#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:32:20 +0100 (jue 24 de mar de 2016) $
#$Revision: 179534 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/03/4500361.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_4500361
loop_
_publ_author_name
'Fujita, Wataru'
'Takahashi, Kazuyuki'
'Kobayashi, Hayao'
_publ_section_title
;
 Structural and Magnetic Studies on Two-Dimensional Square Planar Lattice
 Magnets Composed of Organic Radical Cation Salts
 (Benzo[1,2-d:4,5-d′]Bis[1,3,2]dithiazolyl-2-zolium)·X (X =
 TlBr4, TlI4, and InI4)
;
_journal_issue                   2
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              575
_journal_paper_doi               10.1021/cg101481c
_journal_volume                  11
_journal_year                    2011
_chemical_formula_sum            'C6 H2 Br4 N2 S4 Tl'
_chemical_formula_weight         754.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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            4
_cell_length_a                   10.0243(10)
_cell_length_b                   16.3867(18)
_cell_length_c                   9.0352(10)
_cell_measurement_temperature    120(2)
_cell_volume                     1484.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10706
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    22.191
_exptl_absorpt_correction_T_max  0.0953
_exptl_absorpt_correction_T_min  0.0953
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    3.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.547
_refine_diff_density_min         -1.657
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.269
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0402
_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)+(0.0093P)²+13.1502P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                1684
_reflns_number_total             1758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101481c_si_001.cif
_cod_data_source_block           090316tlbr41
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4500361
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Tl1 Tl 0.18609(4) 0.2500 0.03115(4) 0.01391(12) Uani 1 2 d S
Br2 Br 0.39211(10) 0.2500 -0.13811(12) 0.0169(2) Uani 1 2 d S
Br3 Br 0.04963(7) 0.38031(5) 0.00334(8) 0.01884(18) Uani 1 1 d .
Br4 Br 0.27533(13) 0.2500 0.29909(13) 0.0251(3) Uani 1 2 d S
S1 S 0.19942(18) 0.53156(11) -0.2458(2) 0.0142(4) Uani 1 1 d .
S2 S 0.21528(18) 0.38204(11) -0.3788(2) 0.0141(4) Uani 1 1 d .
N1 N 0.2745(6) 0.4444(4) -0.2558(7) 0.0146(13) Uani 1 1 d .
C1 C 0.0927(7) 0.4423(4) -0.4531(7) 0.0107(13) Uani 1 1 d .
C2 C 0.0837(7) 0.5202(4) -0.3845(8) 0.0113(14) Uani 1 1 d .
C3 C 0.0091(7) 0.4210(4) -0.5712(7) 0.0114(14) Uani 1 1 d .
H1 H 0.0150 0.3705 -0.6176 0.014 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Tl1 0.0150(2) 0.0141(2) 0.0126(2) 0.000 -0.00273(15) 0.000
Br2 0.0137(5) 0.0153(5) 0.0216(5) 0.000 -0.0001(4) 0.000
Br3 0.0151(4) 0.0212(4) 0.0203(4) 0.0044(3) 0.0014(3) 0.0050(3)
Br4 0.0416(7) 0.0164(5) 0.0173(5) 0.000 -0.0148(5) 0.000
S1 0.0152(9) 0.0148(9) 0.0125(9) -0.0001(7) -0.0041(7) -0.0002(7)
S2 0.0147(9) 0.0157(8) 0.0118(8) -0.0002(7) -0.0020(6) 0.0052(7)
N1 0.011(3) 0.020(3) 0.012(3) 0.002(2) -0.001(2) 0.001(3)
C1 0.011(3) 0.010(3) 0.011(3) 0.001(3) 0.006(3) 0.003(3)
C2 0.012(3) 0.014(3) 0.009(3) 0.002(3) 0.006(3) -0.005(3)
C3 0.011(3) 0.017(3) 0.007(3) -0.003(3) 0.000(3) 0.000(3)
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'
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'
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
Br3 Tl1 Br3 113.85(4) 8_565
Br3 Tl1 Br2 111.88(2) 8_565
Br3 Tl1 Br2 111.88(2) .
Br3 Tl1 Br4 106.17(3) 8_565
Br3 Tl1 Br4 106.17(3) .
Br2 Tl1 Br4 106.24(4) .
N1 S1 C2 100.2(3) .
N1 S2 C1 99.6(3) .
S1 N1 S2 115.1(4) .
C3 C1 C2 121.2(6) .
C3 C1 S2 125.7(5) .
C2 C1 S2 113.1(5) .
C3 C2 C1 122.5(6) 5_564
C3 C2 S1 125.7(5) 5_564
C1 C2 S1 111.9(5) .
C2 C3 C1 116.3(6) 5_564
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tl1 Br3 2.5483(8) 8_565
Tl1 Br3 2.5483(8) .
Tl1 Br2 2.5698(11) .
Tl1 Br4 2.5809(12) .
S1 N1 1.617(6) .
S1 C2 1.718(7) .
S2 N1 1.622(6) .
S2 C1 1.714(7) .
C1 C3 1.401(10) .
C1 C2 1.421(9) .
C2 C3 1.398(10) 5_564
C3 C2 1.398(10) 5_564
