378(5) 0.0048(4) 0.0069(3) -0.0058(4) Os(3) 0.0431(5) 0.0528(5) 0.0478(6) 0.0149(4) 0.0003(4) -0.0032(4) Os(4) 0.0386(4) 0.0464(5) 0.0385(5) 0.0012(4) -0.0008(3) -0.0066(4) Os(5) 0.0372(4) 0.0369(4) 0.0330(5) -0.0002(3) 0.0012(3) -0.0027(3) Os(6) 0.0486(5) 0.0379(4) 0.0328(5) 0.0087(4) 0.0061(4) 0.0000(4) O(17) 0.038(7) 0.027(6) 0.054(9) 0.006(5) 0.004(6) -0.002(6) N(1) 0.032(8) 0.028(8) 0.038(10) -0.001(6) 0.000(7) -0.007(7) N(2) 0.034(8) 0.050(10) 0.028(9) 0.013(7) -0.001(7) -0.015(8) C(17) 0.04(1) 0.027(9) 0.03(1) -0.007(8) -0.006(8) 0.009(8) C(18) 0.05(1) 0.03(1) 0.03(1) -0.003(9) 0.003(9) 0.013(9) C(19) 0.07(1) 0.025(10) 0.05(1) 0.010(10) -0.01(1) -0.002(10) C(20) 0.05(1) 0.04(1) 0.10(2) -0.01(1) 0.01(1) 0.03(1) C(21) 0.09(2) 0.04(1) 0.09(2) -0.02(1) 0.01(2) 0.00(1) C(22) 0.09(2) 0.05(1) 0.06(2) -0.02(1) 0.01(1) -0.01(1) C(23) 0.06(1) 0.06(1) 0.05(1) -0.01(1) 0.01(1) -0.01(1) C(24) 0.04(1) 0.06(1) 0.03(1) 0.004(9) -0.002(8) 0.010(9) C(25) 0.04(1) 0.05(1) 0.06(1) -0.007(9) 0.018(10) -0.01(1) C(26) 0.06(1) 0.04(1) 0.07(2) 0.01(1) 0.02(1) 0.00(1) C(27) 0.03(1) 0.06(1) 0.05(1) 0.008(10) 0.001(9) 0.01(1) C(28) 0.06(1) 0.05(1) 0.04(1) -0.02(1) 0.00(1) 0.00(1) C(29) 0.04(1) 0.026(10) 0.04(1) 0.003(8) -0.006(9) -0.003(8) C(30) 0.05(1) 0.03(1) 0.05(1) 0.012(9) 0.01(1) -0.003(10) C(31) 0.07(1) 0.05(1) 0.03(1) 0.01(1) -0.01(1) -0.003(10) C(32) 0.08(2) 0.07(2) 0.04(1) 0.02(1) 0.01(1) -0.01(1) C(33) 0.12(2) 0.07(2) 0.05(2) 0.05(2) -0.03(2) -0.01(1) C(34) 0.09(2) 0.06(2) 0.10(2) 0.04(1) 0.00(2) 0.01(2) C(35) 0.12(2) 0.05(1) 0.03(1) -0.01(1) 0.00(1) -0.02(1) C(36) 0.08(2) 0.05(1) 0.05(2) 0.01(1) 0.00(1) 0.01(1) C(37) 0.05(1) 0.04(1) 0.06(1) 0.003(9) -0.02(1) 0.01(1) C(38) 0.06(1) 0.05(1) 0.04(1) -0.01(1) 0.01(1) -0.02(1) C(39) 0.07(2) 0.06(2) 0.04(1) -0.03(1) 0.00(1) 0.00(1) C(40) 0.06(2) 0.10(2) 0.07(2) -0.01(1) 0.01(1) 0.00(2) C(41) 0.05(1) 0.06(1) 0.04(1) 0.01(1) 0.012(10) 0.00(1) C(42) 0.04(1) 0.05(1) 0.04(1) 0.003(10) 0.012(9) -0.004(10) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5423 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0511 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0459 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 0.882 _refine_ls_shift/esd_max 0.0040 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.69 _refine_diff_density_max 2.55 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Os(2) 2.891(1) ? ? yes Os(1) Os(4) 2.842(1) ? ? yes Os(1) N(1) 2.10(1) ? ? yes Os(1) C(1) 1.87(2) ? ? yes Os(1) C(2) 1.87(2) ? ? yes Os(1) C(3) 1.85(2) ? ? yes Os(2) Os(3) 2.825(1) ? ? yes Os(2) Os(4) 2.713(1) ? ? yes Os(2) Os(5) 2.862(1) ? ? yes Os(2) O(17) 2.11(1) ? ? yes Os(2) C(4) 1.88(2) ? ? yes Os(2) C(5) 1.84(2) ? ? yes Os(2) C(6) 2.14(2) ? ? yes Os(3) Os(4) 2.885(1) ? ? yes Os(3) N(2) 2.11(1) ? ? yes Os(3) C(7) 1.84(3) ? ? yes Os(3) C(8) 1.86(3) ? ? yes Os(3) C(9) 1.86(2) ? ? yes Os(4) Os(6) 2.914(1) ? ? yes Os(4) O(17) 2.13(1) ? ? yes Os(4) C(10) 1.88(2) ? ? yes Os(4) C(11) 1.81(3) ? ? yes Os(4) C(12) 1.95(3) ? ? yes Os(5) O(17) 2.07(1) ? ? yes Os(5) N(1) 2.07(1) ? ? yes Os(5) C(13) 1.86(2) ? ? yes Os(5) C(14) 1.74(2) ? ? yes Os(5) C(29) 2.06(2) ? ? yes Os(6) O(17) 2.13(1) ? ? yes Os(6) N(2) 2.09(1) ? ? yes