#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:09:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179315 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/12/4321204.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_4321204
loop_
_publ_author_name
'Chi-Wing Tsang'
'Qingchuan Yang'
'Eric Tung-Po Sze'
'Thomas C. W. Mak'
'Dominic T. W. Chan'
'Zuowei Xie'
_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/[σ²(Fo²)+(0.0378P)²+1.6353P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag -0.42522(5) 0.66389(4) 1.23648(4) 0.07902(16) Uani 1 1 d . . .
C1 C -0.5265(4) 1.0056(4) 0.9885(4) 0.0483(13) Uani 1 1 d . . .
H1 H -0.4930 1.0349 0.9241 0.058 Uiso 1 1 calc R . .
C2 C -0.5581(6) 0.4618(5) 1.2850(6) 0.132(4) Uani 1 1 d D . .
H2 H -0.6054 0.4351 1.2424 0.159 Uiso 1 1 calc R . .
C3 C -0.5740(6) 0.5600(6) 1.3224(4) 0.112(3) Uani 1 1 d D . .
H3 H -0.6287 0.6017 1.3009 0.134 Uiso 1 1 calc R . .
C4 C -0.5111(5) 0.5970(5) 1.3903(5) 0.115(3) Uani 1 1 d D . .
H4 H -0.5244 0.6622 1.4165 0.138 Uiso 1 1 calc R . .
C5 C -0.4266(6) 0.5362(5) 1.4202(6) 0.137(4) Uani 1 1 d D . .
H5 H -0.3858 0.5586 1.4692 0.165 Uiso 1 1 calc R . .
C6 C -0.4037(6) 0.4425(5) 1.3765(5) 0.129(3) Uani 1 1 d D . .
H6 H -0.3427 0.4060 1.3914 0.155 Uiso 1 1 calc R . .
C7 C -0.4706(5) 0.4029(6) 1.3113(5) 0.125(4) Uani 1 1 d D . .
H7 H -0.4577 0.3377 1.2851 0.150 Uiso 1 1 calc R . .
Br2 Br -0.37393(5) 0.81855(5) 1.00060(4) 0.06521(17) Uani 1 1 d . . .
Br3 Br -0.68432(5) 0.86403(5) 0.89022(3) 0.05895(17) Uani 1 1 d . . .
Br4 Br -0.68919(6) 1.18155(5) 0.99619(4) 0.06983(18) Uani 1 1 d . . .
Br5 Br -0.37464(5) 1.13630(5) 1.10605(5) 0.0811(2) Uani 1 1 d . . .
Br6 Br -0.61148(4) 0.69239(4) 1.10350(4) 0.05658(14) Uani 1 1 d . . .
Br7 Br -0.84952(4) 0.95997(5) 1.09463(5) 0.06395(16) Uani 1 1 d . . .
Br8 Br -0.62715(7) 1.15104(5) 1.25072(5) 0.0800(2) Uani 1 1 d . . .
Br9 Br -0.39887(5) 0.87982(4) 1.25193(4) 0.05894(15) Uani 1 1 d . . .
Br10 Br -0.69479(5) 0.85939(5) 1.30874(4) 0.06765(18) Uani 1 1 d . . .
B2 B -0.4879(4) 0.9006(4) 1.0460(3) 0.0374(14) Uani 1 1 d . . .
B3 B -0.6224(4) 0.9224(5) 0.9955(4) 0.0439(15) Uani 1 1 d . . .
B4 B -0.6198(5) 1.0568(5) 1.0444(4) 0.0463(16) Uani 1 1 d . . .
B5 B -0.4881(5) 1.0380(4) 1.0914(4) 0.0466(15) Uani 1 1 d . . .
B6 B -0.6016(4) 0.8446(4) 1.1020(5) 0.0487(16) Uani 1 1 d . . .
B7 B -0.6964(5) 0.9536(4) 1.1028(4) 0.0507(15) Uani 1 1 d . . .
B8 B -0.6017(5) 1.0377(5) 1.1676(4) 0.0479(17) Uani 1 1 d . . .
B9 B -0.5103(5) 0.9277(5) 1.1677(4) 0.0466(16) Uani 1 1 d . . .
B10 B -0.6366(5) 0.9117(4) 1.1959(4) 0.0449(16) Uani 1 1 d . . .
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'
Ag Ag -0.8971 1.1015 '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
C3 Ag1 C4 29.87(19) . . ?
C3 Ag1 Br9 123.06(16) . . ?
C4 Ag1 Br9 107.40(15) . . ?
C3 Ag1 Br7 108.76(15) . 3_565 ?
C4 Ag1 Br7 126.65(15) . 3_565 ?
Br9 Ag1 Br7 125.47(3) . 3_565 ?
