#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:04:11 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179091 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/53/4305369.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_4305369
loop_
_publ_author_name
'Marius Kirchmann'
'Klaus Eichele'
'Lars Wesemann'
_publ_contact_author             'Lars Wesemann'
_publ_contact_author_address
;
Institut für Anorganische Chemie
Universität Tübingen
Auf der Morgenstelle 18
72076 Tübingen
Germany
;
_publ_contact_author_fax         0497071292436
_publ_contact_author_phone       04970712976227
_publ_section_title
;
Homoleptic Cadmium and Mercury Compounds of Stanna-closo-dodecaborate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5988
_journal_page_last               5991
_journal_paper_doi               10.1021/ic800357z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'B44 H44 Hg Sn4, 8(C3 H10 N), 2(Cl)'
_chemical_formula_sum            'C24 H124 B44 Cl2 Hg N8 Sn4'
_chemical_formula_weight         1747.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           121
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_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            2
_cell_length_a                   14.9235(16)
_cell_length_b                   14.9235(16)
_cell_length_c                   20.3832(16)
_cell_measurement_temperature    173(2)
_cell_volume                     4539.6(8)
_computing_cell_refinement       'Stoe X-Area 1.26'
_computing_data_collection       'Stoe X-Area 1.26'
_computing_data_reduction        'SToe X-Area 1.26'
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       ω-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  0.0648
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25889
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         5.72
_exptl_absorpt_coefficient_mu    2.855
_exptl_absorpt_correction_T_max  0.7128
_exptl_absorpt_correction_T_min  0.5292
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Stoe X-Red, X-Shape'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.074
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.043(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0538
_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/[σ²(Fo²)+(0.0671P)²+49.5255P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                2083
_reflns_number_total             2175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800357z-file001_1.cif
_cod_data_source_block           compound3
_cod_database_code               4305369
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x, -y, -z'
'-y, -x, z'
'-x, y, -z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+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
Hg Hg 0.5000 0.5000 0.5000 0.0291(3) Uani 1 8 d S . .
Sn Sn 0.38623(5) 0.38623(5) 0.43775(5) 0.0391(3) Uani 1 2 d S . .
B2 B 0.3817(8) 0.2928(7) 0.3468(5) 0.034(2) Uani 1 1 d . . .
H1 H 0.4441 0.2980 0.3184 0.041 Uiso 1 1 calc R . .
B3 B 0.3754(7) 0.2321(7) 0.4273(5) 0.033(2) Uani 1 1 d . . .
H3 H 0.4338 0.1993 0.4499 0.039 Uiso 1 1 calc R . .
B4 B 0.2822(7) 0.2822(7) 0.4751(6) 0.024(3) Uani 1 2 d S . .
H5 H 0.2815 0.2815 0.5291 0.029 Uiso 1 2 calc SR . .
B7 B 0.2652(7) 0.1830(7) 0.4313(6) 0.032(2) Uani 1 1 d . . .
H6 H 0.2549 0.1196 0.4577 0.039 Uiso 1 1 calc R . .
B6 B 0.3239(8) 0.1885(7) 0.3545(5) 0.034(2) Uani 1 1 d . . .
H7 H 0.3515 0.1279 0.3314 0.041 Uiso 1 1 calc R . .
B5 B 0.2772(8) 0.2772(8) 0.3073(7) 0.033(3) Uani 1 2 d S . .
H8 H 0.2751 0.2751 0.2534 0.040 Uiso 1 2 calc SR . .
B8 B 0.2077(8) 0.2077(8) 0.3559(8) 0.037(4) Uani 1 2 d S . .
H10 H 0.1605 0.1605 0.3330 0.044 Uiso 1 2 calc SR . .
N1 N 0.1364(7) 0.4136(7) 0.1468(5) 0.053(3) Uani 1 1 d . . .
H1A H 0.1037 0.4469 0.1756 0.064 Uiso 1 1 calc R . .
C11 C 0.1129(8) 0.3186(7) 0.1588(6) 0.048(3) Uani 1 1 d . . .
H11A H 0.0499 0.3100 0.1514 0.071 Uiso 1 1 calc R . .
H11B H 0.1271 0.3031 0.2033 0.071 Uiso 1 1 calc R . .
H11C H 0.1463 0.2810 0.1294 0.071 Uiso 1 1 calc R . .
C12 C 0.1090(11) 0.4415(9) 0.0802(5) 0.055(3) Uani 1 1 d . . .
H12A H 0.0465 0.4287 0.0740 0.083 Uiso 1 1 calc R . .
H12B H 0.1436 0.4093 0.0483 0.083 Uiso 1 1 calc R . .
