#------------------------------------------------------------------------------ #$Date: 2016-03-23 20:54:45 +0200 (Wed, 23 Mar 2016) $ #$Revision: 179430 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/33/27/4332768.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided the Crystal Eye server at # http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the # Peter Murray-Rust laboratory. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_4332768 loop_ _publ_author_name 'Shorafa, Hashem' 'Seppelt, Konrad' _publ_section_title ; Osmium(VII) Fluorine Compounds ; _journal_issue 19 _journal_name_full 'Inorganic Chemistry' _journal_page_first 7929 _journal_page_last 7934 _journal_paper_doi 10.1021/ic0608290 _journal_volume 45 _journal_year 2006 _chemical_formula_moiety OsO2F3 _chemical_formula_sum 'F6 O4 Os2' _chemical_formula_weight 558.40 _chemical_name_systematic ; Osmiumdioxidtrifluorid Tetramer ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 99.776(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 5.4181(10) _cell_length_b 9.9332(18) _cell_length_c 12.296(2) _cell_measurement_temperature 133(2) _cell_volume 652.1(2) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type Bruker-Smart-CCD-1000-TM _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 10551 _diffrn_reflns_theta_full 30.55 _diffrn_reflns_theta_max 30.55 _diffrn_reflns_theta_min 2.65 _exptl_absorpt_coefficient_mu 39.034 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.516976 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour green _exptl_crystal_density_diffrn 5.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cube _exptl_crystal_F_000 952 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 3.523 _refine_diff_density_min -2.990 _refine_diff_density_rms 0.390 _refine_ls_extinction_coef 0.00072(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 1989 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0289 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+6.6602P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.0631 _reflns_number_gt 1621 _reflns_number_total 1989 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic0608290sup3.cif _cod_data_source_block oso2f3t _cod_original_sg_symbol_H-M P2(1)/c _cod_database_code 4332768 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag Os1 Os 0.34034(5) 0.98966(3) 0.21874(2) 0.01098(9) Uani 1 1 d O1 O 0.5422(10) 1.0631(6) 0.1411(4) 0.0124(11) Uani 1 1 d O2 O 0.4001(10) 1.0768(5) 0.3389(5) 0.0138(11) Uani 1 1 d O3 O 0.4811(10) 0.8410(6) 0.2515(5) 0.0139(12) Uani 1 1 d F1 F 0.1949(8) 0.9079(5) 0.0561(4) 0.0126(9) Uani 1 1 d Os2 Os 0.01417(5) 1.25149(3) -0.00082(2) 0.01070(9) Uani 1 1 d O4 O 0.2704(9) 1.1708(5) -0.0451(4) 0.0092(10) Uani 1 1 d F2 F 0.0205(8) 0.9390(5) 0.2299(4) 0.0159(10) Uani 1 1 d F3 F 0.1066(8) 1.1573(4) 0.1429(4) 0.0129(9) Uani 1 1 d F4 F 0.1958(9) 1.3987(5) 0.0541(4) 0.0194(10) Uani 1 1 d F5 F -0.0905(9) 1.3354(5) -0.1348(4) 0.0156(10) Uani 1 1 d F6 F -0.2607(9) 1.3086(5) 0.0538(4) 0.0224(11) Uani 1 1 d loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.01351(15) 0.00878(16) 0.00972(14) -0.00073(12) -0.00067(10) 0.00081(11) O1 0.014(2) 0.014(3) 0.011(3) 0.002(2) 0.006(2) 0.001(2) O2 0.015(3) 0.012(3) 0.014(3) -0.003(2) 0.001(2) 0.003(2) O3 0.016(3) 0.009(3) 0.015(3) 0.005(2) -0.003(2) 0.004(2) F1 0.014(2) 0.016(2) 0.007(2) 0.0003(18) 0.0014(17) -0.0025(18) Os2 0.01338(15) 0.01039(16) 0.00739(14) -0.00030(11) -0.00094(10) -0.00152(11) O4 0.009(2) 0.009(3) 0.009(3) -0.003(2) -0.0012(19) 0.000(2) F2 0.014(2) 0.019(3) 0.014(2) 0.000(2) 0.0029(18) -0.0030(19) F3 0.016(2) 0.010(2) 0.013(2) 0.0024(18) 0.0018(18) 0.0049(17) F4 0.024(2) 0.014(2) 0.020(3) -0.002(2) 0.001(2) -0.004(2) F5 0.020(2) 0.015(2) 0.011(2) 0.0034(18) 0.0001(19) -0.0023(18) F6 0.019(2) 0.027(3) 0.021(3) -0.002(2) 0.004(2) 0.000(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O3 Os1 O2 103.2(3) . . O3 Os1 O1 101.5(3) . . O2 Os1 O1 102.7(3) . . O3 Os1 F2 97.9(2) . . O2 Os1 F2 96.8(2) . . O1 Os1 F2 148.4(2) . . O3 Os1 F1 88.3(2) . . O2 Os1 F1 167.5(2) . . O1 Os1 F1 79.3(2) . . F2 Os1 F1 76.54(18) . . O3 Os1 F3 166.4(2) . . O2 Os1 F3 89.6(2) . . O1 Os1 F3 79.6(2) . . F2 Os1 F3 75.88(19) . . F1 Os1 F3 78.52(17) . . Os2 F1 Os1 134.7(2) 3_575 . O4 Os2 F6 170.8(2) . . O4 Os2 F4 94.3(2) . . F6 Os2 F4 92.1(2) . . O4 Os2 F5 93.9(2) . . F6 Os2 F5 92.4(2) . . F4 Os2 F5 91.9(2) . . O4 Os2 F3 88.2(2) . . F6 Os2 F3 85.3(2) . . F4 Os2 F3 90.5(2) . . F5 Os2 F3 176.67(18) . . O4 Os2 F1 88.0(2) . 3_575 F6 Os2 F1 85.4(2) . 3_575 F4 Os2 F1 177.41(18) . 3_575 F5 Os2 F1 89.04(19) . 3_575 F3 Os2 F1 88.42(19) . 3_575 Os2 F3 Os1 140.6(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Os1 O3 1.680(5) . Os1 O2 1.695(6) . Os1 O1 1.730(5) . Os1 F2 1.832(4) . Os1 F1 2.178(5) . Os1 F3 2.201(4) . F1 Os2 1.998(4) 3_575 Os2 O4 1.767(5) . Os2 F6 1.825(5) . Os2 F4 1.827(5) . Os2 F5 1.847(5) . Os2 F3 1.988(5) . Os2 F1 1.998(4) 3_575