#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:50:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179992 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/86/7028633.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_7028633
loop_
_publ_author_name
'Rong, Yi'
'Palmer, Joshua H.'
'Parkin, Gerard'
_publ_section_title
;
 Benzannulated tris(2-mercapto-1-imidazolyl)hydroborato ligands:
 tetradentate κ4-S3H binding and access to monomeric monovalent thallium
 in an [S3] coordination environment.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1397
_journal_page_last               1407
_journal_paper_doi               10.1039/c3dt52418c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C36 H46 B K N6 O4 S3'
_chemical_formula_weight         772.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            12
_cell_length_a                   15.7585(12)
_cell_length_b                   15.7585(12)
_cell_length_c                   52.744(4)
_cell_measurement_reflns_used    9646
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.32
_cell_volume                     11343.1(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            56765
_diffrn_reflns_theta_full        30.61
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.7848
_exptl_absorpt_correction_T_min  0.7531
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4896
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.78
_exptl_crystal_size_min          0.72
_platon_squeeze_details
; 
The unit cell contains twelve acetone molecules which have been treated as a diffuse contribution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON. 
;
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         7721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0440
_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)+(0.0689P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1237
_reflns_number_gt                5441
_reflns_number_total             7721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52418c.txt
_cod_data_source_block           tmks10(jhp-2-97-b)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7028633
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
B1 B -0.6667 -0.3333 -0.00154(5) 0.0170(5) Uani 1 3 d S
H1 H -0.6667 -0.3333 0.0198(5) 0.020 Uiso 1 3 d S
B2 B 0.0000 0.0000 0.17461(5) 0.0168(5) Uani 1 3 d S
H2 H 0.0000 0.0000 0.1535(5) 0.020 Uiso 1 3 d S
K1 K -0.6667 -0.3333 0.065166(11) 0.02788(14) Uani 1 3 d S
K2 K 0.0000 0.0000 0.107253(10) 0.02601(13) Uani 1 3 d S
N11 N -0.58404(9) -0.23120(9) -0.01026(2) 0.0162(2) Uani 1 1 d .
N12 N -0.44748(9) -0.08836(9) -0.00648(2) 0.0187(2) Uani 1 1 d .
N21 N -0.01884(9) 0.08330(9) 0.18312(2) 0.0170(2) Uani 1 1 d .
N22 N -0.03286(9) 0.21515(9) 0.17724(2) 0.0202(3) Uani 1 1 d .
O1 O -0.60263(11) -0.41507(11) 0.09922(3) 0.0462(4) Uani 1 1 d .
O2 O -0.12276(10) -0.11704(10) 0.06894(2) 0.0368(3) Uani 1 1 d .
S1 S -0.46233(3) -0.22180(3) 0.028051(7) 0.02197(10) Uani 1 1 d .
S2 S 0.08563(3) 0.20023(3) 0.142969(7) 0.02410(10) Uani 1 1 d .
C11 C -0.49958(10) -0.18060(10) 0.00330(3) 0.0175(3) Uani 1 1 d .
C12 C -0.58493(11) -0.16906(10) -0.02899(3) 0.0176(3) Uani 1 1 d .
C13 C -0.49915(11) -0.07847(11) -0.02651(3) 0.0184(3) Uani 1 1 d .
C14 C -0.47786(12) 0.00154(11) -0.04167(3) 0.0231(3) Uani 1 1 d .
H14A H -0.4197 0.0629 -0.0395 0.028 Uiso 1 1 calc R
C15 C -0.54625(13) -0.01282(12) -0.06031(3) 0.0257(3) Uani 1 1 d .
H15A H -0.5354 0.0403 -0.0709 0.031 Uiso 1 1 calc R
C16 C -0.63038(12) -0.10370(12) -0.06368(3) 0.0248(3) Uani 1 1 d .
H16A H -0.6746 -0.1114 -0.0769 0.030 Uiso 1 1 calc R
C17 C -0.65149(11) -0.18348(11) -0.04824(3) 0.0213(3) Uani 1 1 d .