Os(6) C(15) 1.88(2) ? ? yes Os(6) C(16) 1.80(2) ? ? yes Os(6) C(42) 2.03(2) ? ? yes O(1) C(1) 1.17(2) ? ? yes O(2) C(2) 1.14(2) ? ? yes O(3) C(3) 1.18(2) ? ? yes O(4) C(4) 1.15(2) ? ? yes O(5) C(5) 1.19(2) ? ? yes O(6) C(6) 0.77(2) ? ? yes O(7) C(7) 1.20(3) ? ? yes O(8) C(8) 1.17(3) ? ? yes O(9) C(9) 1.19(2) ? ? yes O(10) C(10) 1.17(2) ? ? yes O(11) C(11) 1.20(3) ? ? yes O(12) C(12) 1.09(3) ? ? yes O(13) C(13) 1.17(2) ? ? yes O(14) C(14) 1.23(2) ? ? yes O(15) C(15) 1.14(2) ? ? yes O(16) C(16) 1.16(2) ? ? yes N(1) C(17) 1.30(2) ? ? yes N(2) C(30) 1.29(2) ? ? yes C(17) C(18) 1.51(2) ? ? yes C(17) C(24) 1.49(2) ? ? yes C(18) C(19) 1.35(2) ? ? yes C(18) C(23) 1.39(3) ? ? yes C(19) C(20) 1.39(3) ? ? yes C(20) C(21) 1.38(3) ? ? yes C(21) C(22) 1.35(3) ? ? yes C(22) C(23) 1.40(3) ? ? yes C(24) C(25) 1.37(2) ? ? yes C(24) C(29) 1.42(2) ? ? yes C(25) C(26) 1.36(3) ? ? yes C(26) C(27) 1.37(3) ? ? yes C(27) C(28) 1.37(3) ? ? yes C(28) C(29) 1.41(2) ? ? yes C(30) C(31) 1.49(2) ? ? yes C(30) C(37) 1.50(3) ? ? yes C(31) C(32) 1.42(3) ? ? yes C(31) C(36) 1.35(3) ? ? yes C(32) C(33) 1.35(3) ? ? yes C(33) C(34) 1.34(3) ? ? yes C(34) C(35) 1.34(3) ? ? yes C(35) C(36) 1.40(3) ? ? yes C(37) C(38) 1.36(3) ? ? yes C(37) C(42) 1.46(2) ? ? yes C(38) C(39) 1.36(3) ? ? yes C(39) C(40) 1.39(3) ? ? yes C(40) C(41) 1.39(3) ? ? yes C(41) C(42) 1.40(2) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Os(2) Os(1) Os(4) 56.47(3) ? ? ? yes Os(2) Os(1) N(1) 84.7(4) ? ? ? yes Os(2) Os(1) C(1) 110.4(6) ? ? ? yes Os(2) Os(1) C(2) 156.1(7) ? ? ? yes Os(2) Os(1) C(3) 87.0(7) ? ? ? yes Os(4) Os(1) N(1) 85.9(4) ? ? ? yes Os(4) Os(1) C(1) 166.4(6) ? ? ? yes Os(4) Os(1) C(2) 100.3(7) ? ? ? yes Os(4) Os(1) C(3) 90.8(7) ? ? ? yes N(1) Os(1) C(1) 89.5(7) ? ? ? yes N(1) Os(1) C(2) 100.0(7) ? ? ? yes N(1) Os(1) C(3) 171.5(8) ? ? ? yes C(1) Os(1) C(2) 93.1(9) ? ? ? yes C(1) Os(1) C(3) 92.0(10) ? ? ? yes C(2) Os(1) C(3) 88.3(9) ? ? ? yes Os(1) Os(2) Os(3) 117.62(4) ? ? ? yes Os(1) Os(2) Os(4) 60.85(3) ? ? ? yes Os(1) Os(2) Os(5) 74.60(3) ? ? ? yes Os(1) Os(2) O(17) 81.2(3) ? ? ? yes Os(1) Os(2) C(4) 161.8(7) ? ? ? yes Os(1) Os(2) C(5) 92.0(7) ? ? ? yes Os(1) Os(2) C(6) 71.5(4) ? ? ? yes Os(3) Os(2) Os(4) 62.76(3) ? ? ? yes Os(3) Os(2) Os(5) 127.07(4) ? ? ? yes Os(3) Os(2) O(17) 83.1(3) ? ? ? yes Os(3) Os(2) C(4) 80.6(7) ? ? ? yes Os(3) Os(2) C(5) 87.7(7) ? ? ? yes Os(3) Os(2) C(6) 167.8(4) ? ? ? yes Os(4) Os(2) Os(5) 87.80(3) ? ? ? yes Os(4) Os(2) O(17) 50.6(3) ? ? ? yes Os(4) Os(2) C(4) 135.6(7) ? ? ? yes Os(4) Os(2) C(5) 113.9(7) ? ? ? yes Os(4) Os(2) C(6) 128.9(4) ? ? ? yes Os(5) Os(2) O(17) 46.1(3) ? ? ? yes Os(5) Os(2) C(4) 96.0(6) ? ? ? yes Os(5) Os(2) C(5) 145.2(7) ? ? ? yes Os(5) Os(2) C(6) 61.6(4) ? ? ? yes O(17) Os(2) C(4) 103.8(7) ? ? ? yes O(17) Os(2) C(5) 164.4(8) ? ? ? yes O(17) Os(2) C(6) 107.0(5) ? ? ? yes C(4) Os(2) C(5) 87.0(9) ? ? ? yes C(4) Os(2) C(6) 90.3(8) ? ? ? yes C(5) Os(2) C(6) 83.8(8) ? ? ? yes Os(2) Os(3) Os(4) 56.71(3) ? ? ? yes Os(2) Os(3) N(2) 85.9(4) ? ? ? yes Os(2) Os(3) C(7) 99.6(8) ? ? ? yes Os(2) Os(3) C(8) 167.3(7) ? ? ? yes Os(2) Os(3) C(9) 90.8(7) ? ? ? yes Os(4) Os(3) N(2) 85.2(4) ? ? ? yes Os(4) Os(3) C(7) 155.7(8) ? ? ? yes Os(4) Os(3) C(8) 