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#$Date: 2020-04-04 07:10:10 +0300 (Sat, 04 Apr 2020) $
#$Revision: 250060 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/45/4134533.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_4134533
loop_
_publ_author_name
'Khoury, Jason F.'
'Rettie, Alexander J. E.'
'Robredo, Iñigo'
'Krogstad, Matthew J.'
'Malliakas, Christos D.'
'Bergara, Aitor'
'Vergniory, Maia G.'
'Osborn, Raymond'
'Rosenkranz, Stephan'
'Chung, Duck Young'
'Kanatzidis, Mercouri G.'
_publ_section_title
;
 The Subchalcogenides Ir₂In₈Q (Q = S, Se, Te): Dirac
 Semimetal Candidates with Re-entrant Structural Modulation.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6312
_journal_page_last               6323
_journal_paper_doi               10.1021/jacs.0c00809
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         '0.25(In32 Ir8 S4)'
_chemical_formula_sum            'In8 Ir2 S'
_chemical_formula_weight         1335.02
_space_group_crystal_system      tetragonal
_space_group_IT_number           136
_space_group_name_Hall           '-P 4n 2n'
_space_group_name_H-M_alt        'P 42/m n m'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9200(14)
_cell_length_b                   9.9200(14)
_cell_length_c                   10.140(2)
_cell_measurement_reflns_used    6999
_cell_measurement_temperature    299
_cell_measurement_theta_max      29.931
_cell_measurement_theta_min      2.873
_cell_volume                     997.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      299
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.931
_diffrn_reflns_theta_min         2.873
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    44.806
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.3958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1463 before and 0.0405 after correction.
The Ratio of minimum to maximum transmission is 0.5306.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    8.887
_exptl_crystal_description       plate
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.084
_refine_diff_density_max         2.946
_refine_diff_density_min         -4.687
_refine_diff_density_rms         0.352
_refine_ls_extinction_coef       0.00215(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+34.7316P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                814
_reflns_number_total             820
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c00809_si_002.cif
_cod_data_source_block           jfk_2_98a_rt_0m
_cod_depositor_comments
'Adding full bibliography for 4134530--4134534.cif.'
_cod_database_code               4134533
_shelx_shelxl_version_number     2014/7
_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.
;
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y, x, -z'
'-y, -x, -z'
'-x, -y, -z'
'x, y, -z'
'y-1/2, -x-1/2, -z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y, -x, z'
'y, x, 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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.68758(2) 0.68758(2) 0.73990(3) 0.00305(10) Uani 1 2 d S T P . .
In1 In 0.59567(7) 0.59567(7) 0.5000 0.00968(19) Uani 1 4 d S T P . .
In2 In 0.5000 0.5000 0.83403(10) 0.0119(2) Uani 1 4 d S T P . .
In3 In 0.94780(5) 0.70090(5) 0.80462(5) 0.01297(13) Uani 1 1 d . . . . .
In4 In 0.68412(8) 0.68412(8) 1.0000 0.0180(2) Uani 1 4 d S T P . .
In5 In 0.80032(8) 0.80032(8) 0.5000 0.0394(4) Uani 1 4 d S T P . .
S1 S 1.0000 0.5000 1.0000 0.0433(16) Uani 1 4 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 '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'
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
_geom_angle_publ_flag
In1 Ir1 In2 82.01(3) . . ?
In1 Ir1 In5 60.96(3) . . ?
In2 Ir1 In5 142.97(3) . . ?
In3 Ir1 In1 72.054(14) 6_466 . ?
In3 Ir1 In1 123.670(18) . . ?
In3 Ir1 In1 123.670(18) 16 . ?
In3 Ir1 In1 72.054(14) 12_757 . ?
In3 Ir1 In2 126.332(19) 16 . ?
In3 Ir1 In2 126.332(19) . . ?
In3 Ir1 In2 74.937(14) 12_757 . ?
In3 Ir1 In2 74.937(14) 6_466 . ?
In3 Ir1 In3 152.389(11) 12_757 16 ?
In3 Ir1 In3 71.56(2) 12_757 . ?
In3 Ir1 In3 135.56(3) 6_466 12_757 ?
In3 Ir1 In3 81.00(2) 16 . ?
In3 Ir1 In3 152.389(11) 6_466 . ?
In3 Ir1 In3 71.56(2) 6_466 16 ?
In3 Ir1 In5 79.29(2) 16 . ?