H17A H -0.7089 -0.2453 -0.0507 0.026 Uiso 1 1 calc R
C18 C -0.35156(11) -0.01279(11) 0.00207(3) 0.0250(3) Uani 1 1 d .
H18A H -0.3462 -0.0187 0.0204 0.037 Uiso 1 1 calc R
H18B H -0.3429 0.0518 -0.0019 0.037 Uiso 1 1 calc R
H18C H -0.3008 -0.0205 -0.0066 0.037 Uiso 1 1 calc R
C21 C 0.01016(11) 0.16435(11) 0.16823(3) 0.0188(3) Uani 1 1 d .
C22 C -0.08050(11) 0.08444(11) 0.20204(3) 0.0180(3) Uani 1 1 d .
C23 C -0.08987(11) 0.16680(11) 0.19825(3) 0.0195(3) Uani 1 1 d .
C24 C -0.14819(12) 0.18868(12) 0.21338(3) 0.0251(3) Uani 1 1 d .
H24A H -0.1544 0.2447 0.2104 0.030 Uiso 1 1 calc R
C25 C -0.19719(12) 0.12438(13) 0.23322(3) 0.0283(3) Uani 1 1 d .
H25A H -0.2388 0.1360 0.2439 0.034 Uiso 1 1 calc R
C26 C -0.18619(12) 0.04339(12) 0.23760(3) 0.0268(3) Uani 1 1 d .
H26A H -0.2195 0.0017 0.2515 0.032 Uiso 1 1 calc R
C27 C -0.12803(12) 0.02150(11) 0.22222(3) 0.0227(3) Uani 1 1 d .
H27A H -0.1210 -0.0341 0.2254 0.027 Uiso 1 1 calc R
C28 C -0.02025(14) 0.30533(12) 0.16646(3) 0.0289(4) Uani 1 1 d .
H28A H -0.0285 0.2983 0.1480 0.043 Uiso 1 1 calc R
H28B H 0.0456 0.3593 0.1704 0.043 Uiso 1 1 calc R
H28C H -0.0693 0.3194 0.1736 0.043 Uiso 1 1 calc R
C110 C -0.51930(19) -0.4654(2) 0.12678(5) 0.0626(7) Uani 1 1 d .
H11A H -0.5754 -0.5311 0.1239 0.094 Uiso 1 1 calc R
H11B H -0.5188 -0.4464 0.1445 0.094 Uiso 1 1 calc R
H11C H -0.4585 -0.4657 0.1231 0.094 Uiso 1 1 calc R
C111 C -0.52718(16) -0.39331(16) 0.10959(4) 0.0431(5) Uani 1 1 d .
C112 C -0.43615(18) -0.29900(19) 0.10422(6) 0.0636(7) Uani 1 1 d .
H11D H -0.4516 -0.2588 0.0931 0.095 Uiso 1 1 calc R
H11E H -0.3883 -0.3122 0.0959 0.095 Uiso 1 1 calc R
H11F H -0.4086 -0.2640 0.1202 0.095 Uiso 1 1 calc R
C210 C -0.17340(15) -0.07989(17) 0.03023(3) 0.0407(5) Uani 1 1 d .
H21A H -0.2390 -0.1255 0.0237 0.061 Uiso 1 1 calc R
H21B H -0.1259 -0.0955 0.0227 0.061 Uiso 1 1 calc R
H21C H -0.1557 -0.0127 0.0257 0.061 Uiso 1 1 calc R
C211 C -0.17269(12) -0.08906(12) 0.05850(3) 0.0276(3) Uani 1 1 d .
C212 C -0.23673(14) -0.06092(16) 0.07281(3) 0.0390(4) Uani 1 1 d .
H21D H -0.3028 -0.0948 0.0656 0.059 Uiso 1 1 calc R
H21E H -0.2097 0.0101 0.0716 0.059 Uiso 1 1 calc R
H21F H -0.2396 -0.0796 0.0907 0.059 Uiso 1 1 calc R
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
K K 0.2009 0.2494 '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'
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
H1 B1 N11 107.27(11) . 2_455
H1 B1 N11 107.27(11) . .
