#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:25:23 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180038 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/32/7033283.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_7033283
loop_
_publ_author_name
'Kumar, Vinod'
'Singh, Vikram'
'Gupta, Ajit N.'
'Drew, Michael G. B.'
'Singh, Nanhai'
_publ_section_title
;
 Intermolecular Tl···H-C anagostic interactions in
 luminescent pyridyl functionalized thallium(I) dithiocarbamates.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1716
_journal_page_last               1723
_journal_paper_doi               10.1039/c4dt03032j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C13 H12 N3 S2 Tl'
_chemical_formula_weight         478.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.8429(14)
_cell_length_b                   9.9762(17)
_cell_length_c                   27.222(3)
_cell_measurement_reflns_used    8799
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.53
_cell_volume                     2944.6(7)
_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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0932
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8799
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.53
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    11.242
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.472
_refine_diff_density_min         -1.999
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0724
_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)+(0.0703P)²+12.5957P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1902
_reflns_number_gt                2108
_reflns_number_total             3266
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03032j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7033282--7033285.cif.'
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7033283
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Tl1 Tl 0.58409(6) 0.66528(5) 0.48879(2) 0.0594(3) Uani 1 1 d .
S11 S 0.4934(2) 0.4884(3) 0.40465(12) 0.0403(7) Uani 1 1 d .
S13 S 0.3162(3) 0.6187(4) 0.47232(12) 0.0491(8) Uani 1 1 d .
C12 C 0.3542(9) 0.5691(11) 0.4143(4) 0.032(2) Uani 1 1 d .
N14 N 0.2795(8) 0.5930(9) 0.3773(3) 0.031(2) Uani 1 1 d .
C21 C 0.3029(10) 0.5533(12) 0.3261(4) 0.037(3) Uani 1 1 d .
H21A H 0.2278 0.5160 0.3125 0.044 Uiso 1 1 calc R
H21B H 0.3649 0.4832 0.3259 0.044 Uiso 1 1 calc R
C22 C 0.3449(10) 0.6637(12) 0.2942(4) 0.036(3) Uani 1 1 d .
C23 C 0.4486(11) 0.7411(14) 0.3034(5) 0.044(3) Uani 1 1 d .
H23 H 0.4971 0.7227 0.3308 0.053 Uiso 1 1 calc R
C24 C 0.4804(13) 0.8443(14) 0.2728(6) 0.057(4) Uani 1 1 d .
H24 H 0.5521 0.8930 0.2785 0.069 Uiso 1 1 calc R
C25 C 0.4079(13) 0.8750(15) 0.2344(6) 0.054(4) Uani 1 1 d .
H25 H 0.4298 0.9471 0.2146 0.065 Uiso 1 1 calc R
N26 N 0.3058(13) 0.8065(13) 0.2234(4) 0.064(3) Uani 1 1 d .
C27 C 0.2763(13) 0.7051(15) 0.2537(5) 0.051(3) Uani 1 1 d .
H27 H 0.2039 0.6585 0.2470 0.061 Uiso 1 1 calc R
C31 C 0.1636(9) 0.6702(11) 0.3826(4) 0.033(2) Uani 1 1 d .
H31A H 0.1535 0.7268 0.3539 0.039 Uiso 1 1 calc R
H31B H 0.1706 0.7284 0.4110 0.039 Uiso 1 1 calc R
C32 C 0.0488(10) 0.5837(12) 0.3884(4) 0.034(3) Uani 1 1 d .
C33 C -0.0601(11) 0.6354(14) 0.3721(6) 0.052(4) Uani 1 1 d .
H33 H -0.0636 0.7186 0.3567 0.062 Uiso 1 1 calc R
C34 C -0.1663(11) 0.5583(14) 0.3793(6) 0.062(4) Uani 1 1 d .
H34 H -0.2425 0.5901 0.3688 0.075 Uiso 1 1 calc R
C35 C -0.1581(12) 0.4360(14) 0.4019(6) 0.057(4) Uani 1 1 d .
H35 H -0.2293 0.3846 0.4051 0.068 Uiso 1 1 calc R
N36 N -0.0505(11) 0.3865(12) 0.4198(5) 0.059(3) Uani 1 1 d .
C37 C 0.0492(11) 0.4622(13) 0.4122(5) 0.044(3) Uani 1 1 d .
