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#$Date: 2021-08-31 11:41:37 +0300 (Tue, 31 Aug 2021) $
#$Revision: 268319 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/44/1564477.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_1564477
loop_
_publ_author_name
'Yu, Ji-Ming'
'Cai, Ting'
'Ma, Zhong-Jie'
'Wang, Fei'
'Wang, Huan'
'Yu, Ji-Peng'
'Xiao, Lu-Lu'
'Cheng, Fang-Fang'
'Xiong, Wei-Wei'
_publ_section_title
;
 Using thiol-amine solvent mixture to prepare main group heterometallic
 chalcogenides
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119698
_journal_paper_doi               10.1016/j.ica.2020.119698
_journal_volume                  509
_journal_year                    2020
_chemical_formula_moiety         'C12 Ge4 In N8 O S13'
_chemical_formula_sum            'C12 Ge4 In N8 O S13'
_chemical_formula_weight         1094.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2157(9)
_cell_length_b                   11.3247(5)
_cell_length_c                   15.6853(7)
_cell_measurement_reflns_used    2387
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.0910
_cell_measurement_theta_min      3.2240
_cell_volume                     3768.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'DIAMOND. Version 3.0. Crystal Impact'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.1196
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14644
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.769
_exptl_absorpt_coefficient_mu    4.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.891
_refine_diff_density_min         -2.202
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         4302
_refine_ls_number_restraints     137
_refine_ls_restrained_S_all      1.450
_refine_ls_R_factor_all          0.1603
_refine_ls_R_factor_gt           0.0866
_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)+(0.1156P)²+15.2135P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2165
_refine_ls_wR_factor_ref         0.2747
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2243
_reflns_number_total             4302
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA_2020-509-119698.cif
_cod_data_source_block           compound-3
_cod_database_code               1564477
_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.19249(6) 0.250000 0.05873(8) 0.0495(4) Uani 1 2 d S T P . .
Ge1 Ge 0.34191(6) 0.08928(10) 0.13014(8) 0.0429(4) Uani 1 1 d . . . . .
Ge2 Ge 0.34006(8) 0.250000 -0.07302(11) 0.0378(5) Uani 1 2 d S T P . .
Ge3 Ge 0.03460(11) 0.250000 0.0139(2) 0.0794(8) Uani 1 2 d S TU P . .
S1 S -0.0442(4) 0.250000 0.1078(7) 0.125(2) Uani 1 2 d S TU P . .
S2 S 0.0155(6) 0.250000 -0.1265(7) 0.157(3) Uani 1 2 d S TU P . .
S3 S 0.3802(2) 0.250000 0.1970(3) 0.0481(11) Uani 1 2 d S T P . .
S4 S 0.37652(17) 0.0880(3) -0.0058(2) 0.0520(9) Uani 1 1 d . . . . .
S5 S 0.2359(2) 0.250000 -0.0875(3) 0.0499(11) Uani 1 2 d S T P . .
S6 S 0.23871(18) 0.0788(3) 0.1390(2) 0.0588(9) Uani 1 1 d . . . . .
S7 S 0.3855(2) 0.250000 -0.1976(3) 0.0565(12) Uani 1 2 d S T P . .
S8 S 0.3828(2) -0.0625(3) 0.1938(3) 0.0757(12) Uani 1 1 d . . . . .
S9 S 0.0975(2) 0.1024(4) 0.0431(3) 0.0795(12) Uani 1 1 d . U . . .
C1 C 0.2879(11) 0.250000 0.6046(14) 0.072(6) Uani 1 2 d S TU P . .
C2 C 0.2420(11) 0.250000 0.5331(15) 0.078(4) Uani 1 2 d S TU P . .
C3 C 0.2831(11) 0.0619(16) 0.3771(15) 0.121(8) Uani 1 1 d D . . . .
C4A C 0.2454(15) 0.183(3) 0.383(2) 0.076(5) Uiso 0.5 1 d . U P . .
C4B C 0.2493(14) 0.1279(19) 0.440(2) 0.077(5) Uiso 0.5 1 d D U P . .
C5 C 0.4103(15) -0.250000 -0.0435(16) 0.179(6) Uiso 1 2 d DS U P . .
C6 C 0.4571(11) -0.149(2) -0.1718(18) 0.186(6) Uiso 1 1 d D U . . .
C7 C 0.4144(11) -0.070(2) -0.2234(19) 0.177(6) Uiso 1 1 d D U . . .
C8 C 0.4643(19) -0.200(4) 0.0055(19) 0.180(6) Uiso 0.5 1 d D U P . .
N1 N 0.4685(15) -0.250000 0.0939(19) 0.167(6) Uiso 1 2 d DS U P . .
N2 N 0.2730(9) 0.250000 0.4542(11) 0.072(4) Uani 1 2 d DS TU P . .
N3 N 0.2520(8) 0.250000 0.6912(12) 0.074(5) Uani 1 2 d S TU P . .
N4 N 0.3515(8) 0.0490(14) 0.3823(10) 0.097(5) Uani 1 1 d . . . . .
N5 N 0.4207(12) -0.250000 -0.1384(14) 0.177(5) Uani 1 2 d DS TU P . .
N6 N 0.4546(9) 0.0119(16) -0.2767(11) 0.128(5) Uiso 1 1 d D U . . .
O1 O -0.0639(9) 0.250000 0.0101(15) 0.120(4) Uani 1 2 d S TU P . .
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'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In -0.7276 1.3100 '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'
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
S5 In1 S6 108.65(11) . .
