#------------------------------------------------------------------------------
#$Date: 2021-04-07 10:20:06 +0300 (Wed, 07 Apr 2021) $
#$Revision: 263939 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/15/1561527.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_1561527
loop_
_publ_author_name
'Yohannan, Jinu P.'
'Vidyasagar, Kanamaluru'
_publ_section_title
;
 Syntheses, structural variants and characterization of AInM′S4
 (A=alkali metals, Tl; M′ = Ge, Sn) compounds; facile ion-exchange
 reactions of layered NaInSnS4 and KInSnS4 compounds
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              291
_journal_page_last               302
_journal_paper_doi               10.1016/j.jssc.2016.03.045
_journal_volume                  238
_journal_year                    2016
_chemical_formula_sum            'Ge In S4 Tl'
_chemical_formula_weight         520.08
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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_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                   17.2759(12)
_cell_length_b                   7.3404(5)
_cell_length_c                   11.6671(8)
_cell_measurement_reflns_used    590
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.79
_cell_measurement_theta_min      3.49
_cell_volume                     1479.53(18)
_computing_cell_refinement       APEXII,Bruker,2004
_computing_data_collection       APEXII,Bruker,2004
_computing_data_reduction        SAINT,Bruker,2004
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Bruker ApexII ccd area detector'
_diffrn_measurement_method       'phi and omega 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  0.0657
_diffrn_reflns_av_sigmaI/netI    0.1264
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3770
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    29.868
_exptl_absorpt_correction_T_max  0.550
_exptl_absorpt_correction_T_min  0.355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS(Bruker,2004)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1807
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.721
_refine_diff_density_min         -2.168
_refine_diff_density_rms         0.416
_refine_ls_extinction_coef       0.0001
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1809
_refine_ls_R_factor_gt           0.0748
_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)+(0.1018P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1725
_refine_ls_wR_factor_ref         0.2236
_reflns_number_gt                761
_reflns_number_total             1707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2016-238-291.cif
_cod_data_source_block           TlInGeS4-4-Alpha
_cod_original_sg_symbol_Hall     -P2ac2n
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               1561527
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Tl1 Tl 0.15726(11) 0.2500 0.0632(2) 0.0966(9) Uani 1 2 d S . .
Tl2 Tl 0.05514(13) 0.2500 0.3828(2) 0.0937(9) Uani 1 2 d S . .
In1 In 0.15494(9) 0.9988(2) 0.74427(19) 0.0328(5) Uani 0.70 1 d P . .
Ge1 Ge 0.15494(9) 0.9988(2) 0.74427(19) 0.0328(5) Uani 0.30 1 d P . .
In2 In 0.32504(13) 0.2500 0.8113(3) 0.0313(8) Uani 0.46 2 d SP . .
Ge2 Ge 0.32504(13) 0.2500 0.8113(3) 0.0313(8) Uani 0.54 2 d SP . .
In3 In 0.48406(15) 0.2500 0.6869(3) 0.0322(8) Uani 0.14 2 d SP . .
Ge3 Ge 0.48406(15) 0.2500 0.6869(3) 0.0322(8) Uani 0.86 2 d SP . .
S1 S 0.3483(5) 0.2500 0.1188(9) 0.046(2) Uani 1 2 d S . .
S2 S 0.1602(5) 0.2500 0.6194(10) 0.045(2) Uani 1 2 d S . .
S3 S 0.3643(5) 0.2500 0.6173(9) 0.050(3) Uani 1 2 d S . .
S4 S 0.4546(5) 0.2500 0.8764(8) 0.054(3) Uani 1 2 d S . .
S5 S 0.0436(4) -0.0027(8) 0.8653(8) 0.055(2) Uani 1 1 d . . .
S6 S 0.2626(4) 0.9907(8) 0.8698(9) 0.061(2) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1550 1.8000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7280 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8360 9.6690 '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
S1 In1 S2 103.0(3) 2_565 1_565
S1 In1 S6 112.7(3) 2_565 .
S2 In1 S6 111.9(3) 1_565 .
S1 In1 S5 110.3(3) 2_565 1_565
S2 In1 S5 113.7(3) 1_565 1_565
S6 In1 S5 105.5(3) . 1_565
S1 Ge1 S2 103.0(3) 2_565 1_565
S1 Ge1 S6 112.7(3) 2_565 .
S2 Ge1 S6 111.9(3) 1_565 .
S1 Ge1 S5 110.3(3) 2_565 1_565
S2 Ge1 S5 113.7(3) 1_565 1_565
S6 Ge1 S5 105.5(3) . 1_565
S6 In2 S6 112.3(4) 1_545 8_575
S6 In2 S3 114.8(3) 1_545 .
S6 In2 S3 114.8(3) 8_575 .
S6 In2 S4 110.5(2) 1_545 .
S6 In2 S4 110.5(2) 8_575 .
S3 In2 S4 92.1(3) . .
S6 In2 Ge3 123.7(2) 1_545 .
S6 In2 Ge3 123.7(2) 8_575 .
S3 In2 Ge3 45.5(2) . .
S4 In2 Ge3 46.6(3) . .
S6 In2 In3 123.7(2) 1_545 .
S6 In2 In3 123.7(2) 8_575 .
S3 In2 In3 45.5(2) . .
S4 In2 In3 46.6(3) . .
Ge3 In2 In3 0.00(12) . .
S6 Ge2 S6 112.3(4) 1_545 8_575
S6 Ge2 S3 114.8(3) 1_545 .
S6 Ge2 S3 114.8(3) 8_575 .
S6 Ge2 S4 110.5(2) 1_545 .
