Lewis Acid Behavior of ReO2F3: Synthesis of (ReO2F3)∞, ReO2F4-, Re2O4F7-, Re3O6F10-, and ReO2F3(CH3CN) and Study by NMR Spectroscopy, Raman Spectroscopy, and Density Functional Theory Calculations; and X-ray Structures of [Li][ReO2F4], [K][Re2O4F7], [K][Re2O4F7].2ReO2F3, [Cs][Re3O6F10], and ReO3F(CH3CN)2.CH3CN
William J. Casteel; David A. Dixon; Nicolas LeBlond; Philippa E. Lock; Hélène P. A. Mercier; Gary J. Schrobilgen; Inorganic Chemistry 38 (1999) 2340–2358; doi:10.1021/ic980695t

data_4321984
_publ_section_title
;
 Lewis Acid Behavior of ReO2F3: Synthesis of (ReO2F3)\\infty, ReO2F4-,
 Re2O4F7-, Re3O6F10-, and ReO2F3(CH3CN) and Study by NMR Spectroscopy,
 Raman Spectroscopy, and Density Functional Theory Calculations; and X-ray
 Structures of [Li][ReO2F4], [K][Re2O4F7], [K][Re2O4F7].2ReO2F3,
 [Cs][Re3O6F10], and ReO3F(CH3CN)2.CH3CN
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2340
_journal_page_last               2358
_journal_paper_doi               10.1021/ic980695t
_journal_volume                  38
_journal_year                    1999
_chemical_formula_analytical     K+Re2O4F7-/2ReO2F3
_chemical_formula_structural     K+Re2O4F7-/2ReO2F3
_chemical_formula_sum            'F13 K O8 Re2'
_chemical_formula_weight         786.48
_chemical_name_systematic
'mu-fluorohexafluorotetraoxodirhenate dioxotrifluororhenium adduct'
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 99.53(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   27.319(24)
_cell_length_b                   5.274(5)
_cell_length_c                   5.355(3)
_cell_measurement_temperature    213(2)
_cell_volume                     760.9(11)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            4192
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    32.167
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.058
_exptl_crystal_description       needle
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.831
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.303
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.56(2)
_refine_ls_extinction_coef       0.0058(2)
_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   1.162
_refine_ls_goodness_of_fit_obs   1.162
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1718
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.294
_refine_ls_restrained_S_obs      1.161
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_obs          0.0244
_refine_ls_shift/esd_max         -15.787
_refine_ls_shift/esd_mean        0.322
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+3.3856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0677
_refine_ls_wR_factor_obs         0.0603
_reflns_number_observed          1690
_reflns_number_total             1719
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980695t_3.cif
_cod_data_source_block           Kre2o4f7.2reo2f3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+3.3856P] 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^)+(0.0333P)^2^+3.3856P] where P=(Fo^2^+2Fc^2^)/3'.

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

2022-02-23
Changed obviously wrong number of Re atoms in formula
                 miguel
;
_cod_original_formula_sum            'F13 K O8 Re4'
_cod_original_formula_weight         1158.90
_cod_database_code               4321984