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_4321638
_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            'C19 H25 Ag B11 Br6 Cl5'
_chemical_formula_weight         1136.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.17(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.709(7)
_cell_length_b                   12.168(6)
_cell_length_c                   18.138(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     3688(4)
_computing_cell_refinement       'MAC/AFC Diffractometer Control'
_computing_data_collection       'MAC/AFC Diffractometer Control'
_computing_data_reduction        'MAC/AFC Diffractometer Control'
_computing_molecular_graphics    'Seimens SHELXTL'
_computing_publication_material  'Seimens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1475
_diffrn_reflns_av_sigmaI/netI    0.1765
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13122
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0.2397
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.426
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7300
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.00097(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_ref   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.1727
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.277
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                2923
_reflns_number_total             6507
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000354r_2.cif
_cod_data_source_block           Ag[1-H-CB11Cl5Br6](mesitylene)2
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4321638