#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:34:00 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179796 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/92/7009234.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_7009234
loop_
_publ_author_name
'Kimblin, Clare'
'Bridgewater, Brian M.'
'Hascall, Tony'
'Parkin, Gerard'
_publ_section_title
;
 The synthesis and structural characterization of
 bis(mercaptoimidazolyl)(pyrazolyl)hydroborato and
 tris(mercaptoimidazolyl)hydroborato complexes of thallium(I) and
 thallium(III)
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1267
_journal_paper_doi               10.1039/a909542j
_journal_year                    2000
_chemical_formula_sum            'C55 H45 B2 Cl3 N12 S6 Tl2'
_chemical_formula_weight         1603.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.389(2)
_cell_angle_beta                 95.630(2)
_cell_angle_gamma                100.605(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3343(9)
_cell_length_b                   10.6394(10)
_cell_length_c                   14.8014(14)
_cell_measurement_temperature    243(2)
_cell_volume                     1539.2(2)
_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      243(2)
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.887
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11080
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    5.609
_exptl_absorpt_correction_T_max  0.6039
_exptl_absorpt_correction_T_min  0.4000
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00000(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         6814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          2.345
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0156P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                4612
_reflns_number_total             6814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909542j.txt
_cod_data_source_block           tls10-2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009234
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Tl Tl 1.63305(2) 0.87722(2) 0.506828(16) 0.05147(10) Uani 1 1 d . . .
S1 S 1.73748(12) 0.97639(13) 0.74221(9) 0.0514(4) Uani 1 1 d . . .
S2 S 1.40817(12) 1.30868(11) 0.69964(9) 0.0439(3) Uani 1 1 d . . .
S3 S 1.33014(14) 0.82194(12) 0.48805(9) 0.0523(3) Uani 1 1 d . . .
N11 N 1.5182(3) 1.0596(3) 0.7996(2) 0.0335(9) Uani 1 1 d . . .
N12 N 1.6910(4) 1.1183(4) 0.9100(3) 0.0419(10) Uani 1 1 d . . .
N21 N 1.3014(3) 1.0577(3) 0.7070(2) 0.0325(9) Uani 1 1 d . . .
N22 N 1.1611(3) 1.1883(3) 0.7251(3) 0.0340(9) Uani 1 1 d . . .
N31 N 1.3970(3) 0.8547(3) 0.6766(3) 0.0320(8) Uani 1 1 d . . .
N32 N 1.3281(3) 0.6484(3) 0.5976(3) 0.0376(9) Uani 1 1 d . . .
Cl1 Cl 2.4204(3) 1.3740(3) 1.1204(3) 0.0870(10) Uani 0.50 1 d P A -1
Cl2 Cl 2.2640(3) 1.5501(3) 1.0677(2) 0.0782(9) Uani 0.50 1 d P A -1
Cl3 Cl 2.5024(18) 1.5133(17) 0.9842(8) 0.095(2) Uani 0.50 1 d P A -1
C1 C 2.4240(10) 1.5218(10) 1.0871(8) 0.059(3) Uani 0.50 1 d P A -1
H1A H 2.4778 1.5956 1.1382 0.071 Uiso 0.50 1 calc PR A -1
C11 C 1.6489(4) 1.0550(4) 0.8184(3) 0.0334(11) Uani 1 1 d . . .
C12 C 1.4809(5) 1.1245(5) 0.8819(4) 0.0477(13) Uani 1 1 d . . .
H12A H 1.3959 1.1415 0.8890 0.057 Uiso 1 1 calc R . .
C13 C 1.5853(5) 1.1588(5) 0.9493(4) 0.0529(14) Uani 1 1 d . . .
H13A H 1.5866 1.2027 1.0124 0.063 Uiso 1 1 calc R . .
C21 C 1.2894(4) 1.1841(4) 0.7117(3) 0.0331(10) Uani 1 1 d . . .
C22 C 1.1820(4) 0.9851(4) 0.7163(3) 0.0417(12) Uani 1 1 d . . .
H22A H 1.1639 0.8948 0.7152 0.050 Uiso 1 1 calc R . .
C23 C 1.0954(4) 1.0647(4) 0.7273(3) 0.0461(13) Uani 1 1 d . . .
H23A H 1.0058 1.0405 0.7350 0.055 Uiso 1 1 calc R . .
C31 C 1.3530(4) 0.7756(4) 0.5902(3) 0.0351(11) Uani 1 1 d . . .
C32 C 1.4009(5) 0.7750(5) 0.7386(4) 0.0469(13) Uani 1 1 d . . .
H32A H 1.4289 0.8050 0.8037 0.056 Uiso 1 1 calc R . .
C33 C 1.3584(5) 0.6489(4) 0.6905(3) 0.0451(12) Uani 1 1 d . . .
H33A H 1.3505 0.5746 0.7152 0.054 Uiso 1 1 calc R . .
C41 C 1.8215(5) 1.1412(4) 0.9597(3) 0.0408(12) Uani 1 1 d . . .
C42 C 1.9272(5) 1.2112(5) 0.9295(4) 0.0552(14) Uani 1 1 d . . .