N11 B1 N11 111.58(10) 2_455 .
H1 B1 N11 107.27(11) . 3_445
N11 B1 N11 111.58(10) 2_455 3_445
N11 B1 N11 111.58(10) . 3_445
H2 B2 N21 106.84(10) . .
H2 B2 N21 106.84(10) . 3
N21 B2 N21 111.97(9) . 3
H2 B2 N21 106.84(10) . 2
N21 B2 N21 111.97(9) . 2
N21 B2 N21 111.97(9) 3 2
H1 K1 O1 132.01(3) . 3_445
H1 K1 O1 132.01(3) . 2_455
O1 K1 O1 80.10(5) 3_445 2_455
H1 K1 O1 132.01(3) . .
O1 K1 O1 80.11(5) 3_445 .
O1 K1 O1 80.11(5) 2_455 .
H1 K1 S1 54.972(10) . 2_455
O1 K1 S1 91.01(3) 3_445 2_455
O1 K1 S1 98.44(3) 2_455 2_455
O1 K1 S1 171.12(4) . 2_455
H1 K1 S1 54.972(10) . 3_445
O1 K1 S1 98.44(3) 3_445 3_445
O1 K1 S1 171.12(4) 2_455 3_445
O1 K1 S1 91.01(3) . 3_445
S1 K1 S1 90.334(14) 2_455 3_445
H1 K1 S1 54.969(10) . .
O1 K1 S1 171.12(4) 3_445 .
O1 K1 S1 91.01(3) 2_455 .
O1 K1 S1 98.44(3) . .
S1 K1 S1 90.332(14) 2_455 .
S1 K1 S1 90.333(14) 3_445 .
H2 K2 O2 136.90(3) . .
H2 K2 O2 136.90(3) . 2
O2 K2 O2 72.56(5) . 2
H2 K2 O2 136.90(3) . 3
O2 K2 O2 72.56(5) . 3
O2 K2 O2 72.56(5) 2 3
H2 K2 S2 55.514(10) . 3
O2 K2 S2 118.91(3) . 3
O2 K2 S2 83.94(3) 2 3
O2 K2 S2 149.59(3) 3 3
H2 K2 S2 55.514(10) . 2
O2 K2 S2 83.94(3) . 2
O2 K2 S2 149.59(3) 2 2
O2 K2 S2 118.91(3) 3 2
S2 K2 S2 91.096(15) 3 2
H2 K2 S2 55.512(10) . .
O2 K2 S2 149.59(3) . .
O2 K2 S2 118.91(3) 2 .
O2 K2 S2 83.94(3) 3 .
S2 K2 S2 91.094(15) 3 .
S2 K2 S2 91.094(15) 2 .
C11 N11 C12 108.08(12) . .
C11 N11 B1 121.30(13) . .
C12 N11 B1 129.84(12) . .
C11 N12 C13 109.44(12) . .
C11 N12 C18 125.60(12) . .
C13 N12 C18 124.93(12) . .
C21 N21 C22 107.89(12) . .
C21 N21 B2 120.54(13) . .
C22 N21 B2 130.23(12) . .
C21 N22 C23 109.28(12) . .
C21 N22 C28 124.95(13) . .
C23 N22 C28 125.77(13) . .
C111 O1 K1 136.80(15) . .
C211 O2 K2 117.05(11) . .
C11 S1 K1 102.81(5) . .
C21 S2 K2 104.25(5) . .
N12 C11 N11 108.46(12) . .
N12 C11 S1 124.22(11) . .
N11 C11 S1 127.32(11) . .
C17 C12 N11 132.18(14) . .
C17 C12 C13 119.95(13) . .
N11 C12 C13 107.85(12) . .
C14 C13 N12 130.72(14) . .
C14 C13 C12 123.10(14) . .
N12 C13 C12 106.16(12) . .
C13 C14 C15 116.40(14) . .
C14 C15 C16 121.27(14) . .
C17 C16 C15 121.92(14) . .