110.6(7) ? ? ? yes Os(4) Os(3) C(9) 87.6(7) ? ? ? yes N(2) Os(3) C(7) 99.6(8) ? ? ? yes N(2) Os(3) C(8) 92.7(8) ? ? ? yes N(2) Os(3) C(9) 172.7(8) ? ? ? yes C(7) Os(3) C(8) 93(1) ? ? ? yes C(7) Os(3) C(9) 87(1) ? ? ? yes C(8) Os(3) C(9) 89.1(10) ? ? ? yes Os(1) Os(4) Os(2) 62.68(3) ? ? ? yes Os(1) Os(4) Os(3) 117.26(4) ? ? ? yes Os(1) Os(4) Os(6) 126.72(3) ? ? ? yes Os(1) Os(4) O(17) 82.0(3) ? ? ? yes Os(1) Os(4) C(10) 79.1(6) ? ? ? yes Os(1) Os(4) C(11) 87.0(9) ? ? ? yes Os(1) Os(4) C(12) 166.0(8) ? ? ? yes Os(2) Os(4) Os(3) 60.53(3) ? ? ? yes Os(2) Os(4) Os(6) 87.57(3) ? ? ? yes Os(2) Os(4) O(17) 49.8(3) ? ? ? yes Os(2) Os(4) C(10) 130.8(6) ? ? ? yes Os(2) Os(4) C(11) 113.2(9) ? ? ? yes Os(2) Os(4) C(12) 126.8(8) ? ? ? yes Os(3) Os(4) Os(6) 74.71(3) ? ? ? yes Os(3) Os(4) O(17) 81.2(3) ? ? ? yes Os(3) Os(4) C(10) 163.0(6) ? ? ? yes Os(3) Os(4) C(11) 92.1(9) ? ? ? yes Os(3) Os(4) C(12) 67.9(8) ? ? ? yes Os(6) Os(4) O(17) 46.9(3) ? ? ? yes Os(6) Os(4) C(10) 92.0(6) ? ? ? yes Os(6) Os(4) C(11) 146.3(9) ? ? ? yes Os(6) Os(4) C(12) 66.6(8) ? ? ? yes O(17) Os(4) C(10) 97.6(6) ? ? ? yes O(17) Os(4) C(11) 162.7(10) ? ? ? yes O(17) Os(4) C(12) 111.9(8) ? ? ? yes C(10) Os(4) C(11) 93(1) ? ? ? yes C(10) Os(4) C(12) 97(1) ? ? ? yes C(11) Os(4) C(12) 79(1) ? ? ? yes Os(2) Os(5) O(17) 47.3(3) ? ? ? yes Os(2) Os(5) N(1) 85.9(4) ? ? ? yes Os(2) Os(5) C(13) 92.9(6) ? ? ? yes Os(2) Os(5) C(14) 123.4(7) ? ? ? yes Os(2) Os(5) C(29) 151.0(5) ? ? ? yes O(17) Os(5) N(1) 83.5(5) ? ? ? yes O(17) Os(5) C(13) 90.7(7) ? ? ? yes O(17) Os(5) C(14) 170.7(8) ? ? ? yes O(17) Os(5) C(29) 105.7(6) ? ? ? yes N(1) Os(5) C(13) 173.1(8) ? ? ? yes N(1) Os(5) C(14) 97.0(8) ? ? ? yes N(1) Os(5) C(29) 79.7(6) ? ? ? yes C(13) Os(5) C(14) 89.3(9) ? ? ? yes C(13) Os(5) C(29) 98.4(8) ? ? ? yes C(14) Os(5) C(29) 83.5(8) ? ? ? yes Os(4) Os(6) O(17) 46.8(3) ? ? ? yes Os(4) Os(6) N(2) 84.8(4) ? ? ? yes Os(4) Os(6) C(15) 97.6(6) ? ? ? yes Os(4) Os(6) C(16) 120.1(6) ? ? ? yes Os(4) Os(6) C(42) 153.4(5) ? ? ? yes O(17) Os(6) N(2) 82.4(5) ? ? ? yes O(17) Os(6) C(15) 93.7(7) ? ? ? yes O(17) Os(6) C(16) 166.7(7) ? ? ? yes O(17) Os(6) C(42) 108.7(6) ? ? ? yes N(2) Os(6) C(15) 172.1(7) ? ? ? yes N(2) Os(6) C(16) 99.7(7) ? ? ? yes N(2) Os(6) C(42) 80.7(7) ? ? ? yes C(15) Os(6) C(16) 85.7(8) ? ? ? yes C(15) Os(6) C(42) 94.1(8) ? ? ? yes C(16) Os(6) C(42) 84.5(8) ? ? ? yes Os(2) O(17) Os(4) 79.7(4) ? ? ? yes Os(2) O(17) Os(5) 86.6(5) ? ? ? yes Os(2) O(17) Os(6) 133.8(5) ? ? ? yes Os(4) O(17) Os(5) 134.4(6) ? ? ? yes Os(4) O(17) Os(6) 86.3(4) ? ? ? yes Os(5) O(17) Os(6) 131.2(6) ? ? ? yes Os(1) N(1) Os(5) 113.3(6) ? ? ? yes Os(1) N(1) C(17) 132(1) ? ? ? yes Os(5) N(1) C(17) 114(1) ? ? ? yes Os(3) N(2) Os(6) 113.8(7) ? ? ? yes Os(3) N(2) C(30) 131(1) ? ? ? yes Os(6) N(2) C(30) 114(1) ? ? ? yes Os(1) C(1) O(1) 178(1) ? ? ? yes Os(1) C(2) O(2) 174(1) ? ? ? yes Os(1) C(3) O(3) 177(2) ? ? ? yes Os(2) C(4) O(4) 174(1) ? ? ? yes Os(2) C(5) O(5) 175(2) ? ? ? yes Os(2) C(6) O(6) 164(1) ? ? ? yes Os(3) C(7) O(7) 173(2) ? ? ? yes Os(3) C(8) O(8) 175(2) ? ? ? yes Os(3) C(9) O(9) 177(2) ? ? ? yes Os(4) C(10) O(10) 173(1) ? ? ? yes Os(4) C(11) O(11) 174(2) ? ? ? yes Os(4) C(12) O(12) 161(2) ? ? ? yes Os(5) C(13) O(13) 178(1) ? ? ? yes