X-ray Crystal Structures of [XF6][Sb2F11] (X = Cl, Br, I); 35,37Cl, 79,81Br, and 127I NMR Studies and Electronic Structure Calculations of the XF6+ Cations
John F. Lehmann; Gary J. Schrobilgen; Karl O. Christe; Andreas Kornath; Reijo J. Suontamo; Inorganic Chemistry 43 (2004) 6905–6921; doi:10.1021/ic040015o

data_4311868
_publ_section_title
;
 X-ray Crystal Structures of [XF6][Sb2F11] (X = Cl, Br, I); 35,37Cl,
 79,81Br, and 127I NMR Studies and Electronic Structure Calculations of
 the XF6+ Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6905
_journal_page_last               6921
_journal_paper_doi               10.1021/ic040015o
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'Br2 F17 Sb2'
_chemical_formula_weight         726.32
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.558(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.930(2)
_cell_length_b                   8.4918(15)
_cell_length_c                   12.103(2)
_cell_measurement_temperature    143(2)
_cell_volume                     1215.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0866
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10838
_diffrn_reflns_theta_full        28.96
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    11.227
_exptl_crystal_density_diffrn    3.969
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1300
_refine_diff_density_max         2.980
_refine_diff_density_min         -2.430
_refine_diff_density_rms         0.320
_refine_ls_extinction_coef       0.00045(9)
_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   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0707
_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^)+(0.0215P)^2^+58.9173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                1943
_reflns_number_total             2946
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040015o_2.cif
_cod_data_source_block           BrF6+Sb2F11-
_cod_database_code               4311868