H12C H 0.1190 0.5046 0.0751 0.083 Uiso 1 1 calc R . .
C13 C 0.2272(11) 0.4334(10) 0.1587(9) 0.077(5) Uani 1 1 d . . .
H13A H 0.2426 0.4156 0.2025 0.115 Uiso 1 1 calc R . .
H13B H 0.2369 0.4967 0.1538 0.115 Uiso 1 1 calc R . .
H13C H 0.2640 0.4015 0.1279 0.115 Uiso 1 1 calc R . .
Cl1 Cl 0.0000 0.5000 0.2500 0.0480(11) Uani 1 4 d S . .
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
Sn Hg Sn 124.29(4) . 3_665 ?
Sn Hg Sn 102.609(18) . 4_656 ?
Sn Hg Sn 102.609(19) 3_665 4_656 ?
Sn Hg Sn 102.609(19) . 2_566 ?
Sn Hg Sn 102.609(18) 3_665 2_566 ?
Sn Hg Sn 124.29(4) 4_656 2_566 ?
B3 Sn B3 81.5(5) 8 . ?
B3 Sn B2 47.7(4) 8 8 ?
B3 Sn B2 81.7(4) . 8 ?
B3 Sn B2 81.7(4) 8 . ?
B3 Sn B2 47.7(4) . . ?
B2 Sn B2 47.7(5) 8 . ?
B3 Sn B4 47.1(3) 8 . ?
B3 Sn B4 47.1(3) . . ?
B2 Sn B4 80.8(4) 8 . ?
B2 Sn B4 80.8(4) . . ?
B3 Sn Hg 135.0(3) 8 . ?
B3 Sn Hg 135.0(3) . . ?
B2 Sn Hg 140.1(3) 8 . ?
B2 Sn Hg 140.1(3) . . ?
B4 Sn Hg 133.0(3) . . ?
B5 B2 B6 60.0(7) . . ?
B5 B2 B3 106.9(9) . . ?
B6 B2 B3 58.6(6) . . ?
B5 B2 B2 58.0(4) . 8 ?
B6 B2 B2 105.9(5) . 8 ?
B3 B2 B2 107.8(4) . 8 ?
B5 B2 Sn 117.9(6) . . ?
B6 B2 Sn 117.9(6) . . ?
B3 B2 Sn 66.0(4) . . ?
B2 B2 Sn 66.1(3) 8 . ?
B5 B2 H1 120.9 . . ?
B6 B2 H1 121.1 . . ?
B3 B2 H1 122.6 . . ?
B2 B2 H1 123.2 8 . ?
Sn B2 H1 110.7 . . ?
B6 B3 B7 59.9(6) . . ?
B6 B3 B4 105.0(8) . . ?
B7 B3 B4 57.1(6) . . ?
B6 B3 B2 58.2(6) . . ?
B7 B3 B2 106.3(7) . . ?
B4 B3 B2 107.6(7) . . ?
B6 B3 Sn 117.8(6) . . ?
B7 B3 Sn 117.6(6) . . ?
B4 B3 Sn 66.7(5) . . ?
B2 B3 Sn 66.3(5) . . ?
B6 B3 H3 121.6 . . ?
B7 B3 H3 121.5 . . ?
B4 B3 H3 123.6 . . ?
B2 B3 H3 122.8 . . ?
Sn B3 H3 110.4 . . ?
B7 B4 B7 59.5(9) 8 . ?
B7 B4 B3 59.9(6) 8 8 ?
B7 B4 B3 107.9(8) . 8 ?
B7 B4 B3 107.9(8) 8 . ?
B7 B4 B3 59.9(6) . . ?
B3 B4 B3 109.2(9) 8 . ?
B7 B4 Sn 119.7(7) 8 . ?
B7 B4 Sn 119.7(7) . . ?
B3 B4 Sn 66.2(5) 8 . ?
B3 B4 Sn 66.2(5) . . ?
B7 B4 H5 120.1 8 . ?
B7 B4 H5 120.1 . . ?
B3 B4 H5 121.9 8 . ?
B3 B4 H5 121.9 . . ?
Sn B4 H5 109.9 . . ?
B7 B7 B4 60.2(4) 8 . ?
B7 B7 B6 108.2(5) 8 . ?
B4 B7 B6 109.7(8) . . ?
B7 B7 B8 61.2(4) 8 . ?
B4 B7 B8 109.5(8) . . ?
B6 B7 B8 58.6(6) . . ?
B7 B7 B3 111.0(5) 8 . ?
B4 B7 B3 63.0(6) . . ?
