Syntheses, Raman Spectra, and X-ray Crystal Structures of [XeF5][μ-F(OsO3F2)2] and [M][OsO3F3] (M = XeF5+, Xe2F11+)
Michael J. Hughes; Hélène P. A. Mercier; Gary J. Schrobilgen; Inorganic Chemistry 49 (2010) 3501–3515; doi:10.1021/ic100062x

data_4315227
_publ_section_title
;
 Syntheses, Raman Spectra, and X-ray Crystal Structures of
 [XeF5][\m-F(OsO3F2)2] and [M][OsO3F3] (M = XeF5+, Xe2F11+)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3501
_journal_page_last               3515
_journal_paper_doi               10.1021/ic100062x
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'F8 O3 Os Xe'
_chemical_formula_weight         521.50
_chemical_name_common            'Xe F5 Os O3 F3'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.8876(3)
_cell_length_b                   16.8876(3)
_cell_length_c                   5.3414(2)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78
_cell_measurement_theta_min      0
_cell_volume                     1523.32(7)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            41027
_diffrn_reflns_theta_full        38.88
_diffrn_reflns_theta_max         38.88
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    21.243
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2.0-2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.230
_refine_diff_density_min         -2.010
_refine_diff_density_rms         0.333
_refine_ls_extinction_coef       0.00029(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   1.356
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         4345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.356
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                3623
_reflns_number_total             4345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100062x_si_002_2.cif
_cod_data_source_block           XeF5OsO3F3
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4315227