Weakly Coordinating Nature of a Carborane Cage Bearing Different Halogen Atoms. Synthesis and Structural Characterization of Icosahedral Mixed Halocarborane Anions, 1-H-CB11Y5X6- (X, Y = Cl, Br, I)
Chi-Wing Tsang; Qingchuan Yang; Eric Tung-Po Sze; Thomas C. W. Mak; Dominic T. W. Chan; Zuowei Xie; Inorganic Chemistry 39 (2000) 5851–5858; doi:10.1021/ic000354r

data_4321642
_publ_section_title
;
 Weakly Coordinating Nature of a Carborane Cage Bearing Different Halogen
 Atoms. Synthesis and Structural Characterization of Icosahedral Mixed
 Halocarborane Anions, 1-H-CB11Y5X6- (X, Y = Cl, Br, I)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5851
_journal_page_last               5858
_journal_paper_doi               10.1021/ic000354r
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C5 H9 B11 Br5 Cs I6 O'
_chemical_formula_weight         1497.89
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.736(16)
_cell_length_b                   11.319(4)
_cell_length_c                   13.804(5)
_cell_measurement_temperature    296(2)
_cell_volume                     3084(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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    0.0682
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2821
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    13.688
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5561
_exptl_absorpt_correction_type   abscor
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.636(8)
_refine_ls_extinction_coef       0.000067(12)
_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   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         2821
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.422
_refine_ls_shift/su_mean         0.039
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+13.4302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                2264
_reflns_number_total             2821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000354r_6.cif
_cod_data_source_block           Cs[1-H-CB11Br5I6](THF)
_cod_database_code               4321642