#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/90/7009035.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_7009035
loop_
_publ_author_name
'Slavin, Paul A.'
'Reglinski, John'
'Spicer, Mark D.'
'Kennedy, Alan R.'
_publ_section_title
;
 Preparation and crystal structure of the
 [bis{hydrotris(methimazolyl)borato}thallium(III)] cation: modulated
 chemistry resulting from the use of soft and hard tripodal ligands
;
_journal_issue                   3
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              239
_journal_paper_doi               10.1039/a908236k
_journal_year                    2000
_chemical_formula_sum            'C12 H16 B I2 N6 S3 Tl'
_chemical_formula_weight         809.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Tue Aug  3 13:43:22 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                87.41(2)
_cell_angle_beta                 88.53(1)
_cell_angle_gamma                86.64(1)
_cell_formula_units_Z            2
_cell_length_a                   10.468(2)
_cell_length_b                   10.543(2)
_cell_length_c                   10.620(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203.2
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      24.3
_cell_volume                     1168.5(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  'SHELXL-93, (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993) '
_computing_structure_solution    'SHELXS (Sheldrick, 1986)'
_diffrn_ambient_temperature      203.2
_diffrn_measurement_device       AFC7S
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.09450
_diffrn_orient_matrix_UB_12      -0.01234
_diffrn_orient_matrix_UB_13      0.01145
_diffrn_orient_matrix_UB_21      0.01179
_diffrn_orient_matrix_UB_22      0.08604
_diffrn_orient_matrix_UB_23      -0.04070
_diffrn_orient_matrix_UB_31      -0.00961
_diffrn_orient_matrix_UB_32      0.03858
_diffrn_orient_matrix_UB_33      0.08427
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  1.97
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5392
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        -5.64
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.819
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.300
_exptl_crystal_density_meas      0.000
_exptl_crystal_description       plate
_exptl_crystal_F_000             740.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.150
_refine_diff_density_max         4.224
_refine_diff_density_min         -1.764
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     250
_refine_ls_number_reflns         5107
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_obs          0.0.0542
_refine_ls_shift/esd_max         0.016
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0522P)²+8.0539P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1410
_refine_ls_wR_factor_obs         0.1328
_reflns_number_observed          4212
_reflns_number_total             5107
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908236k.txt
_cod_data_source_block           '[Tl(Tm)2]+[TlI4]-'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+8.0539P] 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^)+(0.0522P)^2^+8.0539P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1168.6(4)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C12 H16 B I2 N6 S3 Tl '
_cod_database_code               7009035
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Tl1 Tl 0.0000 0.0000 0.0000 0.0420(2) Uani 1 d S .
Tl2 Tl 0.4598(3) 0.4136(3) 0.4166(3) 0.1357(11) Uani 0.50 d P .
I1 I 0.55285(15) 0.5668(2) 0.58374(14) 0.0290(3) Uani 0.50 d P .
I2 I 0.53777(12) 0.18273(12) 0.45049(12) 0.0476(3) Uani 0.50 d P .
I3 I 0.53401(15) 0.50675(14) 0.1789(2) 0.0718(5) Uani 0.50 d P .
I4 I 0.18436(11) 0.43331(12) 0.45840(12) 0.0495(3) Uani 0.50 d P .
S1 S 0.2083(2) -0.1308(3) -0.0844(2) 0.0589(7) Uani 1 d . .
S2 S -0.0879(2) -0.2024(3) 0.1289(2) 0.0511(6) Uani 1 d . .
S3 S 0.1212(2) 0.0760(3) 0.2000(2) 0.0488(5) Uani 1 d . .
N1 N 0.2014(7) -0.3167(9) 0.1081(8) 0.054(2) Uani 1 d . .
N2 N 0.1603(9) -0.3826(12) -0.0761(10) 0.074(3) Uani 1 d . .
N3 N 0.1029(7) -0.2135(8) 0.3060(7) 0.045(2) Uani 1 d . .
N4 N -0.0866(8) -0.1540(10) 0.3773(8) 0.066(3) Uani 1 d . .