Os(5) C(14) O(14) 178(1) ? ? ? yes Os(6) C(15) O(15) 175(1) ? ? ? yes Os(6) C(16) O(16) 179(1) ? ? ? yes N(1) C(17) C(18) 122(1) ? ? ? yes N(1) C(17) C(24) 118(1) ? ? ? yes C(18) C(17) C(24) 118(1) ? ? ? yes C(17) C(18) C(19) 118(1) ? ? ? yes C(17) C(18) C(23) 123(1) ? ? ? yes C(19) C(18) C(23) 117(1) ? ? ? yes C(18) C(19) C(20) 122(2) ? ? ? yes C(19) C(20) C(21) 118(2) ? ? ? yes C(20) C(21) C(22) 119(2) ? ? ? yes C(21) C(22) C(23) 121(2) ? ? ? yes C(18) C(23) C(22) 119(1) ? ? ? yes C(17) C(24) C(25) 127(1) ? ? ? yes C(17) C(24) C(29) 111(1) ? ? ? yes C(25) C(24) C(29) 121(1) ? ? ? yes C(24) C(25) C(26) 119(1) ? ? ? yes C(25) C(26) C(27) 120(1) ? ? ? yes C(26) C(27) C(28) 120(1) ? ? ? yes C(27) C(28) C(29) 120(1) ? ? ? yes Os(5) C(29) C(24) 114(1) ? ? ? yes Os(5) C(29) C(28) 128(1) ? ? ? yes C(24) C(29) C(28) 116(1) ? ? ? yes N(2) C(30) C(31) 125(1) ? ? ? yes N(2) C(30) C(37) 117(1) ? ? ? yes C(31) C(30) C(37) 116(1) ? ? ? yes C(30) C(31) C(32) 119(1) ? ? ? yes C(30) C(31) C(36) 122(1) ? ? ? yes C(32) C(31) C(36) 117(1) ? ? ? yes C(31) C(32) C(33) 121(2) ? ? ? yes C(32) C(33) C(34) 118(2) ? ? ? yes C(33) C(34) C(35) 122(2) ? ? ? yes C(34) C(35) C(36) 120(2) ? ? ? yes C(31) C(36) C(35) 119(1) ? ? ? yes C(30) C(37) C(38) 127(1) ? ? ? yes C(30) C(37) C(42) 112(1) ? ? ? yes C(38) C(37) C(42) 119(1) ? ? ? yes C(37) C(38) C(39) 123(1) ? ? ? yes C(38) C(39) C(40) 119(1) ? ? ? yes C(39) C(40) C(41) 118(2) ? ? ? yes C(40) C(41) C(42) 124(1) ? ? ? yes Os(6) C(42) C(37) 113(1) ? ? ? yes Os(6) C(42) C(41) 131(1) ? ? ? yes C(37) C(42) C(41) 114(1) ? ? ? yes #------------------------------------------------------------------------------ #=========================end of file============================= data_wt0336w-JW014-compound 9 _database_code_CSD 174859 #------------------------------------------------------------------------------ _audit_creation_date 'Thu Sep 23 16:25:51 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 9.505(2) _cell_length_b 11.528(3) _cell_length_c 16.272(2) _cell_angle_alpha 85.65(3) _cell_angle_beta 83.24(1) _cell_angle_gamma 67.06(2) _cell_volume 1629.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 298.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'block' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 3.159 _exptl_crystal_density_meas ? _chemical_formula_weight 1550.38 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H9 N O15 Os5 ' _chemical_formula_moiety 'C28 H9 N O15 Os5 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1368.00 _exptl_absorpt_coefficient_mu 19.481 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 298.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 10031 _reflns_number_total 6972 _reflns_number_observed 5943 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 3.77 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.47 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Os 0 10 -1.216 7.603 'International Tables' C 0 56 0.003 0.002 'International Tables' N 0 2 0.006 0.003 'International Tables' O 0 30 0.011 0.006 'International Tables' H 0 18 0.000 0.000 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Os(1) 0.86540(7) 0.08380(6) 0.82490(5) 0.0311(2) Uij ? ? Os(2) 0.66237(7) 0.32887(6) 0.84723(4) 0.0279(2) Uij ? ? Os(3) 0.97517(7) 0.27241(6) 0.83507(4) 0.0280(2) Uij ? ? Os(4) 0.83441(7) 0.27172(6) 0.69026(4) 0.0278(2) Uij ? ? Os(5) 0.76925(7) 0.52858(6) 0.81096(4) 0.0288(2) Uij ? ? O(1) 1.153(2) -0.156(1) 0.792(1) 0.067(5) Uij ? ? O(2) 0.665(2) -0.056(2) 0.792(1) 0.077(6) Uij ? ? O(3) 0.823(2) 0.036(1) 1.007(1) 0.069(5) Uij ? ? O(4) 0.441(2) 0.193(1) 0.882(1) 0.072(6) Uij ? ? O(5) 0.623(2) 0.371(1) 1.0309(9) 0.061(5) Uij ? ? O(6) 0.384(1) 0.554(1) 0.7940(10) 0.049(4) Uij ? ? O(7) 1.281(1) 0.047(1) 0.807(1) 0.060(5) Uij ? ? O(8) 0.992(2) 0.260(2) 1.0216(9) 0.065(5) Uij ? ? O(9) 1.182(2) 0.420(1) 0.800(1) 0.066(5) Uij ? ? O(10) 0.506(2) 0.294(2) 0.6724(9) 0.057(5) Uij ? ? O(11) 0.963(2) 0.005(1) 0.6252(10) 0.064(5) Uij ? ? O(12) 1.161(2) 0.261(2) 0.6404(9) 0.063(5) Uij ? ? O(13) 0.789(2) 0.564(2) 0.9944(9) 0.075(6) Uij ? ? O(14) 0.484(2) 0.770(1) 0.822(1) 0.066(5) Uij ? ? O(15) 0.961(2) 0.685(1) 0.758(1) 0.058(5) Uij ? ? N(1) 0.771(1) 0.470(1) 0.6904(8) 0.025(3) Uij ? ? C(1) 1.045(2) -0.067(2) 0.807(1) 0.041(5) Uij ? ? C(2) 0.741(2) -0.003(2) 0.803(1) 0.040(5) Uij ? ? C(3) 0.839(2) 0.055(2) 0.938(1) 0.045(6) Uij ? ? C(4) 0.531(2) 0.239(2) 0.864(1) 0.048(6) Uij ? ? C(5) 0.636(2) 0.356(2) 0.9622(10) 0.035(5) Uij ? ? C(6) 0.494(2) 0.476(2) 0.816(1) 0.036(5) Uij ? ? C(7) 1.162(2) 0.126(2) 0.817(1) 0.040(5) Uij ? ? C(8) 0.989(2) 0.263(2) 0.951(1) 0.035(4) Uij ? ? C(9) 1.093(2) 0.375(2) 0.811(1) 0.036(5) Uij ? ? C(10) 0.617(2) 0.291(2) 0.688(1) 0.038(5) Uij ? ? C(11) 0.912(2) 0.099(2) 0.660(1) 0.043(5) Uij ? ? C(12) 1.048(2) 0.264(2) 0.669(1) 0.043(5) Uij ? ? C(13) 0.779(2) 0.550(2) 0.928(1) 0.037(4) Uij ? ? C(14) 0.588(2) 0.681(2) 0.811(1) 0.038(5) Uij ? ? C(15) 0.887(2) 0.627(2) 0.774(1) 0.038(5) Uij ? ? C(16) 0.742(2) 0.530(2) 0.620(1) 0.037(5) Uij ? ? C(17) 0.764(2) 0.455(2) 0.547(1) 0.040(5) Uij ? ? C(18) 0.812(2) 0.323(2) 0.563(1) 0.031(4) Uij ? ? C(19) 0.837(2) 0.246(2) 0.495(1) 0.044(6) Uij ? ? C(20) 0.808(2) 0.302(2) 0.416(1) 0.050(6) Uij ? ? C(21) 0.763(3) 0.429(2) 0.402(1) 0.054(7) Uij ? ? C(22) 0.738(2) 0.507(2) 0.469(1) 0.047(6) Uij ? ? C(23) 0.690(2) 0.669(2) 0.612(1) 0.044(6) Uij ? ? C(24) 0.789(3) 0.727(2) 0.581(2) 0.058(7) Uij ? ? C(25) 0.737(3) 0.855(2) 0.570(2) 0.069(9) Uij ? ? C(26) 0.585(4) 0.928(2) 0.588(2) 0.09(1) Uij ? ? C(27) 0.488(3) 0.873(2) 0.615(2) 0.087(10) Uij ? ? C(28) 0.535(3) 0.743(2) 0.627(2) 0.061(7) Uij ? ? H(1) 0.8733 0.1573 0.5028 0.0531 Uij ? ? H(2) 0.8204 0.2500 0.3708 0.0597 Uij ? ? H(3) 0.7491 0.4646 0.3471 0.0648 Uij ? ? H(4) 0.7018 0.5963 0.4600 0.0559 Uij ? ? H(5) 0.8947 0.6768 0.5667 0.0697 Uij ? ? H(6) 0.8065 0.8940 0.5504 0.0828 Uij ? ? H(7) 0.5499 1.0173 0.5819 0.1036 Uij ? ? H(8) 0.3826 0.9241 0.6263 0.1046 Uij ? ? H(9) 0.4631 0.7058 0.6458 0.0730 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Os(1) 0.0319(3) 0.0206(3) 0.0409(4) -0.0090(3) -0.0089(3) 0.0017(3) Os(2) 0.0250(3) 0.0237(3) 0.0339(4) -0.0082(2) -0.0027(3) -0.0016(3) Os(3) 0.0253(3) 0.0237(3) 0.0353(4) -0.0083(2) -0.0086(3) 0.0000(3) Os(4) 0.0304(3) 0.0232(3) 0.0293(4) -0.0087(3) -0.0065(3) -0.0011(3) Os(5) 0.0314(3) 0.0208(3) 0.0341(4) -0.0089(3) -0.0052(3) -0.0025(3) O(1) 0.039(8) 