#------------------------------------------------------------------------------ #$Date: 2014-01-30 01:52:48 +0200 (Thu, 30 Jan 2014) $ #$Revision: 98538 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/33/27/4332767.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_4332767 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 ; _space_group_IT_number 7 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P -2yc' _symmetry_space_group_name_H-M 'P 1 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 99.896(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.4057(5) _cell_length_b 5.0131(5) _cell_length_c 12.1373(12) _cell_measurement_temperature 133(2) _cell_volume 324.02(5) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 20 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _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 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10247 _diffrn_reflns_theta_full 41.00 _diffrn_reflns_theta_max 41.00 _diffrn_reflns_theta_min 3.41 _exptl_absorpt_coefficient_mu 39.281 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.1879 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour green _exptl_crystal_density_diffrn 5.723 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needles _exptl_crystal_F_000 476 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _refine_diff_density_max 7.925 _refine_diff_density_min -7.076 _refine_diff_density_rms 0.565 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(4) _refine_ls_extinction_coef 0.0061(5) _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 1.072 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 111 _refine_ls_number_reflns 3322 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0368 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+3.2085P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.0868 _reflns_number_gt 2980 _reflns_number_total 3322 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic0608290sup2.cif _[local]_cod_data_source_block oso2f3 _[local]_cod_cif_authors_sg_H-M Pc _cod_database_code 4332767 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, 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 0.81777(5) 0.48143(6) 0.44372(3) 0.00930(8) Uani 1 1 d F1 F 0.9466(16) 0.2936(14) 0.5920(7) 0.0120(13) Uani 1 1 d F2 F 1.0340(16) 0.7985(14) 0.5026(7) 0.0121(13) Uani 1 1 d F11 F 1.1225(18) 0.3623(15) 0.4117(7) 0.0135(13) Uani 1 1 d F12 F 0.748(2) 0.6450(15) 0.3081(8) 0.0152(15) Uani 1 1 d F13 F 0.6604(15) 0.1726(15) 0.3911(9) 0.0146(14) Uani 1 1 d O11 O 0.583(2) 0.6118(18) 0.5050(10) 0.0129(15) Uani 1 1 d Os2 Os 1.17800(5) -0.03159(6) 0.66254(3) 0.01154(9) Uani 1 1 d F21 F 0.8621(18) -0.1372(15) 0.6799(8) 0.0177(15) Uani 1 1 d O21 O 1.320(2) -0.3297(14) 0.7023(9) 0.0141(15) Uani 1 1 d O22 O 1.243(2) 0.1387(17) 0.7863(9) 0.0155(17) Uani 1 1 d O23 O 1.3840(19) 0.1124(16) 0.5886(9) 0.0120(15) 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 0.01201(16) 0.00654(12) 0.00920(16) 0.00156(14) 0.00140(12) 0.00070(14) F1 0.015(4) 0.012(3) 0.008(3) 0.003(2) 0.000(2) 0.005(2) F2 0.015(4) 0.010(2) 0.011(3) -0.003(2) 0.001(3) -0.004(2) F11 0.013(3) 0.014(3) 0.014(3) -0.005(2) 0.002(2) 0.001(2) F12 0.021(4) 0.014(3) 0.008(3) 0.007(2) -0.003(3) 0.001(3) F13 0.014(3) 0.008(2) 0.021(3) -0.003(2) 0.000(3) -0.003(2) O11 0.005(3) 0.020(3) 0.014(3) -0.001(3) 0.000(3) 0.002(2) Os2 0.0178(2) 0.00605(12) 0.01059(18) -0.00133(15) 0.00204(15) 0.00006(15) F21 0.019(4) 0.018(3) 0.019(3) -0.004(2) 0.008(3) -0.003(2) O21 0.021(4) 0.007(2) 0.013(3) 0.000(3) -0.002(3) 0.003(3) O22 0.021(5) 0.013(3) 0.012(3) 0.001(3) 0.003(3) 0.004(3) O23 0.013(4) 0.007(3) 0.015(3) 0.005(2) 0.002(3) 0.001(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 O11 Os1 F12 99.6(5) . . O11 Os1 F13 98.1(4) . . F12 Os1 F13 93.1(4) . . O11 Os1 F11 165.4(5) . . F12 Os1 F11 90.6(4) . . F13 Os1 F11 91.8(3) . . O11 Os1 F2 88.4(4) . . F12 Os1 F2 89.1(4) . . F13 Os1 F2 172.7(4) . . F11 Os1 F2 81.2(3) . . O11 Os1 F1 87.7(5) . . F12 Os1 F1 172.0(4) . . F13 Os1 F1 89.1(4) . . F11 Os1 F1 81.7(3) . . F2 Os1 F1 87.8(4) . . Os1 F1 Os2 142.2(4) . . Os1 F2 Os2 136.8(4) . 1_565 O23 Os2 O21 102.5(5) . . O23 Os2 O22 101.3(5) . . O21 Os2 O22 100.0(5) . . O23 Os2 F21 152.6(5) . . O21 Os2 F21 95.5(4) . . O22 Os2 F21 95.6(5) . . O23 Os2 F2 82.0(4) . 1_545 O21 Os2 F2 89.0(4) . 1_545 O22 Os2 F2 169.4(4) . 1_545 F21 Os2 F2 77.8(3) . 1_545 O23 Os2 F1 81.8(4) . . O21 Os2 F1 168.6(5) . . O22 Os2 F1 89.4(4) . . F21 Os2 F1 77.0(4) . . F2 Os2 F1 81.0(4) 1_545 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Os1 O11 1.707(10) . Os1 F12 1.820(9) . Os1 F13 1.828(8) . Os1 F11 1.855(9) . Os1 F2 2.029(7) . Os1 F1 2.044(8) . F1 Os2 2.142(7) . F2 Os2 2.140(8) 1_565 Os2 O23 1.706(9) . Os2 O21 1.710(8) . Os2 O22 1.711(11) . Os2 F21 1.834(9) . Os2 F2 2.140(8) 1_545