S5 In1 S6 108.65(11) . 7_565
S6 In1 S6 101.07(17) . 7_565
S5 In1 S9 101.47(14) . 7_565
S6 In1 S9 146.81(15) . 7_565
S6 In1 S9 81.68(13) 7_565 7_565
S5 In1 S9 101.47(14) . .
S6 In1 S9 81.68(13) . .
S6 In1 S9 146.81(15) 7_565 .
S9 In1 S9 78.9(2) 7_565 .
S8 Ge1 S6 109.04(16) . .
S8 Ge1 S3 106.38(16) . .
S6 Ge1 S3 111.94(16) . .
S8 Ge1 S4 107.46(15) . .
S6 Ge1 S4 112.58(14) . .
S3 Ge1 S4 109.16(15) . .
S7 Ge2 S5 110.37(19) . .
S7 Ge2 S4 105.53(12) . 7_565
S5 Ge2 S4 112.91(12) . 7_565
S7 Ge2 S4 105.53(12) . .
S5 Ge2 S4 112.91(12) . .
S4 Ge2 S4 109.07(19) 7_565 .
O1 Ge3 S9 128.0(2) . .
O1 Ge3 S9 128.0(2) . 7_565
S9 Ge3 S9 99.7(3) . 7_565
O1 Ge3 S1 43.0(6) . .
S9 Ge3 S1 108.6(2) . .
S9 Ge3 S1 108.6(2) 7_565 .
O1 Ge3 S2 77.9(7) . .
S9 Ge3 S2 108.4(2) . .
S9 Ge3 S2 108.4(2) 7_565 .
S1 Ge3 S2 120.9(4) . .
O1 S1 Ge3 63.9(8) . .
Ge1 S3 Ge1 107.82(19) 7_565 .
Ge2 S4 Ge1 108.98(13) . .
Ge2 S5 In1 106.01(19) . .
Ge1 S6 In1 108.40(14) . .
Ge3 S9 In1 90.07(17) . .
C2 C1 N3 109.8(19) . .
N2 C2 C1 111(2) . .
N2 C2 C4B 47.5(9) . .
C1 C2 C4B 119.8(15) . .
N2 C2 C4B 47.5(9) . 7_565
C1 C2 C4B 119.8(15) . 7_565
C4B C2 C4B 86.5(19) . 7_565
C4B C3 N4 121(2) . .
C4B C3 C4A 42.1(16) . .
N4 C3 C4A 125.7(18) . .
C4B C4A N2 69(2) . .
C4B C4A C4A 125(2) . 7_565
N2 C4A C4A 58.9(13) . 7_565
C4B C4A C3 61.2(18) . .
N2 C4A C3 107(2) . .
C4A C4A C3 149.5(14) 7_565 .
C4A C4B C3 77(2) . .
C4A C4B N2 68(2) . .
C3 C4B N2 114.8(18) . .
C4A C4B C2 101(2) . .
C3 C4B C2 154(2) . .
N2 C4B C2 44.0(10) . .
C8 C5 C8 44(4) . 7
C8 C5 N5 113.4(19) . .
C8 C5 N5 113.4(19) 7 .
N5 C6 C7 109.5(16) . .
C6 C7 N6 108.8(15) . .
C8 C8 C5 67.8(18) 7 .
C8 C8 N1 67.9(18) 7 .
C5 C8 N1 112.3(19) . .
C8 N1 C8 44(4) 7 .
C2 N2 C4A 119.0(18) . 7_565
C2 N2 C4A 119.0(18) . .
C4A N2 C4A 62(3) 7_565 .
C2 N2 C4B 88.5(13) . .
C4A N2 C4B 103(2) 7_565 .
C4A N2 C4B 43.3(16) . .
C2 N2 C4B 88.5(13) . 7_565
C4A N2 C4B 43.3(16) 7_565 7_565
C4A N2 C4B 103(2) . 7_565
C4B N2 C4B 137(3) . 7_565
C6 N5 C6 101(3) 7 .
C6 N5 C5 115.3(16) 7 .
C6 N5 C5 115.3(16) . .
S1 O1 Ge3 73.1(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
In1 S5 2.472(5) .
In1 S6 2.511(4) .
In1 S6 2.511(4) 7_565
In1 S9 2.630(5) 7_565
In1 S9 2.630(5) .
Ge1 S8 2.169(4) .
Ge1 S6 2.197(4) .
Ge1 S3 2.252(3) .
Ge1 S4 2.256(3) .
Ge2 S7 2.179(5) .
Ge2 S5 2.221(5) .
Ge2 S4 2.253(3) 7_565
Ge2 S4 2.253(3) .
Ge3 O1 2.091(19) .
Ge3 S9 2.188(5) .
Ge3 S9 2.188(5) 7_565
Ge3 S1 2.228(9) .
Ge3 S2 2.239(10) .
S1 O1 1.59(2) .
C1 C2 1.49(3) .
C1 N3 1.56(3) .
C2 N2 1.40(3) .
C2 C4B 2.02(3) .
C2 C4B 2.02(3) 7_565
C3 C4B 1.431(18) .
C3 N4 1.46(3) .
C3 C4A 1.59(4) .
C4A C4B 1.09(4) .
C4A N2 1.48(3) .
C4A C4A 1.52(6) 7_565
C4B N2 1.488(17) .
C5 C8 1.490(19) .
C5 C8 1.490(19) 7
C5 N5 1.506(18) .
C6 N5 1.474(16) .
C6 C7 1.506(17) .
C7 N6 1.516(17) .
C8 C8 1.13(9) 7
C8 N1 1.499(19) .