H37 H 0.1243 0.4304 0.4239 0.052 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'
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'
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
N36 Tl1 S13 84.2(2) 7_665 .
N36 Tl1 S11 85.1(3) 7_665 .
S13 Tl1 S11 58.83(8) . .
N36 Tl1 S13 157.0(3) 7_665 5_666
S13 Tl1 S13 103.92(8) . 5_666
S11 Tl1 S13 81.13(8) . 5_666
N36 Tl1 S11 149.5(3) 7_665 5_666
S13 Tl1 S11 79.41(8) . 5_666
S11 Tl1 S11 107.51(7) . 5_666
S13 Tl1 S11 53.27(8) 5_666 5_666
N36 Tl1 S13 79.5(3) 7_665 3_566
S13 Tl1 S13 148.09(6) . 3_566
S11 Tl1 S13 145.01(8) . 3_566
S13 Tl1 S13 101.69(5) 5_666 3_566
S11 Tl1 S13 101.49(8) 5_666 3_566
N36 Tl1 Tl1 134.1(2) 7_665 5_666
S13 Tl1 Tl1 54.75(7) . 5_666
S11 Tl1 Tl1 57.78(7) . 5_666
S13 Tl1 Tl1 49.17(7) 5_666 5_666
S11 Tl1 Tl1 49.73(6) 5_666 5_666
S13 Tl1 Tl1 146.32(7) 3_566 5_666
C12 S11 Tl1 84.2(4) . .
C12 S11 Tl1 82.2(4) . 5_666
Tl1 S11 Tl1 72.49(7) . 5_666
C12 S13 Tl1 87.1(4) . .
C12 S13 Tl1 88.2(4) . 5_666
Tl1 S13 Tl1 76.08(8) . 5_666
C12 S13 Tl1 129.5(4) . 3_466
Tl1 S13 Tl1 124.31(12) . 3_466
Tl1 S13 Tl1 133.61(12) 5_666 3_466
N14 C12 S13 120.5(8) . .
N14 C12 S11 120.4(9) . .
S13 C12 S11 119.1(6) . .
C12 N14 C31 123.0(9) . .
C12 N14 C21 124.8(9) . .
C31 N14 C21 112.2(9) . .
N14 C21 C22 114.2(9) . .
C27 C22 C23 114.3(12) . .
C27 C22 C21 121.5(11) . .
C23 C22 C21 124.1(11) . .
C24 C23 C22 120.9(14) . .
C25 C24 C23 119.9(13) . .
N26 C25 C24 122.9(13) . .
C25 N26 C27 116.5(13) . .
N26 C27 C22 125.5(13) . .
N14 C31 C32 114.1(9) . .
C33 C32 C37 119.3(11) . .
C33 C32 C31 117.4(11) . .
C37 C32 C31 123.1(10) . .
C32 C33 C34 117.4(12) . .
C35 C34 C33 120.0(12) . .
C34 C35 N36 122.7(12) . .
C37 N36 C35 115.8(12) . .
C37 N36 Tl1 128.9(9) . 7_655
C35 N36 Tl1 113.5(9) . 7_655
N36 C37 C32 124.7(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tl1 N36 2.921(13) 7_665
Tl1 S13 2.976(4) .
Tl1 S11 3.054(3) .
Tl1 S13 3.212(4) 5_666
Tl1 S11 3.387(3) 5_666
Tl1 S13 3.478(3) 3_566
Tl1 Tl1 3.8174(12) 5_666
S11 C12 1.731(11) .
S11 Tl1 3.387(3) 5_666
S13 C12 1.706(12) .
S13 Tl1 3.212(4) 5_666
S13 Tl1 3.478(3) 3_466
C12 N14 1.313(13) .
N14 C31 1.481(13) .
N14 C21 1.471(14) .
C21 C22 1.475(16) .
C22 C27 1.395(16) .
C22 C23 1.386(16) .
C23 C24 1.37(2) .
C24 C25 1.34(2) .
C25 N26 1.335(19) .
N26 C27 1.343(18) .
C31 C32 1.522(15) .
C32 C33 1.363(16) .
C32 C37 1.375(17) .
C33 C34 1.399(17) .
C34 C35 1.369(19) .
C35 N36 1.357(18) .
N36 C37 1.335(16) .
N36 Tl1 2.921(12) 7_655
