#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:33:56 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179335 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/32/4323204.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4323204
loop_
_publ_author_name
'Zuowei Xie'
'Chi-Wing Tsang'
'Eric Tung-Po Sze'
'Qingchuan Yang'
'Dominic T. W. Chan'
'Thomas C. W. Mak'
_publ_section_title
;
 Highly Chlorinated, Brominated, and Iodinated Icosahedral Carborane
 Anions: 1-H-CB11X11-, 1-CH3-CB11X11- (X = Cl, Br, I); 1-Br-CB11Br11-
;
_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
; 
 ? 
;
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0210P)²+6.0101P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Br1 Br 0.93105(6) 0.37021(6) -0.21385(2) 0.0558(2) Uani 0.9101(5) d PD .
Br2 Br 1.15071(6) 0.72899(7) -0.31228(2) 0.0554(2) Uani 0.9101(5) d PD .
Br3 Br 1.22580(6) 0.26301(5) -0.14948(2) 0.0501(2) Uani 0.9101(5) d PD .
Br4 Br 1.08911(6) 0.48223(6) -0.05077(2) 0.0484(2) Uani 0.9101(5) d PD .
B1 B 1.1425(4) 0.5289(6) -0.1953(3) 0.072(2) Uani 1 d D .
B2 B 1.2433(4) 0.6986(4) -0.2407(2) 0.043(2) Uani 1 d D .
B3 B 1.2835(5) 0.4781(3) -0.1663(2) 0.0250(13) Uani 1 d D .
B4 B 1.2215(5) 0.5839(5) -0.11965(14) 0.034(2) Uani 1 d D .
Cs1 Cs 0.6667 1.3333 0.05388(6) 0.0593(3) Uani 0.50 d SP .
Cs2 Cs 0.6667 1.3333 -0.08317(8) 0.0756(5) Uani 0.50 d SP .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
B1 Br1 Cs2 109.2(2) . 1_545 ?
B1 Br1 Cs1 101.3(2) . 7_534 ?
Cs2 Br1 Cs1 124.87(2) 1_545 7_534 ?
B2 Br2 Cs1 109.91(14) . 7_544 ?
B3 Br3 Cs1 110.75(13) . 7_534 ?
B3 Br3 Cs2 99.77(13) . 1_645 ?
Cs1 Br3 Cs2 124.99(2) 7_534 1_645 ?
B4 Br4 Cs2 112.56(13) . 1_545 ?
B3 B1 B2 59.2(3) 3_775 . ?
B3 B1 B2 109.0(3) 3_775 2_755 ?
B2 B1 B2 63.2(3) . 2_755 ?
B3 B1 B3 107.3(3) 3_775 . ?
B2 B1 B3 108.5(3) . . ?
B2 B1 B3 57.9(2) 2_755 . ?
B3 B1 B4 59.7(3) 3_775 . ?
B2 B1 B4 106.8(3) . . ?
B2 B1 B4 105.4(3) 2_755 . ?
B3 B1 B4 58.8(3) . . ?
B3 B1 Br1 123.8(3) 3_775 . ?
B2 B1 Br1 121.0(3) . . ?
B2 B1 Br1 119.5(3) 2_755 . ?
B3 B1 Br1 121.3(3) . . ?
B4 B1 Br1 124.7(3) . . ?
B3 B2 B1 60.5(3) 3_775 . ?
B3 B2 B1 61.4(3) 3_775 3_775 ?
B1 B2 B1 109.3(4) . 3_775 ?
B3 B2 B2 106.9(2) 3_775 3_775 ?
B1 B2 B2 107.6(3) . 3_775 ?
B1 B2 B2 57.6(3) 3_775 3_775 ?
B3 B2 B2 107.0(2) 3_775 2_755 ?
B1 B2 B2 59.2(3) . 2_755 ?
B1 B2 B2 106.3(2) 3_775 2_755 ?
B2 B2 B2 60.0 3_775 2_755 ?
B3 B2 Br2 125.8(3) 3_775 . ?
B1 B2 Br2 121.9(2) . . ?
B1 B2 Br2 123.4(3) 3_775 . ?
B2 B2 Br2 119.71(14) 3_775 . ?
B2 B2 Br2 119.1(2) 2_755 . ?
B2 B3 B4 109.1(3) 2_755 . ?
B2 B3 B1 60.3(2) 2_755 2_755 ?
B4 B3 B1 107.7(2) . 2_755 ?
B2 B3 B4 108.8(2) 2_755 2_755 ?
B4 B3 B4 57.5(3) . 2_755 ?
B1 B3 B4 61.3(3) 2_755 2_755 ?
B2 B3 B1 60.7(2) 2_755 . ?
B4 B3 B1 60.6(3) . . ?
B1 B3 B1 108.5(3) 2_755 . ?
B4 B3 B1 106.6(3) 2_755 . ?
B2 B3 Br3 120.8(3) 2_755 . ?
B4 B3 Br3 122.0(2) . . ?
B1 B3 Br3 121.3(3) 2_755 . ?
B4 B3 Br3 122.4(3) 2_755 . ?
