Synthesis and Lewis Acid Properties of (ReO3F)∞and the X-ray Crystal Structures of (HF)2ReO3F.HF and [N(CH3)4]2-[{ReO3(μ-F)}3(μ3-O)].CH3CN
Maria V. Ivanova; Tobias Köchner; Hélène P. A. Mercier; Gary J. Schrobilgen; Inorganic Chemistry 52 (2013) 6806–6819; doi:10.1021/ic302221y

data_4335158
_publ_section_title
;
 Synthesis and Lewis Acid Properties of (ReO3F)\\infty and the X-ray
 Crystal Structures of (HF)2ReO3F.HF and
 [N(CH3)4]2-[{ReO3(\m-F)}3(\m3-O)].CH3CN
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6806
_journal_page_last               6819
_journal_paper_doi               10.1021/ic302221y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'KF 4(HF)'
_chemical_formula_sum            'F5 K'
_chemical_formula_weight         134.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :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            4
_cell_length_a                   6.287(5)
_cell_length_b                   6.287(5)
_cell_length_c                   12.937(5)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68
_cell_measurement_theta_min      0
_cell_volume                     511.4(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'SHELXTL V6.10 2001  Bruker-AXS'
_computing_publication_material  'SHELXTL V6.10 2001  Bruker-AXS'
_computing_structure_refinement  'SHELXTL V6.10 2001 Bruker-AXS'
_computing_structure_solution    'SHELXTL V6.10 2001  Bruker-AXS'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4237
_diffrn_reflns_theta_full        33.87
_diffrn_reflns_theta_max         33.87
_diffrn_reflns_theta_min         7.43
_exptl_absorpt_coefficient_mu    1.023
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       plates
_exptl_crystal_F_000             256
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                411
_reflns_number_total             494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302221y_si_002_3.cif
_cod_data_source_block           KF.4HF
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4335158