H42A H 1.9140 1.2412 0.8750 0.066 Uiso 1 1 calc R . .
C43 C 2.0529(5) 1.2365(5) 0.9801(4) 0.0621(15) Uani 1 1 d . . .
H43A H 2.1257 1.2835 0.9596 0.075 Uiso 1 1 calc R . .
C44 C 2.0728(6) 1.1941(5) 1.0598(4) 0.0600(15) Uani 1 1 d . . .
H44A H 2.1588 1.2114 1.0935 0.072 Uiso 1 1 calc R . .
C45 C 1.9678(6) 1.1267(5) 1.0902(4) 0.0568(14) Uani 1 1 d . . .
H45A H 1.9813 1.0980 1.1452 0.068 Uiso 1 1 calc R . .
C46 C 1.8415(5) 1.1006(5) 1.0405(3) 0.0509(13) Uani 1 1 d . . .
H46A H 1.7690 1.0548 1.0620 0.061 Uiso 1 1 calc R . .
C51 C 1.1012(4) 1.3021(4) 0.7395(3) 0.0348(11) Uani 1 1 d . . .
C52 C 0.9776(5) 1.2886(5) 0.6894(3) 0.0454(12) Uani 1 1 d . . .
H52A H 0.9367 1.2093 0.6447 0.054 Uiso 1 1 calc R . .
C53 C 0.9148(5) 1.3942(5) 0.7065(4) 0.0578(15) Uani 1 1 d . . .
H53A H 0.8301 1.3866 0.6735 0.069 Uiso 1 1 calc R . .
C54 C 0.9761(6) 1.5106(5) 0.7717(4) 0.0610(15) Uani 1 1 d . . .
H54A H 0.9336 1.5824 0.7826 0.073 Uiso 1 1 calc R . .
C55 C 1.0993(5) 1.5213(5) 0.8205(4) 0.0536(14) Uani 1 1 d . . .
H55A H 1.1410 1.6009 0.8645 0.064 Uiso 1 1 calc R . .
C56 C 1.1624(4) 1.4169(4) 0.8057(3) 0.0420(12) Uani 1 1 d . . .
H56A H 1.2459 1.4238 0.8402 0.050 Uiso 1 1 calc R . .
C61 C 1.2711(5) 0.5315(4) 0.5237(3) 0.0387(11) Uani 1 1 d . . .
C62 C 1.1549(5) 0.4525(5) 0.5340(4) 0.0510(13) Uani 1 1 d . . .
H62A H 1.1137 0.4762 0.5874 0.061 Uiso 1 1 calc R . .
C63 C 1.0993(6) 0.3374(5) 0.4646(5) 0.0690(17) Uani 1 1 d . . .
H63A H 1.0196 0.2831 0.4708 0.083 Uiso 1 1 calc R . .
C64 C 1.1601(6) 0.3029(5) 0.3873(4) 0.0597(15) Uani 1 1 d . . .
H64A H 1.1207 0.2259 0.3399 0.072 Uiso 1 1 calc R . .
C65 C 1.2771(6) 0.3789(5) 0.3784(4) 0.0600(15) Uani 1 1 d . . .
H65A H 1.3193 0.3530 0.3258 0.072 Uiso 1 1 calc R . .
C66 C 1.3346(5) 0.4959(5) 0.4475(4) 0.0483(13) Uani 1 1 d . . .
H66A H 1.4153 0.5489 0.4418 0.058 Uiso 1 1 calc R . .
B B 1.4338(5) 1.0081(5) 0.7015(4) 0.0330(13) Uani 1 1 d . . .
H1 H 1.482(3) 1.041(3) 0.648(2) 0.023(9) Uiso 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 '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
S3 Tl H1 57.6(6) . . ?
S3 Tl S3 95.76(3) . 2_876 ?
H1 Tl S3 64.2(6) . 2_876 ?
S3 Tl S1 104.53(3) . . ?
H1 Tl S1 57.0(6) . . ?
S3 Tl S1 86.75(3) 2_876 . ?
S3 Tl B 55.14(9) . . ?
H1 Tl B 12.8(6) . . ?
S3 Tl B 76.81(7) 2_876 . ?
S1 Tl B 52.45(8) . . ?
S3 Tl S2 64.35(3) . . ?
H1 Tl S2 19.2(6) . . ?
S3 Tl S2 45.43(3) 2_876 . ?
S1 Tl S2 66.40(2) . . ?
B Tl S2 32.02(7) . . ?
C11 S1 Tl 122.40(17) . . ?
C21 S2 Tl 83.09(13) . . ?
C31 S3 Tl 84.67(14) . . ?
C31 S3 Tl 119.73(16) . 2_876 ?
Tl S3 Tl 84.24(3) . 2_876 ?
C11 N11 C12 107.7(4) . . ?
C11 N11 B 124.5(3) . . ?
C12 N11 B 127.7(4) . . ?
C11 N12 C13 108.7(4) . . ?
C11 N12 C41 127.0(3) . . ?
C13 N12 C41 124.3(4) . . ?
C21 N21 C22 109.1(3) . . ?