B1 B3 Br3 121.7(2) . . ?
B4 B4 B4 60.0 3_775 2_755 ?
B4 B4 B3 109.4(3) 3_775 . ?
B4 B4 B3 61.5(3) 2_755 . ?
B4 B4 B3 61.1(3) 3_775 3_775 ?
B4 B4 B3 109.0(3) 2_755 3_775 ?
B3 B4 B3 108.1(3) . 3_775 ?
B4 B4 B1 108.7(2) 3_775 . ?
B4 B4 B1 109.8(2) 2_755 . ?
B3 B4 B1 60.6(3) . . ?
B3 B4 B1 59.0(3) 3_775 . ?
B4 B4 Br4 122.6(2) 3_775 . ?
B4 B4 Br4 121.4(3) 2_755 . ?
B3 B4 Br4 119.7(3) . . ?
B3 B4 Br4 121.9(3) 3_775 . ?
B1 B4 Br4 119.9(2) . . ?
Cs2 Cs1 Br2 78.72(2) . 4_455 ?
Cs2 Cs1 Br2 78.72(2) . 5_665 ?
Br2 Cs1 Br2 116.270(13) 4_455 5_665 ?
Cs2 Cs1 Br2 78.72(2) . 6_575 ?
Br2 Cs1 Br2 116.270(13) 4_455 6_575 ?
Br2 Cs1 Br2 116.268(13) 5_665 6_575 ?
Cs2 Cs1 Br3 139.86(2) . 6_675 ?
Br2 Cs1 Br3 62.22(2) 4_455 6_675 ?
Br2 Cs1 Br3 125.58(2) 5_665 6_675 ?
Br2 Cs1 Br3 109.45(2) 6_575 6_675 ?
Cs2 Cs1 Br3 139.86(2) . 4_465 ?
Br2 Cs1 Br3 109.45(2) 4_455 4_465 ?
Br2 Cs1 Br3 62.22(2) 5_665 4_465 ?
Br2 Cs1 Br3 125.58(2) 6_575 4_465 ?
Br3 Cs1 Br3 67.87(3) 6_675 4_465 ?
Cs2 Cs1 Br3 139.86(2) . 5 ?
Br2 Cs1 Br3 125.58(2) 4_455 5 ?
Br2 Cs1 Br3 109.45(2) 5_665 5 ?
Br2 Cs1 Br3 62.22(2) 6_575 5 ?
Br3 Cs1 Br3 67.87(3) 6_675 5 ?
Br3 Cs1 Br3 67.87(3) 4_465 5 ?
Cs2 Cs1 Br1 109.84(2) . 6_675 ?
Br2 Cs1 Br1 56.365(10) 4_455 6_675 ?
Br2 Cs1 Br1 77.598(10) 5_665 6_675 ?
Br2 Cs1 Br1 165.43(2) 6_575 6_675 ?
Br3 Cs1 Br1 56.32(2) 6_675 6_675 ?
Br3 Cs1 Br1 55.203(15) 4_465 6_675 ?
Br3 Cs1 Br1 110.30(3) 5 6_675 ?
Cs2 Cs1 Br1 109.84(2) . 5 ?
Br2 Cs1 Br1 77.598(10) 4_455 5 ?
Br2 Cs1 Br1 165.43(2) 5_665 5 ?
Br2 Cs1 Br1 56.364(10) 6_575 5 ?
Br3 Cs1 Br1 55.203(15) 6_675 5 ?
Br3 Cs1 Br1 110.30(3) 4_465 5 ?
Br3 Cs1 Br1 56.32(2) 5 5 ?
Br1 Cs1 Br1 109.10(2) 6_675 5 ?
Cs2 Cs1 Br1 109.84(2) . 4_465 ?
Br2 Cs1 Br1 165.43(2) 4_455 4_465 ?
Br2 Cs1 Br1 56.364(10) 5_665 4_465 ?
Br2 Cs1 Br1 77.597(10) 6_575 4_465 ?
Br3 Cs1 Br1 110.30(3) 6_675 4_465 ?
Br3 Cs1 Br1 56.32(2) 4_465 4_465 ?
Br3 Cs1 Br1 55.202(15) 5 4_465 ?
Br1 Cs1 Br1 109.10(2) 6_675 4_465 ?
Br1 Cs1 Br1 109.10(2) 5 4_465 ?
Cs1 Cs2 Br4 78.89(3) . 1_565 ?
Cs1 Cs2 Br4 78.89(3) . 3_675 ?
Br4 Cs2 Br4 116.38(2) 1_565 3_675 ?
Cs1 Cs2 Br4 78.89(3) . 2_665 ?
Br4 Cs2 Br4 116.38(2) 1_565 2_665 ?
Br4 Cs2 Br4 116.38(2) 3_675 2_665 ?
Cs1 Cs2 Br1 139.84(2) . 1_565 ?
Br4 Cs2 Br1 62.00(2) 1_565 1_565 ?
Br4 Cs2 Br1 109.45(2) 3_675 1_565 ?
Br4 Cs2 Br1 125.33(3) 2_665 1_565 ?
