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_4321206
_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            'C18 H23 B9 Cl9 N'
_chemical_formula_weight         669.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.17(3)
_cell_angle_beta                 72.62(3)
_cell_angle_gamma                77.04(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2258(18)
_cell_length_b                   13.043(3)
_cell_length_c                   13.816(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1533.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Rikagu
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5651
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8154
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0348P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1049
_reflns_number_gt                3092
_reflns_number_total             5391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000137q_4.cif
_cod_data_source_block           R4N[2]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Psi-scan' changed to
'psi-scan' 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 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1533.1(5)
_cod_database_code               4321206