#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:44:19 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179260 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/80/4318072.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_4318072
loop_
_publ_author_name
'Chongchan Lee'
'Junghyun Lee'
'Soon W. Lee'
'Sang Ook Kang'
'Jaejung Ko'
_publ_section_title
;
 Synthesis and Reactivity of 1,2-Bis(chlorodimethylgermyl)carborane and
 1,2-Bis(bromodimethylstannyl)carborane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3084
_journal_page_last               3090
_journal_paper_doi               10.1021/ic0110878
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C8 H28 B10 Sn3'
_chemical_formula_weight         588.47
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   15.5491(7)
_cell_length_b                   11.7044(5)
_cell_length_c                   11.4205(5)
_cell_measurement_reflns_used    12892
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.21
_cell_volume                     2078.45(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12892
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    3.561
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.204
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2705
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0407P)²+1.6026P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0897
_reflns_number_gt                2332
_reflns_number_total             2705
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0110878_2.cif
_cod_data_source_block           kjj31
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_database_code               4318072
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Sn1 Sn 0.302187(16) 0.078864(19) 0.39541(3) 0.04332(10) Uani 1 1 d . . .
Sn2 Sn 0.28896(3) 0.2500 0.56032(4) 0.04920(12) Uani 1 2 d S . .
C1 C 0.3649(2) 0.1774(3) 0.2535(3) 0.0424(7) Uani 1 1 d . . .
C2 C 0.3865(3) -0.0592(4) 0.4389(5) 0.0681(12) Uani 1 1 d . . .
H2A H 0.4373 -0.0295 0.4758 0.082 Uiso 1 1 calc R . .
H2B H 0.4022 -0.0994 0.3689 0.082 Uiso 1 1 calc R . .
H2C H 0.3579 -0.1105 0.4916 0.082 Uiso 1 1 calc R . .
C3 C 0.1906(3) 0.0125(4) 0.3119(5) 0.0606(11) Uani 1 1 d . . .
H3A H 0.1537 0.0744 0.2891 0.073 Uiso 1 1 calc R . .
H3B H 0.1605 -0.0367 0.3651 0.073 Uiso 1 1 calc R . .
H3C H 0.2072 -0.0300 0.2437 0.073 Uiso 1 1 calc R . .
C4 C 0.4039(4) 0.2500 0.6639(6) 0.0658(16) Uani 1 2 d S . .
H4A H 0.4532 0.2500 0.6133 0.079 Uiso 1 2 calc SR . .
H4B H 0.4050 0.1830 0.7124 0.079 Uiso 0.50 1 calc PR . .
H4C H 0.4050 0.3170 0.7124 0.079 Uiso 0.50 1 calc PR . .
C5 C 0.1727(5) 0.2500 0.6615(6) 0.0681(17) Uani 1 2 d S . .
H5A H 0.1240 0.2500 0.6098 0.082 Uiso 1 2 calc SR . .
H5B H 0.1710 0.3170 0.7100 0.082 Uiso 0.50 1 calc PR . .
H5C H 0.1710 0.1830 0.7100 0.082 Uiso 0.50 1 calc PR . .
B1 B 0.3534(5) 0.2500 0.0232(7) 0.0572(16) Uani 1 2 d S . .
H1 H 0.3222 0.2500 -0.0493 0.069 Uiso 1 2 calc SR . .
B2 B 0.2991(4) 0.2500 0.1583(5) 0.0429(12) Uani 1 2 d S . .
H2 H 0.2375 0.2500 0.1641 0.052 Uiso 1 2 calc SR . .
B3 B 0.5157(5) 0.2500 0.1452(8) 0.0643(19) Uani 1 2 d S . .
H3 H 0.5774 0.2500 0.1426 0.077 Uiso 1 2 calc SR . .
B4 B 0.3582(3) 0.1275(4) 0.1137(4) 0.0524(10) Uani 1 1 d . . .
H4 H 0.3302 0.0573 0.0930 0.063 Uiso 1 1 calc R . .
B5 B 0.4518(4) 0.1740(4) 0.0399(5) 0.0619(13) Uani 1 1 d . . .
H5 H 0.4771 0.1313 -0.0230 0.074 Uiso 1 1 calc R . .
B6 B 0.4565(3) 0.1274(4) 0.1882(5) 0.0545(11) Uani 1 1 d . . .
H6 H 0.4847 0.0575 0.2099 0.065 Uiso 1 1 calc R . .
B7 B 0.4582(4) 0.2500 0.2807(7) 0.0504(13) Uani 1 2 d S . .
H7 H 0.4862 0.2500 0.3556 0.060 Uiso 1 2 calc SR . .
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'
Sn Sn -0.6537 1.4246 '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 Sn1 C2 109.19(19) . . ?
C3 Sn1 C1 102.76(17) . . ?
C2 Sn1 C1 107.05(18) . . ?
C3 Sn1 Sn2 120.71(14) . . ?
C2 Sn1 Sn2 115.82(15) . . ?
C1 Sn1 Sn2 98.89(9) . . ?
C4 Sn2 C5 113.9(3) . . ?
C4 Sn2 Sn1 108.35(13) . . ?
C5 Sn2 Sn1 115.51(13) . . ?
C4 Sn2 Sn1 108.35(13) . 7_565 ?
C5 Sn2 Sn1 115.51(13) . 7_565 ?
Sn1 Sn2 Sn1 93.187(16) . 7_565 ?
C1 C1 B4 110.02(19) 7_565 . ?
C1 C1 B7 60.19(15) 7_565 . ?
B4 C1 B7 113.1(4) . . ?
C1 C1 B6 109.99(18) 7_565 . ?
B4 C1 B6 61.6(3) . . ?
B7 C1 B6 62.8(3) . . ?
C1 C1 B2 60.33(15) 7_565 . ?