C16 C17 C12 117.28(14) . .
N22 C21 N21 108.36(12) . .
N22 C21 S2 123.51(11) . .
N21 C21 S2 128.12(11) . .
C27 C22 C23 120.29(14) . .
C27 C22 N21 131.79(14) . .
C23 C22 N21 107.92(12) . .
C24 C23 N22 130.59(14) . .
C24 C23 C22 122.85(14) . .
N22 C23 C22 106.55(12) . .
C23 C24 C25 116.60(15) . .
C24 C25 C26 120.98(15) . .
C27 C26 C25 122.09(15) . .
C22 C27 C26 117.14(15) . .
O1 C111 C112 121.6(2) . .
O1 C111 C110 120.4(2) . .
C112 C111 C110 117.78(19) . .
O2 C211 C212 122.47(16) . .
O2 C211 C210 121.71(17) . .
C212 C211 C210 115.81(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
B1 H1 1.12(3) .
B1 N11 1.5498(14) 2_455
B1 N11 1.5498(14) .
B1 N11 1.5498(14) 3_445
B2 H2 1.12(3) .
B2 N21 1.5500(14) .
B2 N21 1.5500(14) 3
B2 N21 1.5500(14) 2
K1 H1 2.39(3) .
K1 O1 2.6839(14) 3_445
K1 O1 2.6839(14) 2_455
K1 O1 2.6838(14) .
K1 S1 3.4103(5) 2_455
K1 S1 3.4103(5) 3_445
K1 S1 3.4103(5) .
K2 H2 2.44(3) .
K2 O2 2.7675(13) .
K2 O2 2.7676(13) 2
K2 O2 2.7676(13) 3
K2 S2 3.3268(5) 3
K2 S2 3.3268(5) 2
K2 S2 3.3269(5) .
N11 C11 1.3628(18) .
N11 C12 1.3958(17) .
N12 C11 1.3635(18) .
N12 C13 1.3893(18) .
N12 C18 1.4514(19) .
N21 C21 1.3687(18) .
N21 C22 1.3993(17) .
N22 C21 1.3670(19) .
N22 C23 1.3897(19) .
N22 C28 1.4493(19) .
O1 C111 1.193(2) .
O2 C211 1.210(2) .
S1 C11 1.6888(15) .
S2 C21 1.6844(15) .
C12 C17 1.394(2) .
C12 C13 1.397(2) .
C13 C14 1.385(2) .
C14 C15 1.391(2) .
C15 C16 1.393(2) .
C16 C17 1.392(2) .
C22 C27 1.391(2) .
C22 C23 1.392(2) .
C23 C24 1.385(2) .
C24 C25 1.391(2) .
C25 C26 1.391(2) .
C26 C27 1.390(2) .
C110 C111 1.507(3) .
C111 C112 1.488(3) .
C210 C211 1.499(2) .
C211 C212 1.494(3) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.016 0.490 0.370 21 0 ' '
2 0.000 0.000 0.500 119 12 ' '
3 0.016 0.510 0.630 21 0 ' '
4 0.156 0.839 0.963 21 0 ' '
5 0.172 0.349 0.703 21 0 ' '
6 0.161 0.317 0.963 21 0 ' '
7 0.177 0.828 0.703 21 0 ' '
8 0.333 0.667 0.167 115 12 ' '
9 0.317 0.156 0.037 21 0 ' '
10 0.349 0.177 0.297 21 0 ' '
11 0.490 0.506 0.630 21 0 ' '
12 0.506 0.016 0.370 21 0 ' '
13 0.494 0.984 0.630 21 0 ' '
14 0.510 0.494 0.370 21 0 ' '
15 0.667 0.333 0.833 115 12 ' '
16 0.651 0.823 0.703 21 0 ' '
17 0.682 0.843 0.963 21 0 ' '
18 0.823 0.172 0.297 21 0 ' '
19 0.839 0.682 0.037 21 0 ' '
20 0.828 0.651 0.297 21 0 ' '
21 0.843 0.161 0.037 21 0 ' '
