The OsO4F-, OsO4F22-, and OsO3F3- Anions, Their Study by Vibrational and NMR Spectroscopy and Density Functional Theory Calculations, and the X-ray Crystal Structures of [N(CH3)4][OsO4F] and [N(CH3)4][OsO3F3]
Michael Gerken; David A. Dixon; Gary J. Schrobilgen; Inorganic Chemistry 39 (2000) 4244–4255; doi:10.1021/ic000259i

data_4321352
_publ_section_title
;
 The OsO4F-, OsO4F22-, and OsO3F3- Anions, Their Study by Vibrational and
 NMR Spectroscopy and Density Functional Theory Calculations, and the
 X-ray Crystal Structures of [N(CH3)4][OsO4F] and [N(CH3)4][OsO3F3]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4244
_journal_page_last               4255
_journal_paper_doi               10.1021/ic000259i
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C4 H12 F N O4 Os'
_chemical_formula_weight         347.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           39
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2b'
_symmetry_space_group_name_H-M   'A e m 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0174(14)
_cell_length_b                   11.401(2)
_cell_length_c                   10.925(2)
_cell_measurement_temperature    223(2)
_cell_volume                     874.1(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3996
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    7.894
_exptl_crystal_density_diffrn    2.639
_exptl_crystal_F_000             640
_refine_diff_density_max         2.081
_refine_diff_density_min         -1.458
_refine_diff_density_rms         0.257
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.135
_refine_ls_goodness_of_fit_obs   1.156
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1214
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.134
_refine_ls_restrained_S_obs      1.155
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_obs          0.0282
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+4.9382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0754
_refine_ls_wR_factor_obs         0.0748
_reflns_number_observed          1154
_reflns_number_total             1214
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000259i_1.cif
_cod_data_source_block           '[N(CH3)4][OsO4F]_at_-50C'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+4.9382P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+4.9382P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2021-11-23
Space group name changed to comply with IUCR recomendations
                 miguel
;
_cod_original_sg_symbol_H-M   'A b m 2'
_cod_database_code               4321352