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_4321353
_publ_section_title
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 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 F3 N O3 Os'
_chemical_formula_weight         369.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 134.128(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.347(4)
_cell_length_b                   13.475(3)
_cell_length_c                   11.435(3)
_cell_measurement_temperature    156(2)
_cell_volume                     1808.0(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      156(2)
_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  0.0948
_diffrn_reflns_av_sigmaI/netI    0.1014
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6005
_diffrn_reflns_theta_max         26.45
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    14.125
_exptl_crystal_density_diffrn    2.714
_exptl_crystal_F_000             1360
_refine_diff_density_max         3.681
_refine_diff_density_min         -3.919
_refine_diff_density_rms         0.410
_refine_ls_extinction_coef       0.00043(12)
_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_all   1.005
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1727
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_obs          0.0614
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1508
_refine_ls_wR_factor_obs         0.1318
_reflns_number_observed          1140
_reflns_number_total             1739
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000259i_2.cif
_cod_data_source_block           '[N(CH3)4][OsO3F3]_at_-117C'
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+0.0000P] 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^)+(0.0839P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        1808.1(7)
_cod_database_code               4321353