Synthesis and Structural Characterization of Highly Chlorinated, Brominated, Iodinated, and Methylated Carborane Anions, 1-H-CB9X9-, 1-NH2-CB9X9- (X = Cl, Br, I), and 1-H-CB9(CH3)9-
Chi-Wing Tsang; Qingchuan Yang; Eric Tung-Po Sze; Thomas C. W. Mak; Dominic T. W. Chan; Zuowei Xie; Inorganic Chemistry 39 (2000) 3582–3589; doi:10.1021/ic000137q

data_4321204
_publ_section_title
;
 Synthesis and Structural Characterization of Highly Chlorinated,
 Brominated, Iodinated, and Methylated Carborane Anions, 1-H-CB9X9-,
 1-NH2-CB9X9- (X = Cl, Br, I), and 1-H-CB9(CH3)9-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3582
_journal_page_last               3589
_journal_paper_doi               10.1021/ic000137q
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C7 H7 Ag B9 Br9'
_chemical_formula_weight         1015.48
_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                   12.716(3)
_cell_length_b                   12.726(3)
_cell_length_c                   14.638(3)
_cell_measurement_temperature    296(2)
_cell_volume                     2368.8(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'IP Rigaku'
_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    0.1048
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3861
_diffrn_reflns_theta_full        25.52
_diffrn_reflns_theta_max         25.52
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    16.026
_exptl_absorpt_correction_T_max  1.292
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_type   Abscor
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.847
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.516(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3861
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+1.6353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                3403
_reflns_number_total             3861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000137q_2.cif
_cod_data_source_block           Ag[3](benzene)
_cod_original_cell_volume        2368.8(8)
_cod_database_code               4321204