Cs1 Cs2 Br1 139.84(2) . 3_675 ?
Br4 Cs2 Br1 125.33(3) 1_565 3_675 ?
Br4 Cs2 Br1 62.00(2) 3_675 3_675 ?
Br4 Cs2 Br1 109.45(2) 2_665 3_675 ?
Br1 Cs2 Br1 67.90(3) 1_565 3_675 ?
Cs1 Cs2 Br1 139.84(2) . 2_665 ?
Br4 Cs2 Br1 109.45(2) 1_565 2_665 ?
Br4 Cs2 Br1 125.33(3) 3_675 2_665 ?
Br4 Cs2 Br1 62.00(2) 2_665 2_665 ?
Br1 Cs2 Br1 67.90(3) 1_565 2_665 ?
Br1 Cs2 Br1 67.90(3) 3_675 2_665 ?
Cs1 Cs2 Br3 109.98(2) . 2_655 ?
Br4 Cs2 Br3 77.158(12) 1_565 2_655 ?
Br4 Cs2 Br3 56.717(12) 3_675 2_655 ?
Br4 Cs2 Br3 165.60(3) 2_665 2_655 ?
Br1 Cs2 Br3 54.93(2) 1_565 2_655 ?
Br1 Cs2 Br3 56.38(2) 3_675 2_655 ?
Br1 Cs2 Br3 110.17(4) 2_665 2_655 ?
Cs1 Cs2 Br3 109.98(2) . 3_785 ?
Br4 Cs2 Br3 56.717(12) 1_565 3_785 ?
Br4 Cs2 Br3 165.60(3) 3_675 3_785 ?
Br4 Cs2 Br3 77.158(12) 2_665 3_785 ?
Br1 Cs2 Br3 56.38(2) 1_565 3_785 ?
Br1 Cs2 Br3 110.17(4) 3_675 3_785 ?
Br1 Cs2 Br3 54.93(2) 2_665 3_785 ?
Br3 Cs2 Br3 108.96(2) 2_655 3_785 ?
Cs1 Cs2 Br3 109.98(2) . 1_465 ?
Br4 Cs2 Br3 165.60(3) 1_565 1_465 ?
Br4 Cs2 Br3 77.158(12) 3_675 1_465 ?
Br4 Cs2 Br3 56.717(12) 2_665 1_465 ?
Br1 Cs2 Br3 110.17(4) 1_565 1_465 ?
Br1 Cs2 Br3 54.93(2) 3_675 1_465 ?
Br1 Cs2 Br3 56.38(2) 2_665 1_465 ?
Br3 Cs2 Br3 108.96(2) 2_655 1_465 ?
Br3 Cs2 Br3 108.96(2) 3_785 1_465 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 B1 1.917(3) . ?
Br1 Cs2 3.7783(15) 1_545 ?
Br1 Cs1 4.2724(10) 7_534 ?
Br2 B2 1.922(4) . ?
Br2 Cs1 3.7080(9) 7_544 ?
Br3 B3 1.930(3) . ?
Br3 Cs1 3.7571(12) 7_534 ?
Br3 Cs2 4.2885(10) 1_645 ?
Br4 B4 1.925(3) . ?
Br4 Cs2 3.7156(8) 1_545 ?
B1 B3 1.768(7) 3_775 ?
B1 B2 1.764(6) . ?
B1 B2 1.795(6) 2_755 ?
B1 B3 1.808(8) . ?
B1 B4 1.809(7) . ?
B2 B3 1.744(6) 3_775 ?
B2 B1 1.795(6) 3_775 ?
B2 B2 1.864(8) 3_775 ?
B2 B2 1.864(8) 2_755 ?
B3 B2 1.744(6) 2_755 ?
B3 B4 1.775(7) . ?
B3 B1 1.768(7) 2_755 ?
B3 B4 1.782(6) 2_755 ?
B4 B4 1.710(6) 3_775 ?
B4 B4 1.710(6) 2_755 ?
B4 B3 1.782(6) 3_775 ?
Cs1 Cs2 3.029(2) . ?
Cs1 Br2 3.7080(9) 4_455 ?
Cs1 Br2 3.7080(9) 5_665 ?
Cs1 Br2 3.7080(9) 6_575 ?
Cs1 Br3 3.7571(12) 6_675 ?
Cs1 Br3 3.7571(12) 4_465 ?
Cs1 Br3 3.7571(12) 5 ?
Cs1 Br1 4.2723(10) 6_675 ?
Cs1 Br1 4.2723(10) 5 ?
Cs1 Br1 4.2724(10) 4_465 ?
Cs2 Br4 3.7156(8) 1_565 ?
Cs2 Br4 3.7156(8) 3_675 ?
Cs2 Br4 3.7156(8) 2_665 ?
Cs2 Br1 3.7783(15) 1_565 ?
Cs2 Br1 3.7783(15) 3_675 ?
Cs2 Br1 3.7783(15) 2_665 ?
Cs2 Br3 4.2885(10) 2_655 ?
Cs2 Br3 4.2885(10) 3_785 ?
Cs2 Br3 4.2885(10) 1_465 ?