C21 N21 B 124.9(3) . . ?
C22 N21 B 125.7(3) . . ?
C21 N22 C23 109.0(3) . . ?
C21 N22 C51 127.4(3) . . ?
C23 N22 C51 123.5(3) . . ?
C31 N31 C32 107.8(4) . . ?
C31 N31 B 125.4(4) . . ?
C32 N31 B 126.8(4) . . ?
C31 N32 C33 108.7(4) . . ?
C31 N32 C61 127.0(4) . . ?
C33 N32 C61 124.1(4) . . ?
Cl1 C1 Cl2 110.9(6) . . ?
Cl1 C1 Cl3 108.6(7) . . ?
Cl2 C1 Cl3 111.2(8) . . ?
N12 C11 N11 107.3(3) . . ?
N12 C11 S1 127.0(3) . . ?
N11 C11 S1 125.7(3) . . ?
C13 C12 N11 108.7(4) . . ?
C12 C13 N12 107.7(4) . . ?
N21 C21 N22 106.1(3) . . ?
N21 C21 S2 126.6(3) . . ?
N22 C21 S2 127.3(3) . . ?
C23 C22 N21 108.2(4) . . ?
C22 C23 N22 107.6(4) . . ?
N31 C31 N32 107.7(4) . . ?
N31 C31 S3 127.3(3) . . ?
N32 C31 S3 124.9(4) . . ?
C33 C32 N31 108.7(4) . . ?
C32 C33 N32 107.0(4) . . ?
C46 C41 C42 119.9(5) . . ?
C46 C41 N12 120.3(4) . . ?
C42 C41 N12 119.7(4) . . ?
C41 C42 C43 119.2(5) . . ?
C44 C43 C42 120.7(5) . . ?
C45 C44 C43 119.9(5) . . ?
C44 C45 C46 120.1(5) . . ?
C41 C46 C45 120.1(5) . . ?
C56 C51 C52 121.7(4) . . ?
C56 C51 N22 120.5(4) . . ?
C52 C51 N22 117.7(4) . . ?
C51 C52 C53 118.6(5) . . ?
C54 C53 C52 120.3(5) . . ?
C55 C54 C53 119.8(4) . . ?
C54 C55 C56 120.8(5) . . ?
C55 C56 C51 118.8(4) . . ?
C66 C61 C62 121.0(5) . . ?
C66 C61 N32 120.8(4) . . ?
C62 C61 N32 118.1(4) . . ?
C61 C62 C63 119.3(5) . . ?
C64 C63 C62 120.1(5) . . ?
C65 C64 C63 120.6(5) . . ?
C64 C65 C66 120.1(5) . . ?
C61 C66 C65 118.8(5) . . ?
N11 B N31 109.1(4) . . ?
N11 B N21 107.8(3) . . ?
N31 B N21 107.2(3) . . ?
N11 B Tl 113.3(2) . . ?
N31 B Tl 72.2(2) . . ?
N21 B Tl 136.6(3) . . ?
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
Tl S3 3.0493(14) . ?
Tl H1 3.13(3) . ?
Tl S3 3.1351(12) 2_876 ?
Tl S1 3.3995(14) . ?
Tl B 3.853(5) . ?
Tl S2 5.8120(12) . ?
S1 C11 1.690(4) . ?
S2 C21 1.688(4) . ?
S3 C31 1.704(5) . ?
S3 Tl 3.1351(12) 2_876 ?
N11 C11 1.364(5) . ?
N11 C12 1.382(5) . ?
N11 B 1.541(6) . ?
N12 C11 1.355(5) . ?
N12 C13 1.378(5) . ?
N12 C41 1.421(6) . ?
N21 C21 1.360(5) . ?
N21 C22 1.368(5) . ?
N21 B 1.558(5) . ?
N22 C21 1.368(5) . ?
N22 C23 1.373(5) . ?
N22 C51 1.441(5) . ?
N31 C31 1.340(5) . ?
N31 C32 1.388(5) . ?
N31 B 1.552(6) . ?
N32 C31 1.362(5) . ?
N32 C33 1.379(5) . ?
N32 C61 1.437(5) . ?
Cl1 C1 1.748(10) . ?
Cl2 C1 1.743(10) . ?
Cl3 C1 1.786(14) . ?
C12 C13 1.330(6) . ?
C22 C23 1.337(5) . ?
C32 C33 1.334(6) . ?
C41 C46 1.372(6) . ?
C41 C42 1.378(6) . ?
C42 C43 1.382(7) . ?
C43 C44 1.368(7) . ?
C44 C45 1.361(7) . ?
C45 C46 1.381(7) . ?
C51 C56 1.375(6) . ?
C51 C52 1.378(6) . ?
C52 C53 1.384(6) . ?
C53 C54 1.380(7) . ?
C54 C55 1.372(7) . ?
C55 C56 1.374(6) . ?
C61 C66 1.374(6) . ?
C61 C62 1.376(6) . ?
C62 C63 1.388(7) . ?
C63 C64 1.367(7) . ?
C64 C65 1.362(7) . ?
C65 C66 1.403(7) . ?