0.051(9) 0.10(1) -0.003(7) -0.016(8) 0.000(9) O(2) 0.07(1) 0.06(1) 0.12(2) -0.038(9) -0.01(1) -0.02(1) O(3) 0.08(1) 0.06(1) 0.05(1) -0.014(9) -0.017(9) 0.018(9) O(4) 0.042(8) 0.045(8) 0.13(2) -0.025(7) -0.008(9) 0.010(10) O(5) 0.064(10) 0.07(1) 0.043(9) -0.016(8) 0.005(7) -0.020(8) O(6) 0.034(7) 0.038(7) 0.07(1) -0.010(6) -0.019(7) -0.004(7) O(7) 0.024(7) 0.044(8) 0.11(1) -0.005(6) -0.005(7) -0.017(8) O(8) 0.09(1) 0.07(1) 0.036(9) -0.025(9) -0.007(8) -0.009(8) O(9) 0.039(8) 0.048(9) 0.11(1) -0.022(7) -0.010(9) 0.014(9) O(10) 0.039(8) 0.09(1) 0.038(8) -0.025(8) -0.008(6) -0.004(8) O(11) 0.10(1) 0.034(8) 0.06(1) -0.015(8) -0.006(9) -0.010(7) O(12) 0.054(9) 0.10(1) 0.043(9) -0.044(9) 0.010(7) -0.016(9) O(13) 0.13(2) 0.07(1) 0.034(9) -0.05(1) -0.019(9) -0.010(8) O(14) 0.037(8) 0.031(7) 0.12(2) -0.001(6) -0.004(9) -0.005(8) O(15) 0.052(9) 0.053(9) 0.08(1) -0.027(7) 0.004(8) -0.004(8) N(1) 0.024(6) 0.024(6) 0.029(7) -0.008(5) -0.005(5) -0.005(6) C(1) 0.026(9) 0.028(9) 0.07(1) -0.005(7) -0.027(9) 0.008(9) C(2) 0.036(9) 0.031(9) 0.05(1) -0.011(8) -0.005(9) -0.002(8) C(3) 0.06(1) 0.034(10) 0.04(1) -0.021(9) 0.001(10) 0.001(8) C(4) 0.04(1) 0.034(10) 0.08(2) -0.014(8) -0.007(10) -0.004(10) C(5) 0.05(1) 0.041(9) 0.010(8) -0.011(8) 0.006(7) -0.002(7) C(6) 0.031(9) 0.039(10) 0.04(1) -0.015(8) -0.008(8) -0.009(8) C(7) 0.029(9) 0.029(9) 0.06(1) -0.006(7) -0.013(9) 0.008(8) C(9) 0.030(9) 0.030(9) 0.05(1) -0.011(7) -0.009(8) 0.002(8) C(10) 0.05(1) 0.041(10) 0.026(9) -0.014(8) -0.016(8) 0.008(8) C(11) 0.05(1) 0.04(1) 0.03(1) -0.018(9) 0.008(9) -0.005(8) C(12) 0.035(10) 0.05(1) 0.04(1) -0.016(9) -0.002(9) 0.005(9) C(14) 0.038(10) 0.036(10) 0.04(1) -0.015(8) -0.003(8) -0.009(8) C(15) 0.038(9) 0.024(8) 0.05(1) -0.012(7) 0.002(8) -0.001(8) C(16) 0.039(10) 0.035(9) 0.04(1) -0.018(8) 0.000(8) 0.002(8) C(17) 0.05(1) 0.04(1) 0.031(10) -0.024(9) 0.005(8) 0.002(8) C(18) 0.016(7) 0.042(9) 0.031(9) -0.003(7) -0.011(6) -0.002(8) C(19) 0.06(1) 0.04(1) 0.03(1) -0.022(10) -0.003(9) -0.006(8) C(20) 0.05(1) 0.06(1) 0.04(1) -0.01(1) -0.005(9) -0.011(10) C(21) 0.06(1) 0.07(1) 0.04(1) -0.02(1) -0.007(10) 0.00(1) C(22) 0.05(1) 0.05(1) 0.04(1) -0.018(9) -0.013(9) 0.002(9) C(23) 0.04(1) 0.04(1) 0.05(1) -0.014(9) -0.014(9) 0.000(9) C(24) 0.06(1) 0.04(1) 0.09(2) -0.023(10) -0.03(1) 0.02(1) C(25) 0.11(2) 0.05(1) 0.06(2) -0.05(2) -0.03(2) 0.02(1) C(26) 0.13(3) 0.03(1) 0.09(2) -0.02(1) -0.01(2) 0.00(1) C(27) 0.06(2) 0.04(1) 0.13(3) 0.01(1) -0.02(2) 0.01(2) C(28) 0.05(1) 0.04(1) 0.08(2) -0.02(1) -0.01(1) 0.01(1) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5943 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0572 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0703 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.984 _refine_ls_shift/esd_max 0.0030 _refine_ls_shift/esd_mean ? _refine_diff_density_min -3.01 _refine_diff_density_max 6.56 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os(1) Os(2) 2.7528(9) ? ? yes Os(1) Os(3) 2.7762(9) ? ? yes Os(1) Os(4) 2.9180(9) ? ? yes Os(1) C(1) 1.91(2) ? ? yes Os(1) C(2) 1.90(2) ? ? yes Os(1) C(3) 1.85(2) ? ? yes Os(2) Os(3) 2.7703(9) ? ? yes Os(2) Os(4) 2.8398(9) ? ? yes Os(2) Os(5) 2.8560(9) ? ? yes Os(2) C(4) 1.90(2) ? ? yes