#------------------------------------------------------------------------------
#$Date: 2019-11-15 02:05:54 +0200 (Fri, 15 Nov 2019) $
#$Revision: 227840 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/19/7701928.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_7701928
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            'C8 H7 O2 S2 Tl'
_chemical_formula_weight         403.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-10-04 deposited with the CCDC.
2018-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.16(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.2030(10)
_cell_length_b                   8.045(2)
_cell_length_c                   14.929(5)
_cell_measurement_reflns_used    9305
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.383
_cell_measurement_theta_min      2.729
_cell_volume                     504.7(2)
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL, PLATON, WINGX (Ferrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest SCM Diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9305
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         28.385
_diffrn_reflns_theta_min         2.729
_exptl_absorpt_coefficient_mu    16.376
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.656
_exptl_crystal_description       needle
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.983
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.306
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_coef       0.024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         2354
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0418
_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)+(0.1102P)²+0.7359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                2270
_reflns_number_total             2354
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03694b2.cif
_cod_data_source_block           1
_cod_database_code               7701928
_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+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Tl1 Tl 0.02111(10) 0.54944(16) 0.07102(3) 0.0378(3) Uani 1 1 d . .
O11 O 0.450(4) 0.526(2) 0.2161(8) 0.056(4) Uani 1 1 d . .
C12 C 0.592(4) 0.422(2) 0.2618(10) 0.034(3) Uani 1 1 d . .
C13 C 0.696(4) 0.256(2) 0.2406(10) 0.035(3) Uani 1 1 d . .
H13 H 0.800775 0.194105 0.286835 0.042 Uiso 1 1 calc R U
C14 C 0.655(4) 0.181(2) 0.1606(9) 0.029(3) Uani 1 1 d . .
S15 S 0.5057(8) 0.2587(6) 0.0589(3) 0.0323(8) Uani 1 1 d . .
S16 S 0.7717(12) -0.0281(6) 0.1448(3) 0.0407(9) Uani 1 1 d . .
C17 C 0.974(6) -0.089(3) 0.2477(13) 0.053(5) Uani 1 1 d . .
H17A H 0.991891 -0.210827 0.249841 0.079 Uiso 1 1 calc R U
H17B H 0.853370 -0.050369 0.298992 0.079 Uiso 1 1 calc R U
H17C H 1.187770 -0.040245 0.249891 0.079 Uiso 1 1 calc R U
C21 C 0.657(3) 0.473(2) 0.3580(10) 0.031(3) Uani 1 1 d . .
O22 O 0.846(3) 0.3776(17) 0.4134(8) 0.044(3) Uani 1 1 d . .
C23 C 0.858(5) 0.449(3) 0.4970(11) 0.044(4) Uani 1 1 d . .
H23 H 0.972590 0.408659 0.547888 0.052 Uiso 1 1 calc R U
C24 C 0.678(5) 0.588(3) 0.4939(12) 0.048(5) Uani 1 1 d . .
H24 H 0.644922 0.661684 0.542450 0.058 Uiso 1 1 calc R U
C25 C 0.546(5) 0.605(3) 0.4056(16) 0.052(4) Uani 1 1 d . .
H25 H 0.408633 0.691115 0.384287 0.062 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'
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'
F F 0.0171 0.0103 '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 65.2(3) . .
O11 Tl1 S15 114.9(4) . 1_455
S15 Tl1 S15 83.69(13) . 1_455
O11 Tl1 O11 87.3(4) . 1_455
S15 Tl1 O11 119.0(3) . 1_455
S15 Tl1 O11 59.2(3) 1_455 1_455
O11 Tl1 S15 96.0(4) . 2_655
S15 Tl1 S15 86.90(5) . 2_655
S15 Tl1 S15 139.79(6) 1_455 2_655