B4 C1 B3 70.8(4) . . ?
B4 C1 B5 69.1(4) . . ?
B3 C1 B5 109.3(4) . . ?
B4 C1 B2 107.0(4) . . ?
B3 C1 B2 70.3(3) . . ?
B5 C1 B2 69.3(3) . . ?
C3 C2 C7 119.5(7) . . ?
C4 C3 C2 121.2(7) . . ?
C4 C3 Ag1 75.7(4) . . ?
C2 C3 Ag1 99.2(5) . . ?
C3 C4 C5 119.4(7) . . ?
C3 C4 Ag1 74.5(4) . . ?
C5 C4 Ag1 97.3(5) . . ?
C6 C5 C4 119.6(7) . . ?
C7 C6 C5 120.5(7) . . ?
C6 C7 C2 119.3(7) . . ?
B7 Br7 Ag1 106.04(18) . 3_465 ?
B9 Br9 Ag1 99.67(17) . . ?
C1 B2 B6 108.2(4) . . ?
C1 B2 B9 107.2(4) . . ?
B6 B2 B9 60.7(3) . . ?
C1 B2 B5 54.9(3) . . ?
B6 B2 B5 101.9(4) . . ?
B9 B2 B5 58.6(3) . . ?
C1 B2 B3 54.0(3) . . ?
B6 B2 B3 60.7(3) . . ?
B9 B2 B3 102.2(4) . . ?
B5 B2 B3 90.0(4) . . ?
C1 B2 Br2 119.4(3) . . ?
B6 B2 Br2 123.4(3) . . ?
B9 B2 Br2 124.0(3) . . ?
B5 B2 Br2 129.6(3) . . ?
B3 B2 Br2 129.3(3) . . ?
C1 B3 B4 53.7(3) . . ?
C1 B3 B6 107.0(4) . . ?
B4 B3 B6 99.4(4) . . ?
C1 B3 B7 107.0(4) . . ?
B4 B3 B7 59.3(3) . . ?
B6 B3 B7 58.9(3) . . ?
C1 B3 B2 55.7(3) . . ?
B4 B3 B2 88.2(4) . . ?
B6 B3 B2 57.7(3) . . ?
B7 B3 B2 99.1(4) . . ?
C1 B3 Br3 121.4(4) . . ?
B4 B3 Br3 133.4(4) . . ?
B6 B3 Br3 122.3(4) . . ?
B7 B3 Br3 124.0(3) . . ?
B2 B3 Br3 130.0(4) . . ?
C1 B4 B5 56.9(3) . . ?
C1 B4 B8 111.1(4) . . ?
B5 B4 B8 59.8(3) . . ?
C1 B4 B7 110.0(4) . . ?
B5 B4 B7 102.5(4) . . ?
B8 B4 B7 61.1(3) . . ?
C1 B4 B3 55.5(3) . . ?
B5 B4 B3 92.3(4) . . ?
B8 B4 B3 105.0(4) . . ?
B7 B4 B3 60.9(3) . . ?
C1 B4 Br4 119.2(4) . . ?
B5 B4 Br4 131.2(4) . . ?
B8 B4 Br4 121.4(4) . . ?
B7 B4 Br4 120.6(4) . . ?
B3 B4 Br4 127.1(4) . . ?
C1 B5 B9 108.9(4) . . ?
C1 B5 B4 54.0(3) . . ?
B9 B5 B4 101.0(4) . . ?
C1 B5 B8 109.0(4) . . ?
B9 B5 B8 60.0(3) . . ?
B4 B5 B8 60.3(3) . . ?
C1 B5 B2 55.8(3) . . ?
B9 B5 B2 59.7(3) . . ?
B4 B5 B2 89.4(4) . . ?
B8 B5 B2 102.5(4) . . ?
C1 B5 Br5 119.4(4) . . ?
B9 B5 Br5 123.5(4) . . ?
B4 B5 Br5 130.2(4) . . ?
B8 B5 Br5 121.9(4) . . ?
B2 B5 Br5 130.3(4) . . ?
B10 B6 B2 112.5(4) . . ?
B10 B6 B7 55.7(3) . . ?
B2 B6 B7 103.3(4) . . ?
B10 B6 B9 56.4(4) . . ?
B2 B6 B9 60.4(3) . . ?
B7 B6 B9 88.7(4) . . ?
B10 B6 B3 112.1(4) . . ?
B2 B6 B3 61.7(3) . . ?
B7 B6 B3 60.8(3) . . ?
B9 B6 B3 102.8(4) . . ?
B10 B6 Br6 118.8(4) . . ?
B2 B6 Br6 116.7(3) . . ?
B7 B6 Br6 135.3(3) . . ?
B9 B6 Br6 127.5(4) . . ?