Os(2) C(5) 1.89(2) ? ? yes Os(2) C(6) 1.91(2) ? ? yes Os(3) Os(4) 2.8453(9) ? ? yes Os(3) Os(5) 2.8645(9) ? ? yes Os(3) C(7) 1.92(2) ? ? yes Os(3) C(8) 1.89(2) ? ? yes Os(3) C(9) 1.91(2) ? ? yes Os(4) N(1) 2.13(1) ? ? yes Os(4) C(10) 2.00(2) ? ? yes Os(4) C(11) 1.91(2) ? ? yes Os(4) C(12) 1.99(2) ? ? yes Os(4) C(18) 2.11(2) ? ? yes Os(5) N(1) 2.12(1) ? ? yes Os(5) C(13) 1.96(2) ? ? yes Os(5) C(14) 1.92(2) ? ? yes Os(5) C(15) 1.90(2) ? ? yes O(1) C(1) 1.15(2) ? ? yes O(2) C(2) 1.14(2) ? ? yes O(3) C(3) 1.14(2) ? ? yes O(4) C(4) 1.17(2) ? ? yes O(5) C(5) 1.13(2) ? ? yes O(6) C(6) 1.15(2) ? ? yes O(7) C(7) 1.15(2) ? ? yes O(8) C(8) 1.16(2) ? ? yes O(9) C(9) 1.14(2) ? ? yes O(10) C(10) 1.10(2) ? ? yes O(11) C(11) 1.17(2) ? ? yes O(12) C(12) 1.11(2) ? ? yes O(13) C(13) 1.12(2) ? ? yes O(14) C(14) 1.12(2) ? ? yes O(15) C(15) 1.14(2) ? ? yes N(1) C(16) 1.30(2) ? ? yes C(16) C(17) 1.47(3) ? ? yes C(16) C(23) 1.48(2) ? ? yes C(17) C(18) 1.42(2) ? ? yes C(17) C(22) 1.37(3) ? ? yes C(18) C(19) 1.41(2) ? ? yes C(19) C(20) 1.40(3) ? ? yes C(20) C(21) 1.37(3) ? ? yes C(21) C(22) 1.40(3) ? ? yes C(23) C(24) 1.38(3) ? ? yes C(23) C(28) 1.39(3) ? ? yes C(24) C(25) 1.37(3) ? ? yes C(25) C(26) 1.36(4) ? ? yes C(26) C(27) 1.33(4) ? ? yes C(27) C(28) 1.39(3) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Os(2) Os(1) Os(3) 60.14(2) ? ? ? yes Os(2) Os(1) Os(4) 60.02(2) ? ? ? yes Os(2) Os(1) C(1) 165.0(5) ? ? ? yes Os(2) Os(1) C(2) 104.3(5) ? ? ? yes Os(2) Os(1) C(3) 88.4(6) ? ? ? yes Os(3) Os(1) Os(4) 59.90(2) ? ? ? yes Os(3) Os(1) C(1) 104.9(5) ? ? ? yes Os(3) Os(1) C(2) 162.2(5) ? ? ? yes Os(3) Os(1) C(3) 95.7(6) ? ? ? yes Os(4) Os(1) C(1) 112.8(6) ? ? ? yes Os(4) Os(1) C(2) 105.8(6) ? ? ? yes Os(4) Os(1) C(3) 146.3(6) ? ? ? yes C(1) Os(1) C(2) 90.2(7) ? ? ? yes C(1) Os(1) C(3) 94.9(9) ? ? ? yes C(2) Os(1) C(3) 92.4(9) ? ? ? yes Os(1) Os(2) Os(3) 60.35(2) ? ? ? yes Os(1) Os(2) Os(4) 62.88(2) ? ? ? yes Os(1) Os(2) Os(5) 119.16(3) ? ? ? yes Os(1) Os(2) C(4) 77.8(6) ? ? ? yes Os(1) Os(2) C(5) 106.7(5) ? ? ? yes Os(1) Os(2) C(6) 152.1(5) ? ? ? yes Os(3) Os(2) Os(4) 60.94(2) ? ? ? yes Os(3) Os(2) Os(5) 61.19(2) ? ? ? yes Os(3) Os(2) C(4) 137.1(6) ? ? ? yes Os(3) Os(2) C(5) 93.5(6) ? ? ? yes Os(3) Os(2) C(6) 131.9(5) ? ? ? yes Os(4) Os(2) Os(5) 75.56(2) ? ? ? yes Os(4) Os(2) C(4) 109.4(7) ? ? ? yes Os(4) Os(2) C(5) 154.4(6) ? ? ? yes Os(4) Os(2) C(6) 99.1(6) ? ? ? yes Os(5) Os(2) C(4) 161.5(6) ? ? ? yes Os(5) Os(2) C(5) 92.0(6) ? ? ? yes Os(5) Os(2) C(6) 71.8(5) ? ? ? yes C(4) Os(2) C(5) 89.6(9) ? ? ? yes C(4) Os(2) C(6) 89.7(8) ? ? ? yes C(5) Os(2) C(6) 97.9(8) ? ? ? yes Os(1) Os(3) Os(2) 59.51(2) ? ? ? yes Os(1) Os(3) Os(4) 62.53(2) ? ? ? yes Os(1) Os(3) Os(5) 118.07(3) ? ? ? yes Os(1) Os(3) C(7) 77.8(5) ? ? ? yes Os(1) Os(3) C(8) 98.8(5) ? ? ? yes Os(1) Os(3) C(9) 161.1(6) ? ? ? yes Os(2) Os(3) Os(4) 60.74(2) ? ? ? yes Os(2) Os(3) Os(5) 60.88(2) ? ? ? yes Os(2) Os(3) C(7) 137.2(5) ? ? ? yes Os(2) Os(3) C(8) 95.4(5) ? ? ? yes Os(2) Os(3) C(9) 132.1(5) ? ? ? yes Os(4) Os(3) Os(5) 75.34(2) ? ? ? yes Os(4) Os(3) C(7) 99.8(6) ? ? ? yes Os(4) Os(3) C(8) 154.5(5) ? ? ? yes Os(4) Os(3) C(9) 107.6(6) ? ? ? yes Os(5) Os(3) C(7) 156.3(5) ? ? ? yes Os(5) Os(3) C(8) 101.8(5) ? ? ? yes