Highly Chlorinated, Brominated, and Iodinated Icosahedral Carborane Anions: 1-H-CB11X11-, 1-CH3-CB11X11- (X = Cl, Br, I); 1-Br-CB11Br11-
Zuowei Xie; Chi-Wing Tsang; Eric Tung-Po Sze; Qingchuan Yang; Dominic T. W. Chan; Thomas C. W. Mak; Inorganic Chemistry 37 (1998) 6444–6451; doi:10.1021/ic9805628

data_4323204
_publ_section_title
;
 Highly Chlorinated, Brominated, and Iodinated Icosahedral Carborane
 Anions: 1-H-CB11X11-, 1-CH3-CB11X11- (X = Cl, Br, I); 1-Br-CB11Br11-
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6444
_journal_page_last               6451
_journal_paper_doi               10.1021/ic9805628
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C H B11 Br11 Cs'
_chemical_formula_weight         1143.85
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.8243(14)
_cell_length_b                   9.8243(14)
_cell_length_c                   22.098(4)
_cell_measurement_temperature    296(2)
_cell_volume                     1847.1(5)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC7R '
_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  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            2297
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.57
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    19.338
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.418
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.085
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1506
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.28(5)
_refine_ls_extinction_coef       0.00206(4)
_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_all   1.024
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1136
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.096
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_obs          0.0343
_refine_ls_shift/esd_max         0.546
_refine_ls_shift/esd_mean        0.045
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+6.0101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0877
_refine_ls_wR_factor_obs         0.0727
_reflns_number_observed          813
_reflns_number_total             1148
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9805628_3.cif
_cod_data_source_block           Cs[5]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+6.0101P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+6.0101P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4323204