B3 B6 Br6 122.0(4) . . ?
B10 B7 B6 57.2(4) . . ?
B10 B7 B4 111.7(4) . . ?
B6 B7 B4 100.8(4) . . ?
B10 B7 B3 113.1(4) . . ?
B6 B7 B3 60.3(3) . . ?
B4 B7 B3 59.8(3) . . ?
B10 B7 B8 57.9(3) . . ?
B6 B7 B8 90.7(4) . . ?
B4 B7 B8 59.2(3) . . ?
B3 B7 B8 102.9(4) . . ?
B10 B7 Br7 121.6(4) . . ?
B6 B7 Br7 133.2(3) . . ?
B4 B7 Br7 117.9(4) . . ?
B3 B7 Br7 117.3(4) . . ?
B8 B7 Br7 130.5(4) . . ?
B10 B8 B9 56.3(3) . . ?
B10 B8 B5 110.8(4) . . ?
B9 B8 B5 59.8(3) . . ?
B10 B8 B4 109.2(4) . . ?
B9 B8 B4 100.6(4) . . ?
B5 B8 B4 59.9(3) . . ?
B10 B8 B7 54.6(3) . . ?
B9 B8 B7 88.4(4) . . ?
B5 B8 B7 101.6(4) . . ?
B4 B8 B7 59.7(3) . . ?
B10 B8 Br8 120.4(4) . . ?
B9 B8 Br8 133.4(4) . . ?
B5 B8 Br8 121.4(4) . . ?
B4 B8 Br8 120.2(4) . . ?
B7 B8 Br8 130.1(4) . . ?
B10 B9 B5 113.3(4) . . ?
B10 B9 B8 58.7(3) . . ?
B5 B9 B8 60.2(3) . . ?
B10 B9 B2 111.5(4) . . ?
B5 B9 B2 61.6(3) . . ?
B8 B9 B2 104.1(4) . . ?
B10 B9 B6 56.9(3) . . ?
B5 B9 B6 102.8(4) . . ?
B8 B9 B6 92.2(4) . . ?
B2 B9 B6 58.9(3) . . ?
B10 B9 Br9 119.8(4) . . ?
B5 B9 Br9 120.7(4) . . ?
B8 B9 Br9 134.1(4) . . ?
B2 B9 Br9 115.9(4) . . ?
B6 B9 Br9 126.9(4) . . ?
B7 B10 B9 101.5(4) . . ?
B7 B10 B6 67.0(4) . . ?
B9 B10 B6 66.7(3) . . ?
B7 B10 B8 67.5(4) . . ?
B9 B10 B8 65.0(4) . . ?
B6 B10 B8 102.1(4) . . ?
B7 B10 Br10 129.9(4) . . ?
B9 B10 Br10 128.5(4) . . ?
B6 B10 Br10 128.8(4) . . ?
B8 B10 Br10 129.0(4) . . ?
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
Ag1 C3 2.628(8) . ?
Ag1 C4 2.643(7) . ?
Ag1 Br9 2.7774(9) . ?
Ag1 Br7 2.7790(9) 3_565 ?
C1 B4 1.583(8) . ?
C1 B3 1.618(8) . ?
C1 B5 1.637(8) . ?
C1 B2 1.654(7) . ?
C2 C3 1.379(9) . ?
C2 C7 1.396(9) . ?
C3 C4 1.359(9) . ?
C4 C5 1.396(9) . ?
C5 C6 1.385(9) . ?
C6 C7 1.374(9) . ?
Br2 B2 1.906(5) . ?
Br3 B3 1.883(6) . ?
Br4 B4 1.948(6) . ?
Br5 B5 1.922(6) . ?
Br6 B6 1.942(5) . ?
Br7 B7 1.952(6) . ?
Br7 Ag1 2.7790(9) 3_465 ?
Br8 B8 1.915(6) . ?
Br9 B9 1.975(6) . ?
Br10 B10 1.929(6) . ?
B2 B6 1.808(8) . ?
B2 B9 1.836(7) . ?
B2 B5 1.871(8) . ?
B2 B3 1.884(7) . ?
B3 B4 1.855(8) . ?
B3 B6 1.866(9) . ?
B3 B7 1.874(9) . ?
B4 B5 1.827(9) . ?
B4 B8 1.834(8) . ?
B4 B7 1.845(8) . ?
B5 B9 1.815(8) . ?
B5 B8 1.824(9) . ?
B6 B10 1.678(9) . ?
B6 B7 1.838(8) . ?
B6 B9 1.841(9) . ?
B7 B10 1.650(9) . ?
B7 B8 1.870(9) . ?
B8 B10 1.714(8) . ?
B8 B9 1.819(9) . ?
B9 B10 1.670(9) . ?