B6 B7 B3 59.8(6) . . ?
B8 B7 B3 108.4(9) . . ?
B7 B7 H6 120.6 8 . ?
B4 B7 H6 119.9 . . ?
B6 B7 H6 122.3 . . ?
B8 B7 H6 121.8 . . ?
B3 B7 H6 120.0 . . ?
B8 B6 B5 60.1(8) . . ?
B8 B6 B2 109.7(8) . . ?
B5 B6 B2 59.6(7) . . ?
B8 B6 B3 110.5(8) . . ?
B5 B6 B3 110.2(8) . . ?
B2 B6 B3 63.2(6) . . ?
B8 B6 B7 60.8(8) . . ?
B5 B6 B7 108.3(8) . . ?
B2 B6 B7 110.5(7) . . ?
B3 B6 B7 60.2(6) . . ?
B8 B6 H7 120.7 . . ?
B5 B6 H7 121.9 . . ?
B2 B6 H7 119.9 . . ?
B3 B6 H7 119.5 . . ?
B7 B6 H7 121.2 . . ?
B2 B5 B2 64.0(9) . 8 ?
B2 B5 B8 109.7(9) . . ?
B2 B5 B8 109.7(9) 8 . ?
B2 B5 B6 60.4(6) . . ?
B2 B5 B6 111.0(9) 8 . ?
B8 B5 B6 59.4(6) . . ?
B2 B5 B6 111.0(9) . 8 ?
B2 B5 B6 60.4(6) 8 8 ?
B8 B5 B6 59.4(6) . 8 ?
B6 B5 B6 106.9(11) . 8 ?
B2 B5 H8 118.9 . . ?
B2 B5 H8 118.9 8 . ?
B8 B5 H8 121.7 . . ?
B6 B5 H8 122.0 . . ?
B6 B5 H8 122.0 8 . ?
B6 B8 B6 108.7(12) . 8 ?
B6 B8 B5 60.5(7) . . ?
B6 B8 B5 60.5(7) 8 . ?
B6 B8 B7 60.7(6) . . ?
B6 B8 B7 107.1(10) 8 . ?
B5 B8 B7 108.5(10) . . ?
B6 B8 B7 107.1(10) . 8 ?
B6 B8 B7 60.7(6) 8 8 ?
B5 B8 B7 108.5(10) . 8 ?
B7 B8 B7 57.7(8) . 8 ?
B6 B8 H10 121.4 . . ?
B6 B8 H10 121.4 8 . ?
B5 B8 H10 120.9 . . ?
B7 B8 H10 122.5 . . ?
B7 B8 H10 122.5 8 . ?
C13 N1 C12 111.5(11) . . ?
C13 N1 C11 113.6(11) . . ?
C12 N1 C11 110.8(9) . . ?
C13 N1 H1A 106.8 . . ?
C12 N1 H1A 106.8 . . ?
C11 N1 H1A 106.8 . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
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
Hg Sn 2.7157(10) . ?
Hg Sn 2.7157(10) 3_665 ?
Hg Sn 2.7157(10) 4_656 ?
Hg Sn 2.7157(10) 2_566 ?
Sn B3 2.315(11) 8 ?
Sn B3 2.315(11) . ?
Sn B2 2.320(10) 8 ?
Sn B2 2.320(10) . ?
Sn B4 2.324(14) . ?
B2 B5 1.770(17) . ?
B2 B6 1.785(17) . ?
B2 B3 1.876(15) . ?
B2 B2 1.88(2) 8 ?
B2 H1 1.1000 . ?
B3 B6 1.795(15) . ?
B3 B7 1.802(16) . ?
B3 B4 1.855(13) . ?
B3 H3 1.1000 . ?
B4 B7 1.747(16) 8 ?
B4 B7 1.747(16) . ?
B4 B3 1.855(13) 8 ?
B4 H5 1.1000 . ?
B7 B7 1.73(2) 8 ?
B7 B6 1.796(16) . ?
B7 B8 1.798(18) . ?
B7 H6 1.1000 . ?
B6 B8 1.758(15) . ?
B6 B5 1.778(15) . ?
B6 H7 1.1000 . ?
B5 B2 1.770(17) 8 ?
B5 B8 1.77(3) . ?
B5 B6 1.778(15) 8 ?
B5 H8 1.1000 . ?
B8 B6 1.758(15) 8 ?
B8 B7 1.798(18) 8 ?
B8 H10 1.1000 . ?
N1 C13 1.408(17) . ?
N1 C12 1.477(14) . ?
N1 C11 1.481(13) . ?
N1 H1A 0.9100 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