O11 Tl1 S15 152.3(3) 1_455 2_655
O11 Tl1 S15 152.5(4) . 2
S15 Tl1 S15 140.09(7) . 2
S15 Tl1 S15 84.04(5) 1_455 2
O11 Tl1 S15 85.8(2) 1_455 2
S15 Tl1 S15 78.55(9) 2_655 2
O11 Tl1 S16 123.1(3) . 2_655
S15 Tl1 S16 68.14(11) . 2_655
S15 Tl1 S16 89.92(10) 1_455 2_655
O11 Tl1 S16 145.0(2) 1_455 2_655
S15 Tl1 S16 50.54(11) 2_655 2_655
S15 Tl1 S16 74.02(11) 2 2_655
O11 Tl1 S16 90.8(4) . 1_465
S15 Tl1 S16 153.01(10) . 1_465
S15 Tl1 S16 119.35(11) 1_455 1_465
O11 Tl1 S16 69.1(3) 1_455 1_465
S15 Tl1 S16 83.34(12) 2_655 1_465
S15 Tl1 S16 61.88(11) 2 1_465
S16 Tl1 S16 121.60(13) 2_655 1_465
O11 Tl1 Tl1 51.0(4) . 1_655
S15 Tl1 Tl1 48.98(8) . 1_655
S15 Tl1 Tl1 132.68(8) 1_455 1_655
O11 Tl1 Tl1 138.4(2) 1_455 1_655
S15 Tl1 Tl1 51.70(7) 2_655 1_655
S15 Tl1 Tl1 130.25(7) 2 1_655
S16 Tl1 Tl1 74.07(8) 2_655 1_655
S16 Tl1 Tl1 106.68(8) 1_465 1_655
O11 Tl1 Tl1 129.0(4) . 1_455
S15 Tl1 Tl1 131.02(8) . 1_455
S15 Tl1 Tl1 47.32(8) 1_455 1_455
O11 Tl1 Tl1 41.6(2) 1_455 1_455
S15 Tl1 Tl1 128.30(7) 2_655 1_455
S15 Tl1 Tl1 49.75(7) 2 1_455
S16 Tl1 Tl1 105.92(8) 2_655 1_455
S16 Tl1 Tl1 73.32(8) 1_465 1_455
Tl1 Tl1 Tl1 180.0 1_655 1_455
O11 Tl1 Tl1 108.6(4) . 2_545
S15 Tl1 Tl1 47.71(8) . 2_545
S15 Tl1 Tl1 46.01(7) 1_455 2_545
O11 Tl1 Tl1 103.6(3) 1_455 2_545
S15 Tl1 Tl1 101.36(9) 2_655 2_545
S15 Tl1 Tl1 98.90(9) 2 2_545
S16 Tl1 Tl1 53.59(8) 2_655 2_545
S16 Tl1 Tl1 159.21(7) 1_465 2_545
Tl1 Tl1 Tl1 91.695(14) 1_655 2_545
Tl1 Tl1 Tl1 88.305(14) 1_455 2_545
O11 Tl1 Tl1 116.1(4) . 2
S15 Tl1 Tl1 131.12(9) . 2
S15 Tl1 Tl1 127.00(8) 1_455 2
O11 Tl1 Tl1 109.7(3) 1_455 2
S15 Tl1 Tl1 44.54(8) 2_655 2
S15 Tl1 Tl1 43.11(8) 2 2
S16 Tl1 Tl1 74.33(9) 2_655 2
S16 Tl1 Tl1 47.40(8) 1_465 2
Tl1 Tl1 Tl1 91.694(14) 1_655 2
Tl1 Tl1 Tl1 88.305(14) 1_455 2
Tl1 Tl1 Tl1 124.32(3) 2_545 2
C12 O11 Tl1 141.0(13) . .
C12 O11 Tl1 93.0(11) . 1_655
Tl1 O11 Tl1 87.3(4) . 1_655
O11 C12 C13 130.8(16) . .
O11 C12 C21 115.0(15) . .
C13 C12 C21 114.0(14) . .
C14 C13 C12 125.1(15) . .
C14 C13 H13 117.4 . .
C12 C13 H13 117.4 . .
C13 C14 S15 130.3(14) . .
C13 C14 S16 120.9(11) . .
S15 C14 S16 108.8(8) . .
C14 S15 Tl1 116.4(6) . .
C14 S15 Tl1 89.1(5) . 1_655
Tl1 S15 Tl1 83.69(13) . 1_655
C14 S15 Tl1 96.8(6) . 2_645
Tl1 S15 Tl1 145.90(15) . 2_645
Tl1 S15 Tl1 89.46(10) 1_655 2_645
C14 S15 Tl1 122.7(6) . 2_545
Tl1 S15 Tl1 89.18(9) . 2_545
Tl1 S15 Tl1 146.85(15) 1_655 2_545
Tl1 S15 Tl1 78.55(9) 2_645 2_545
C14 S16 C17 105.8(9) . .
C14 S16 Tl1 91.7(5) . 2_645
C17 S16 Tl1 136.6(9) . 2_645
C14 S16 Tl1 170.5(5) . 1_645
C17 S16 Tl1 82.6(7) . 1_645
Tl1 S16 Tl1 79.00(9) 2_645 1_645
S16 C17 H17A 109.5 . .
S16 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
S16 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
O22 C21 C25 108.8(15) . .
O22 C21 C12 121.0(14) . .
C25 C21 C12 130.2(16) . .
C21 O22 C23 108.8(14) . .
C24 C23 O22 107.9(16) . .
C24 C23 H23 126.1 . .
O22 C23 H23 126.1 . .
C25 C24 C23 108.8(16) . .
C25 C24 H24 125.6 . .
C23 C24 H24 125.6 . .
C24 C25 C21 105.8(17) . .
C24 C25 H25 127.1 . .
C21 C25 H25 127.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tl1 O11 2.795(12) .
Tl1 S15 3.109(4) .
Tl1 S15 3.191(5) 1_455
Tl1 O11 3.271(17) 1_455
Tl1 S15 3.273(4) 2_655
Tl1 S15 3.366(4) 2
Tl1 S16 3.411(5) 2_655
Tl1 S16 3.729(5) 1_465
Tl1 Tl1 4.2030(10) 1_655
Tl1 Tl1 4.2030(10) 1_455
Tl1 Tl1 4.5489(10) 2_545
Tl1 Tl1 4.5489(10) 2
O11 C12 1.23(2) .
C12 C13 1.45(2) .
C12 C21 1.51(2) .
C13 C14 1.35(2) .
C13 H13 0.9500 .
C14 S15 1.747(13) .
C14 S16 1.767(18) .
S16 C17 1.810(17) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C21 O22 1.37(2) .
C21 C25 1.37(3) .
O22 C23 1.38(2) .
C23 C24 1.35(3) .
C23 H23 0.9500 .
C24 C25 1.43(3) .
C24 H24 0.9500 .
C25 H25 0.9500 .
