Fluoride Ion Donor Properties of cis-OsO2F4: Synthesis, Raman Spectroscopic Study, and X-ray Crystal Structure of [OsO2F3][Sb2F11]
Michael J. Hughes; Hélène P. A. Mercier; Gary J. Schrobilgen; Inorganic Chemistry 49 (2010) 271–284; doi:10.1021/ic901999e

data_4314475
_publ_section_title
;
 Fluoride Ion Donor Properties of cis-OsO2F4: Synthesis, Raman
 Spectroscopic Study, and X-ray Crystal Structure of [OsO2F3][Sb2F11]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              271
_journal_page_last               284
_journal_paper_doi               10.1021/ic901999e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'F14 O2 Os Sb2'
_chemical_formula_weight         731.70
_chemical_name_common            'F3 O2 Os, Sb2 F11'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.597(2)
_cell_angle_beta                 111.263(2)
_cell_angle_gamma                110.697(2)
_cell_formula_units_Z            2
_cell_length_a                   7.4284(3)
_cell_length_b                   8.6649(4)
_cell_length_c                   10.0349(4)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69
_cell_measurement_theta_min      0
_cell_volume                     537.39(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker Saint'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12832
_diffrn_reflns_theta_full        34.50
_diffrn_reflns_theta_max         34.50
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    16.981
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.690
_refine_diff_density_min         -2.471
_refine_diff_density_rms         0.397
_refine_ls_extinction_coef       0.0135(4)
_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   1.242
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         4355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0157P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0694
_reflns_number_gt                3724
_reflns_number_total             4355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901999e_si_002.cif
_cod_data_source_block           mh08check
_cod_database_code               4314475