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_4335159
_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_sum            'C10 H27 F3 N3 O10 Re3'
_chemical_formula_weight         964.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 124.301(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1792(5)
_cell_length_b                   20.3457(12)
_cell_length_c                   14.3432(6)
_cell_measurement_temperature    293(2)
_cell_volume                     2212.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_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  0.0688
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            37716
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    16.444
_exptl_crystal_density_diffrn    2.896
_exptl_crystal_F_000             1760
_refine_diff_density_max         7.281
_refine_diff_density_min         -3.100
_refine_diff_density_rms         0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         7951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                6490
_reflns_number_total             7951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302221y_si_002_4.cif
_cod_data_source_block           new
_cod_database_code               4335159