B4 C1 B2 62.6(3) . . ?
B7 C1 B2 112.0(3) . . ?
B6 C1 B2 112.9(3) . . ?
C1 C1 Sn1 121.36(9) 7_565 . ?
B4 C1 Sn1 118.8(2) . . ?
B7 C1 Sn1 120.0(3) . . ?
B6 C1 Sn1 120.5(2) . . ?
B2 C1 Sn1 117.3(3) . . ?
B2 B1 B4 60.5(3) . . ?
B2 B1 B4 60.5(3) . 7_565 ?
B4 B1 B4 108.3(5) . 7_565 ?
B2 B1 B5 108.5(5) . . ?
B4 B1 B5 59.7(3) . . ?
B4 B1 B5 107.8(5) 7_565 . ?
B2 B1 B5 108.5(5) . 7_565 ?
B4 B1 B5 107.8(5) . 7_565 ?
B4 B1 B5 59.7(3) 7_565 7_565 ?
B5 B1 B5 60.0(4) . 7_565 ?
C1 B2 C1 59.3(3) . 7_565 ?
C1 B2 B1 105.6(4) . . ?
C1 B2 B1 105.6(4) 7_565 . ?
C1 B2 B4 58.3(2) . . ?
C1 B2 B4 105.8(4) 7_565 . ?
B1 B2 B4 60.0(3) . . ?
C1 B2 B4 105.8(4) . 7_565 ?
C1 B2 B4 58.3(2) 7_565 7_565 ?
B1 B2 B4 60.0(3) . 7_565 ?
B4 B2 B4 107.5(4) . 7_565 ?
B6 B3 B6 108.0(4) . 7_565 ?
B6 B3 B7 60.0(3) . . ?
B6 B3 B7 60.0(3) 7_565 . ?
B6 B3 B5 59.8(3) . . ?
B6 B3 B5 107.4(5) 7_565 . ?
B7 B3 B5 107.6(4) . . ?
B6 B3 B5 107.4(5) . 7_565 ?
B6 B3 B5 59.8(3) 7_565 7_565 ?
B7 B3 B5 107.6(4) . 7_565 ?
B5 B3 B5 59.4(4) . 7_565 ?
C1 B4 B6 59.4(2) . . ?
C1 B4 B5 106.9(3) . . ?
B6 B4 B5 60.8(3) . . ?
C1 B4 B1 105.8(3) . . ?
B6 B4 B1 108.8(4) . . ?
B5 B4 B1 60.5(3) . . ?
C1 B4 B2 59.1(3) . . ?
B6 B4 B2 108.2(3) . . ?
B5 B4 B2 108.3(3) . . ?
B1 B4 B2 59.5(3) . . ?
B4 B5 B5 107.9(2) . 7_565 ?
B4 B5 B6 59.1(3) . . ?
B5 B5 B6 107.8(2) 7_565 . ?
B4 B5 B1 59.8(3) . . ?
B5 B5 B1 60.0(2) 7_565 . ?
B6 B5 B1 106.9(4) . . ?
B4 B5 B3 106.8(4) . . ?
B5 B5 B3 60.3(2) 7_565 . ?
B6 B5 B3 59.5(3) . . ?
B1 B5 B3 107.5(4) . . ?
C1 B6 B4 58.9(2) . . ?
C1 B6 B3 106.0(3) . . ?
B4 B6 B3 108.5(4) . . ?
C1 B6 B5 106.0(3) . . ?
B4 B6 B5 60.0(3) . . ?
B3 B6 B5 60.7(4) . . ?
C1 B6 B7 58.6(3) . . ?
B4 B6 B7 107.5(3) . . ?
B3 B6 B7 60.3(3) . . ?
B5 B6 B7 108.5(4) . . ?
C1 B7 C1 59.6(3) . 7_565 ?
C1 B7 B6 58.6(2) . . ?
C1 B7 B6 106.3(4) 7_565 . ?
C1 B7 B6 106.3(4) . 7_565 ?
C1 B7 B6 58.6(2) 7_565 7_565 ?
B6 B7 B6 107.3(5) . 7_565 ?
C1 B7 B3 105.5(5) . . ?
C1 B7 B3 105.5(5) 7_565 . ?
B6 B7 B3 59.6(3) . . ?
B6 B7 B3 59.6(3) 7_565 . ?
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
Sn1 C3 2.127(4) . ?
Sn1 C2 2.139(4) . ?
Sn1 C1 2.215(4) . ?
Sn1 Sn2 2.7571(4) . ?
Sn2 C4 2.143(7) . ?
Sn2 C5 2.146(7) . ?
Sn2 Sn1 2.7571(4) 7_565 ?
C1 C1 1.701(6) 7_565 ?
C1 B4 1.703(6) . ?
C1 B7 1.710(6) . ?
C1 B6 1.712(5) . ?
C1 B2 1.718(6) . ?
B1 B2 1.759(9) . ?
B1 B4 1.769(7) . ?
B1 B4 1.769(7) 7_565 ?
B1 B5 1.780(9) . ?
B1 B5 1.780(9) 7_565 ?
B2 C1 1.718(6) 7_565 ?
B2 B4 1.778(6) . ?
B2 B4 1.778(6) 7_565 ?
B3 B6 1.775(6) . ?
B3 B6 1.775(6) 7_565 ?
B3 B7 1.787(10) . ?
B3 B5 1.796(10) . ?
B3 B5 1.796(10) 7_565 ?
B4 B6 1.750(7) . ?
B4 B5 1.767(7) . ?
B5 B5 1.780(10) 7_565 ?
B5 B6 1.780(7) . ?
B6 B7 1.782(7) . ?
B7 C1 1.710(6) 7_565 ?
B7 B6 1.782(7) 7_565 ?
