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#$Date: 2019-11-15 02:05:54 +0200 (Fri, 15 Nov 2019) $
#$Revision: 227840 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/19/7701935.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_7701935
loop_
_publ_author_name
'Yadav, Chote Lal'
'Rajput, Gunjan'
'Manar, Krishna K.'
'Kumari, Kavita'
'Drew, Michael G. B.'
'Singh, Nanhai'
_publ_section_title
;
 Cooperative metal-ligand influence on the formation of coordination
 polymers, and conducting and photophysical properties of Tl(i)
 β-oxodithioester complexes.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16264
_journal_page_last               16278
_journal_paper_doi               10.1039/c8dt03694b
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C10 H8 Br O S2 Tl'
_chemical_formula_weight         492.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_symmetry_space_group_name_Hall  'I 2 -2c'
_symmetry_space_group_name_H-M   'I b a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-08-10 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.252(5)
_cell_length_b                   11.1332(14)
_cell_length_c                   6.9522(7)
_cell_measurement_reflns_used    8051
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.66
_cell_volume                     2418.9(5)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material
'SHELXL-2016/6, PLATON, WINGX (Ferrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1151
_diffrn_reflns_av_unetI/netI     0.1549
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8051
_diffrn_reflns_point_group_measured_fraction_full 0.859
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.992
_diffrn_reflns_theta_min         3.660
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_exptl_absorpt_coefficient_mu    16.972
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.705
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.218
_refine_diff_density_min         -2.223
_refine_diff_density_rms         0.347
_refine_ls_abs_structure_details
;
 Flack x determined using 322 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2962
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0451P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.558
_reflns_Friedel_fraction_full    0.691
_reflns_Friedel_fraction_max     0.655
_reflns_number_gt                1805
_reflns_number_total             2962
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03694b2.cif
_cod_data_source_block           8
_cod_database_code               7701935
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1, -y+1, z+1/2'
'-x+1, y+1, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Tl1 Tl 0.56573(3) 0.36436(7) -0.00358(17) 0.0329(3) Uani 1 1 d . .
Br24 Br 0.83146(10) 0.6376(3) -0.0648(3) 0.0468(8) Uani 1 1 d . .
S15 S 0.5314(2) 0.6084(5) 0.0877(8) 0.0282(13) Uani 1 1 d . .
S16 S 0.5341(2) 0.8370(5) -0.0944(8) 0.0310(14) Uani 1 1 d . .
O11 O 0.6230(6) 0.5375(15) 0.161(2) 0.036(4) Uani 1 1 d . .
C12 C 0.6354(8) 0.6255(19) 0.070(3) 0.028(5) Uani 1 1 d . .
C13 C 0.6083(6) 0.7163(17) -0.010(4) 0.023(4) Uani 1 1 d . .
H13 H 0.621662 0.779593 -0.073179 0.028 Uiso 1 1 calc R U
C14 C 0.5651(6) 0.7184(13) -0.001(5) 0.018(3) Uani 1 1 d . U
C16 C 0.5710(10) 0.945(2) -0.189(4) 0.050(8) Uani 1 1 d . .
H16A H 0.588417 0.975802 -0.086242 0.075 Uiso 1 1 calc R U
H16B H 0.555436 1.009866 -0.247148 0.075 Uiso 1 1 calc R U
H16C H 0.588893 0.907414 -0.283344 0.075 Uiso 1 1 calc R U
C21 C 0.6829(7) 0.6294(17) 0.033(3) 0.023(5) Uani 1 1 d . U
C22 C 0.7040(9) 0.7266(19) -0.056(3) 0.029(6) Uani 1 1 d . .
H22 H 0.687810 0.792182 -0.095240 0.034 Uiso 1 1 calc R U
C23 C 0.7476(8) 0.729(2) -0.086(3) 0.026(5) Uani 1 1 d . .
H23 H 0.760347 0.793104 -0.150102 0.031 Uiso 1 1 calc R U
C24 C 0.7721(8) 0.634(2) -0.021(5) 0.036(6) Uani 1 1 d . .
C25 C 0.7520(8) 0.5348(18) 0.054(3) 0.024(5) Uani 1 1 d . .
H25 H 0.768113 0.467256 0.085247 0.029 Uiso 1 1 calc R U
C26 C 0.7082(8) 0.5334(18) 0.084(3) 0.025(5) Uani 1 1 d . .