S6 Ge2 S4 110.5(2) 8_575 .
S3 Ge2 S4 92.1(3) . .
S6 Ge2 In3 123.7(2) 1_545 .
S6 Ge2 In3 123.7(2) 8_575 .
S3 Ge2 In3 45.5(2) . .
S4 Ge2 In3 46.6(3) . .
S5 In3 S5 114.4(4) 3_556 6_657
S5 In3 S3 109.4(2) 3_556 .
S5 In3 S3 109.4(2) 6_657 .
S5 In3 S4 111.9(3) 3_556 .
S5 In3 S4 111.9(3) 6_657 .
S3 In3 S4 98.5(4) . .
S5 In3 In2 122.8(2) 3_556 .
S5 In3 In2 122.8(2) 6_657 .
S3 In3 In2 49.3(3) . .
S4 In3 In2 49.2(2) . .
S5 In3 Ge2 122.8(2) 3_556 .
S5 In3 Ge2 122.8(2) 6_657 .
S3 In3 Ge2 49.3(3) . .
S4 In3 Ge2 49.2(2) . .
In2 In3 Ge2 0.00(4) . .
S5 Ge3 S5 114.4(4) 3_556 6_657
S5 Ge3 S3 109.4(2) 3_556 .
S5 Ge3 S3 109.4(2) 6_657 .
S5 Ge3 S4 111.9(3) 3_556 .
S5 Ge3 S4 111.9(3) 6_657 .
S3 Ge3 S4 98.5(4) . .
S5 Ge3 In2 122.8(2) 3_556 .
S5 Ge3 In2 122.8(2) 6_657 .
S3 Ge3 In2 49.3(3) . .
S4 Ge3 In2 49.2(2) . .
Ge1 S1 In1 0.00(11) 7_655 7_655
Ge1 S1 In1 102.5(4) 7_655 2_564
In1 S1 In1 102.5(4) 7_655 2_564
Ge1 S1 Ge1 102.5(4) 7_655 2_564
In1 S1 Ge1 102.5(4) 7_655 2_564
In1 S1 Ge1 0.00(12) 2_564 2_564
Ge1 S2 In1 0.00(12) 8_575 8_575
Ge1 S2 In1 103.3(4) 8_575 1_545
In1 S2 In1 103.3(4) 8_575 1_545
Ge1 S2 Ge1 103.3(4) 8_575 1_545
In1 S2 Ge1 103.3(4) 8_575 1_545
In1 S2 Ge1 0.00(9) 1_545 1_545
Ge3 S3 In3 0.00(18) . .
Ge3 S3 In2 85.2(4) . .
In3 S3 In2 85.2(4) . .
Ge3 S3 Ge2 85.2(4) . .
In3 S3 Ge2 85.2(4) . .
In2 S3 Ge2 0.00(11) . .
Ge3 S4 In3 0.00(4) . .
Ge3 S4 In2 84.2(3) . .
In3 S4 In2 84.2(3) . .
Ge3 S4 Ge2 84.2(3) . .
In3 S4 Ge2 84.2(3) . .
In2 S4 Ge2 0.00(4) . .
Ge3 S5 In3 0.0(2) 6_557 6_557
Ge3 S5 In1 102.0(3) 6_557 1_545
In3 S5 In1 102.0(3) 6_557 1_545
Ge3 S5 Ge1 102.0(3) 6_557 1_545
In3 S5 Ge1 102.0(3) 6_557 1_545
In1 S5 Ge1 0.00(9) 1_545 1_545
Ge2 S6 In2 0.00(16) 1_565 1_565
Ge2 S6 In1 99.5(3) 1_565 .
In2 S6 In1 99.5(3) 1_565 .
Ge2 S6 Ge1 99.5(3) 1_565 .
In2 S6 Ge1 99.5(3) 1_565 .
In1 S6 Ge1 0.00(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
In1 S1 2.342(7) 2_565
In1 S2 2.351(7) 1_565
In1 S6 2.368(8) .
In1 S5 2.386(7) 1_565
Ge1 S1 2.342(7) 2_565
Ge1 S2 2.351(7) 1_565
Ge1 S6 2.368(8) .
Ge1 S5 2.386(7) 1_565
In2 S6 2.292(7) 1_545
In2 S6 2.292(7) 8_575
In2 S3 2.363(12) .
In2 S4 2.364(9) .
In2 Ge3 3.107(4) .
In2 In3 3.107(4) .
Ge2 S6 2.292(7) 1_545
Ge2 S6 2.292(7) 8_575
Ge2 S3 2.363(12) .
Ge2 S4 2.364(9) .
Ge2 In3 3.107(4) .
In3 S5 2.207(7) 3_556
In3 S5 2.207(6) 6_657
In3 S3 2.223(8) .
In3 S4 2.268(11) .
Ge3 S5 2.207(7) 3_556
Ge3 S5 2.207(6) 6_657
Ge3 S3 2.223(8) .
Ge3 S4 2.268(11) .
S1 Ge1 2.342(7) 7_655
S1 In1 2.342(7) 7_655
S1 In1 2.342(7) 2_564
S1 Ge1 2.342(7) 2_564
S2 Ge1 2.351(7) 8_575
S2 In1 2.351(7) 8_575
S2 In1 2.351(7) 1_545
S2 Ge1 2.351(7) 1_545
S5 Ge3 2.207(6) 6_557
S5 In3 2.207(6) 6_557
S5 In1 2.386(7) 1_545
S5 Ge1 2.386(7) 1_545
S6 Ge2 2.292(7) 1_565
S6 In2 2.292(7) 1_565
