Osmium(VII) Fluorine Compounds
Shorafa, Hashem; Seppelt, Konrad; Inorganic Chemistry 45 (2006) 7929–7934; doi:10.1021/ic0608290

data_4332767
_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)
_cod_data_source_file            ic0608290sup2.cif
_cod_data_source_block           oso2f3
_cod_original_sg_symbol_H-M      Pc
_cod_database_code               4332767