H26 H 0.695619 0.466315 0.140299 0.030 Uiso 1 1 calc R U
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'
Br Br -0.2901 2.4595 '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'
S S 0.1246 0.1234 '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
O11 Tl1 S15 61.9(4) . .
O11 Tl1 S15 121.6(3) . 7_454
S15 Tl1 S15 88.91(14) . 7_454
O11 Tl1 S15 117.5(4) . 2_665
S15 Tl1 S15 61.21(19) . 2_665
S15 Tl1 S15 80.64(11) 7_454 2_665
O11 Tl1 O11 72.9(4) . 7_454
S15 Tl1 O11 92.7(3) . 7_454
S15 Tl1 O11 58.3(3) 7_454 7_454
S15 Tl1 O11 132.4(3) 2_665 7_454
O11 Tl1 Tl1 42.1(3) . 7_455
S15 Tl1 Tl1 40.86(11) . 7_455
S15 Tl1 Tl1 129.60(11) 7_454 7_455
S15 Tl1 Tl1 77.43(10) 2_665 7_455
O11 Tl1 Tl1 109.4(3) 7_454 7_455
O11 Tl1 Tl1 82.0(3) . 7_454
S15 Tl1 Tl1 64.16(11) . 7_454
S15 Tl1 Tl1 39.84(11) 7_454 7_454
S15 Tl1 Tl1 95.16(11) 2_665 7_454
O11 Tl1 Tl1 37.8(3) 7_454 7_454
Tl1 Tl1 Tl1 98.03(3) 7_455 7_454
C14 S15 Tl1 110.4(7) . .
C14 S15 Tl1 92.7(11) . 7_455
Tl1 S15 Tl1 99.30(17) . 7_455
C14 S15 Tl1 116.9(8) . 2_665
Tl1 S15 Tl1 113.27(18) . 2_665
Tl1 S15 Tl1 121.5(2) 7_455 2_665
C14 S16 C16 106.4(12) . .
C12 O11 Tl1 121.8(13) . .
C12 O11 Tl1 106.6(15) . 7_455
Tl1 O11 Tl1 100.0(5) . 7_455
O11 C12 C13 125(2) . .
O11 C12 C21 115(2) . .
C13 C12 C21 119.7(19) . .
C14 C13 C12 126(2) . .
C14 C13 H13 117.0 . .
C12 C13 H13 117.0 . .
C13 C14 S15 127.7(16) . .
C13 C14 S16 123.2(17) . .
S15 C14 S16 109.0(11) . .
S16 C16 H16A 109.5 . .
S16 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
S16 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C26 C21 C22 116(2) . .
C26 C21 C12 119.9(19) . .
C22 C21 C12 124(2) . .
C23 C22 C21 123(2) . .
C23 C22 H22 118.5 . .
C21 C22 H22 118.5 . .
C22 C23 C24 119(2) . .
C22 C23 H23 120.6 . .
C24 C23 H23 120.6 . .
C25 C24 C23 119(2) . .
C25 C24 Br24 122.0(18) . .
C23 C24 Br24 118.4(19) . .
C26 C25 C24 121(2) . .
C26 C25 H25 119.4 . .
C24 C25 H25 119.4 . .
C21 C26 C25 121(2) . .
C21 C26 H26 119.3 . .
C25 C26 H26 119.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tl1 O11 2.869(16) .
Tl1 S15 2.989(6) .
Tl1 S15 3.053(6) 7_454
Tl1 S15 3.115(6) 2_665
Tl1 O11 3.137(17) 7_454
Tl1 Tl1 4.6049(10) 7_455
Tl1 Tl1 4.6049(10) 7_454
Br24 C24 1.88(2) .
S15 C14 1.73(2) .
S16 C14 1.76(2) .
S16 C16 1.79(3) .
O11 C12 1.23(2) .
C12 C13 1.43(3) .
C12 C21 1.51(3) .
C13 C14 1.35(3) .
C13 H13 0.9300 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C21 C26 1.38(3) .
C21 C22 1.41(3) .
C22 C23 1.38(3) .
C22 H22 0.9300 .
C23 C24 1.38(3) .
C23 H23 0.9300 .
C24 C25 1.37(3) .
C25 C26 1.39(3) .
C25 H25 0.9300 .
C26 H26 0.9300 .