Os(5) Os(3) C(9) 71.2(5) ? ? ? yes C(7) Os(3) C(8) 92.3(8) ? ? ? yes C(7) Os(3) C(9) 88.8(7) ? ? ? yes C(8) Os(3) C(9) 94.9(8) ? ? ? yes Os(1) Os(4) Os(2) 57.10(2) ? ? ? yes Os(1) Os(4) Os(3) 57.58(2) ? ? ? yes Os(1) Os(4) N(1) 131.8(4) ? ? ? yes Os(1) Os(4) C(10) 89.0(5) ? ? ? yes Os(1) Os(4) C(11) 63.0(6) ? ? ? yes Os(1) Os(4) C(12) 101.5(6) ? ? ? yes Os(1) Os(4) C(18) 149.3(5) ? ? ? yes Os(2) Os(4) Os(3) 58.33(2) ? ? ? yes Os(2) Os(4) N(1) 79.1(4) ? ? ? yes Os(2) Os(4) C(10) 67.3(5) ? ? ? yes Os(2) Os(4) C(11) 116.1(6) ? ? ? yes Os(2) Os(4) C(12) 122.7(6) ? ? ? yes Os(2) Os(4) C(18) 140.3(4) ? ? ? yes Os(3) Os(4) N(1) 83.8(4) ? ? ? yes Os(3) Os(4) C(10) 125.3(5) ? ? ? yes Os(3) Os(4) C(11) 105.4(6) ? ? ? yes Os(3) Os(4) C(12) 65.5(6) ? ? ? yes Os(3) Os(4) C(18) 148.2(4) ? ? ? yes N(1) Os(4) C(10) 91.8(6) ? ? ? yes N(1) Os(4) C(11) 164.7(7) ? ? ? yes N(1) Os(4) C(12) 84.9(6) ? ? ? yes N(1) Os(4) C(18) 78.0(6) ? ? ? yes C(10) Os(4) C(11) 92.6(8) ? ? ? yes C(10) Os(4) C(12) 168.4(8) ? ? ? yes C(10) Os(4) C(18) 81.5(6) ? ? ? yes C(11) Os(4) C(12) 87.9(8) ? ? ? yes C(11) Os(4) C(18) 88.2(7) ? ? ? yes C(12) Os(4) C(18) 86.9(7) ? ? ? yes Os(2) Os(5) Os(3) 57.93(2) ? ? ? yes Os(2) Os(5) N(1) 78.8(3) ? ? ? yes Os(2) Os(5) C(13) 92.6(5) ? ? ? yes Os(2) Os(5) C(14) 105.7(5) ? ? ? yes Os(2) Os(5) C(15) 165.0(5) ? ? ? yes Os(3) Os(5) N(1) 83.5(3) ? ? ? yes Os(3) Os(5) C(13) 86.8(5) ? ? ? yes Os(3) Os(5) C(14) 162.9(5) ? ? ? yes Os(3) Os(5) C(15) 108.6(5) ? ? ? yes N(1) Os(5) C(13) 169.5(6) ? ? ? yes N(1) Os(5) C(14) 98.8(6) ? ? ? yes N(1) Os(5) C(15) 93.7(7) ? ? ? yes C(13) Os(5) C(14) 89.2(8) ? ? ? yes C(13) Os(5) C(15) 93.3(8) ? ? ? yes C(14) Os(5) C(15) 88.2(7) ? ? ? yes Os(4) N(1) Os(5) 110.5(6) ? ? ? yes Os(4) N(1) C(16) 116(1) ? ? ? yes Os(5) N(1) C(16) 133(1) ? ? ? yes Os(1) C(1) O(1) 177(1) ? ? ? yes Os(1) C(2) O(2) 178(1) ? ? ? yes Os(1) C(3) O(3) 179(1) ? ? ? yes Os(2) C(4) O(4) 171(1) ? ? ? yes Os(2) C(5) O(5) 178(1) ? ? ? yes Os(2) C(6) O(6) 170(1) ? ? ? yes Os(3) C(7) O(7) 172(1) ? ? ? yes Os(3) C(8) O(8) 177(1) ? ? ? yes Os(3) C(9) O(9) 169(1) ? ? ? yes Os(4) C(10) O(10) 166(1) ? ? ? yes Os(4) C(11) O(11) 165(1) ? ? ? yes Os(4) C(12) O(12) 165(1) ? ? ? yes Os(5) C(13) O(13) 176(1) ? ? ? yes Os(5) C(14) O(14) 171(1) ? ? ? yes Os(5) C(15) O(15) 174(1) ? ? ? yes N(1) C(16) C(17) 117(1) ? ? ? yes N(1) C(16) C(23) 121(1) ? ? ? yes C(17) C(16) C(23) 121(1) ? ? ? yes C(16) C(17) C(18) 114(1) ? ? ? yes C(16) C(17) C(22) 122(1) ? ? ? yes C(18) C(17) C(22) 122(1) ? ? ? yes Os(4) C(18) C(17) 113(1) ? ? ? yes Os(4) C(18) C(19) 129(1) ? ? ? yes C(17) C(18) C(19) 116(1) ? ? ? yes C(18) C(19) C(20) 119(1) ? ? ? yes C(19) C(20) C(21) 121(1) ? ? ? yes C(20) C(21) C(22) 119(1) ? ? ? yes C(17) C(22) C(21) 119(1) ? ? ? yes C(16) C(23) C(24) 121(1) ? ? ? yes C(16) C(23) C(28) 119(1) ? ? ? yes C(24) C(23) C(28) 118(1) ? ? ? yes C(23) C(24) C(25) 120(2) ? ? ? yes C(24) C(25) C(26) 120(2) ? ? ? yes C(25) C(26) C(27) 119(2) ? ? ? yes C(26) C(27) C(28) 122(2) ? ? ? yes C(23) C(28) C(27) 118(2) ? ? ? yes #------------------------------------------------------------------------------ #=================================end of file================================