N5 N 0.3056(7) -0.1258(9) 0.2004(7) 0.051(2) Uani 1 d . .
N6 N 0.3779(8) 0.0614(9) 0.1548(7) 0.054(2) Uani 1 d . .
C1 C 0.1880(8) -0.2767(11) -0.0140(10) 0.056(3) Uani 1 d . .
C2 C 0.1807(10) -0.4454(11) 0.1195(12) 0.064(3) Uani 1 d . .
C3 C 0.1524(12) -0.4839(13) 0.0030(13) 0.073(3) Uani 1 d . .
C4 C 0.1344(14) -0.3792(17) -0.2132(12) 0.094(5) Uani 1 d . .
C5 C -0.0205(9) -0.1900(10) 0.2726(8) 0.049(2) Uani 1 d . .
C6 C 0.1095(11) -0.1930(12) 0.4347(9) 0.061(3) Uani 1 d . .
C7 C -0.0050(12) -0.1554(14) 0.4781(9) 0.075(4) Uani 1 d . .
C8 C -0.2246(12) -0.1164(18) 0.3821(12) 0.096(5) Uani 1 d . .
C9 C 0.2685(9) -0.0014(10) 0.1850(8) 0.046(2) Uani 1 d . .
C10 C 0.4381(9) -0.1411(12) 0.1823(10) 0.058(3) Uani 1 d . .
C11 C 0.4806(9) -0.0261(13) 0.1529(10) 0.062(3) Uani 1 d . .
C12 C 0.3809(11) 0.1949(12) 0.1275(12) 0.067(3) Uani 1 d . .
B1 B 0.2272(10) -0.2439(12) 0.2275(11) 0.049(2) Uani 1 d . .
H1 H 0.2923 -0.2912 0.2798 0.080 Uiso 1 d . .
H2 H 0.1919 -0.4964 0.1957 0.083 Uiso 1 d . .
H3 H 0.1215 -0.5782 -0.0185 0.100 Uiso 1 d . .
H4 H 0.1480 -0.3000 -0.2453 0.133 Uiso 1 d . .
H5 H 0.1889 -0.4435 -0.2514 0.133 Uiso 1 d . .
H6 H 0.0470 -0.4012 -0.2235 0.133 Uiso 1 d . .
H7 H 0.1874 -0.1986 0.4874 0.086 Uiso 1 d . .
H8 H -0.0274 -0.1315 0.5627 0.095 Uiso 1 d . .
H9 H -0.2532 -0.0959 0.4600 0.111 Uiso 1 d . .
H10 H -0.2405 -0.0453 0.3211 0.111 Uiso 1 d . .
H11 H -0.2714 -0.1857 0.3510 0.111 Uiso 1 d . .
H12 H 0.4876 -0.2164 0.1910 0.076 Uiso 1 d . .
H13 H 0.5700 -0.0066 0.1209 0.078 Uiso 1 d . .
H14 H 0.4665 0.2221 0.0999 0.094 Uiso 1 d . .
H15 H 0.3296 0.2212 0.0474 0.094 Uiso 1 d . .
H16 H 0.3483 0.2488 0.1878 0.094 Uiso 1 d . .
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 24 0.003 0.002 'International Tables'
H 0 32 0.000 0.000 'International Tables'
B 0 2 0.001 0.001 'International Tables'
I 0 4 -0.474 1.812 'International Tables'
N 0 12 0.006 0.003 'International Tables'
S 0 6 0.125 0.123 'International Tables'
Tl 0 2 -2.836 9.669 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?
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_2
_geom_angle_site_symmetry_3
S1 Tl1 S1 180.0 . 2 ?
S1 Tl1 S2 86.87(9) . 2 ?
S1 Tl1 S2 93.13(9) 2 2 ?
S1 Tl1 S2 93.13(9) . . ?
S1 Tl1 S2 86.87(9) 2 . ?
S2 Tl1 S2 180.0 2 . ?
S1 Tl1 S3 92.53(7) . . ?
S1 Tl1 S3 87.47(7) 2 . ?
S2 Tl1 S3 87.35(8) 2 . ?
