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_4335157
_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         'C4 H12 N, O4 Re'
_chemical_formula_sum            'C4 H12 N O4 Re'
_chemical_formula_weight         324.35
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.7730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.7206(2)
_cell_length_b                   12.4740(3)
_cell_length_c                   13.1586(4)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      78
_cell_measurement_theta_min      0
_cell_volume                     845.58(4)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4944
_diffrn_reflns_theta_full        39.01
_diffrn_reflns_theta_max         39.01
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    14.335
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.548
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.884
_refine_diff_density_min         -4.242
_refine_diff_density_rms         0.329
_refine_ls_extinction_coef       0.0092(6)
_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   0.909
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         4944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+4.5547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                4090
_reflns_number_total             4944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302221y_si_002_2.cif
_cod_data_source_block           N(CH3)4ReO4
_cod_original_cell_volume        845.57(4)
_cod_database_code               4335157