S2 Tl1 S3 92.65(8) . . ?
S1 Tl1 S3 87.47(7) . 2 ?
S1 Tl1 S3 92.53(7) 2 2 ?
S2 Tl1 S3 92.65(8) 2 2 ?
S2 Tl1 S3 87.35(8) . 2 ?
S3 Tl1 S3 180.0 . 2 ?
I2 Tl2 I1 113.17(10) . . ?
I2 Tl2 I3 110.64(11) . . ?
I1 Tl2 I3 106.67(9) . . ?
I2 Tl2 I4 108.54(11) . . ?
I1 Tl2 I4 104.97(9) . . ?
I3 Tl2 I4 112.77(11) . . ?
C1 S1 Tl1 101.1(3) . . ?
C5 S2 Tl1 101.5(3) . . ?
C9 S3 Tl1 102.2(3) . . ?
C1 N1 C2 108.8(9) . . ?
C1 N1 B1 131.6(9) . . ?
C2 N1 B1 119.5(9) . . ?
C3 N2 C1 111.5(10) . . ?
C3 N2 C4 125.6(11) . . ?
C1 N2 C4 122.8(13) . . ?
C5 N3 C6 107.5(8) . . ?
C5 N3 B1 132.1(8) . . ?
C6 N3 B1 120.0(8) . . ?
C5 N4 C7 109.9(9) . . ?
C5 N4 C8 124.8(10) . . ?
C7 N4 C8 125.3(10) . . ?
C9 N5 C10 109.3(9) . . ?
C9 N5 B1 131.1(8) . . ?
C10 N5 B1 119.5(9) . . ?
C11 N6 C9 108.8(9) . . ?
C11 N6 C12 126.6(9) . . ?
C9 N6 C12 124.7(9) . . ?
N1 C1 N2 105.4(11) . . ?
N1 C1 S1 129.7(7) . . ?
N2 C1 S1 124.8(9) . . ?
C3 C2 N1 107.7(12) . . ?
N2 C3 C2 106.6(11) . . ?
N4 C5 N3 106.9(8) . . ?
N4 C5 S2 124.0(8) . . ?
N3 C5 S2 129.1(7) . . ?
C7 C6 N3 109.2(9) . . ?
C6 C7 N4 106.5(9) . . ?
N5 C9 N6 106.4(8) . . ?
N5 C9 S3 131.0(7) . . ?
N6 C9 S3 122.6(8) . . ?
C11 C10 N5 107.2(10) . . ?
C10 C11 N6 108.4(9) . . ?
N5 B1 N1 113.6(8) . . ?
N5 B1 N3 112.5(8) . . ?
N1 B1 N3 112.2(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Tl1 S1 2.668(3) . ?
Tl1 S1 2.668(3) 2 ?
Tl1 S2 2.679(3) 2 ?
Tl1 S2 2.679(3) . ?
Tl1 S3 2.679(2) . ?
Tl1 S3 2.679(2) 2 ?
Tl2 I2 2.534(3) . ?
Tl2 I1 2.690(2) . ?
Tl2 I3 2.776(3) . ?
Tl2 I4 2.903(3) . ?
S1 C1 1.702(13) . ?
S2 C5 1.711(10) . ?
S3 C9 1.709(10) . ?
N1 C1 1.354(14) . ?
N1 C2 1.385(14) . ?
N1 B1 1.550(13) . ?
N2 C3 1.33(2) . ?
N2 C1 1.371(13) . ?
N2 C4 1.49(2) . ?
N3 C5 1.354(12) . ?
N3 C6 1.398(11) . ?
N3 B1 1.553(13) . ?
N4 C5 1.351(12) . ?
N4 C7 1.386(14) . ?
N4 C8 1.476(14) . ?
N5 C9 1.349(13) . ?
N5 C10 1.397(12) . ?
N5 B1 1.543(15) . ?
N6 C11 1.375(14) . ?
N6 C9 1.379(12) . ?
N6 C12 1.427(15) . ?
C2 C3 1.36(2) . ?
C6 C7 1.32(2) . ?
C10 C11 1.34(2) . ?