In3 Ir1 In5 92.410(16) 6_466 . ?
In3 Ir1 In5 79.29(2) . . ?
In3 Ir1 In5 92.410(16) 12_757 . ?
In4 Ir1 In1 151.02(3) . . ?
In4 Ir1 In2 69.01(3) . . ?
In4 Ir1 In3 99.402(17) . 12_757 ?
In4 Ir1 In3 76.54(2) . . ?
In4 Ir1 In3 76.54(2) . 16 ?
In4 Ir1 In3 99.402(17) . 6_466 ?
In4 Ir1 In5 148.02(3) . . ?
Ir1 In1 Ir1 124.15(4) 10_556 . ?
Ir1 In1 In3 52.645(12) . 12_757 ?
Ir1 In1 In3 119.48(2) 10_556 12_757 ?
Ir1 In1 In3 52.645(12) 10_556 13_575 ?
Ir1 In1 In3 119.48(2) 10_556 6_466 ?
Ir1 In1 In3 52.645(12) 10_556 3_644 ?
Ir1 In1 In3 119.48(2) . 3_644 ?
Ir1 In1 In3 119.48(2) . 13_575 ?
Ir1 In1 In3 52.645(12) . 6_466 ?
Ir1 In1 In5 62.074(19) 10_556 . ?
Ir1 In1 In5 62.074(19) . . ?
In1 In1 Ir1 117.926(19) 9_666 . ?
In1 In1 Ir1 117.926(19) 9_666 10_556 ?
In1 In1 In3 97.028(19) 9_666 13_575 ?
In1 In1 In3 97.028(19) 9_666 6_466 ?
In1 In1 In3 97.028(19) 9_666 3_644 ?
In1 In1 In3 97.028(19) 9_666 12_757 ?
In1 In1 In5 180.00(4) 9_666 . ?
In3 In1 In3 165.94(4) 6_466 3_644 ?
In3 In1 In3 165.94(4) 12_757 13_575 ?
In3 In1 In3 101.34(2) 3_644 13_575 ?
In3 In1 In3 101.34(2) 6_466 12_757 ?
In3 In1 In3 76.91(2) 6_466 13_575 ?
In3 In1 In3 76.91(2) 12_757 3_644 ?
In5 In1 In3 82.972(19) . 6_466 ?
In5 In1 In3 82.972(19) . 12_757 ?
In5 In1 In3 82.972(19) . 13_575 ?
In5 In1 In3 82.972(19) . 3_644 ?
Ir1 In2 Ir1 140.13(4) 2_665 . ?
Ir1 In2 In2 109.94(2) 2_665 9_667 ?
Ir1 In2 In2 109.94(2) . 9_667 ?
Ir1 In2 In3 110.22(2) . 5_646 ?
Ir1 In2 In3 50.651(11) 2_665 5_646 ?
Ir1 In2 In3 110.22(2) . 11_577 ?
Ir1 In2 In3 50.651(11) 2_665 11_577 ?
Ir1 In2 In3 110.22(2) 2_665 12_757 ?
Ir1 In2 In3 110.22(2) 2_665 6_466 ?
Ir1 In2 In3 50.651(11) . 12_757 ?
Ir1 In2 In3 50.651(11) . 6_466 ?
Ir1 In2 In4 53.022(17) . . ?
Ir1 In2 In4 53.023(17) 2_665 9_667 ?
Ir1 In2 In4 166.85(4) 2_665 . ?
Ir1 In2 In4 166.85(4) . 9_667 ?
Ir1 In2 In5 100.114(8) 2_665 3_645 ?
Ir1 In2 In5 100.113(8) . 11_577 ?
Ir1 In2 In5 100.114(8) 2_665 11_577 ?
Ir1 In2 In5 100.113(8) . 3_645 ?
In3 In2 In2 115.022(19) 12_757 9_667 ?
In3 In2 In2 115.02(2) 11_577 9_667 ?
In3 In2 In2 115.022(19) 5_646 9_667 ?
In3 In2 In2 115.022(19) 6_466 9_667 ?
In3 In2 In3 95.69(2) 11_577 5_646 ?
In3 In2 In3 129.96(4) 11_577 12_757 ?
In3 In2 In3 129.96(4) 5_646 6_466 ?
In3 In2 In3 95.69(2) 12_757 6_466 ?
In3 In2 In3 62.805(19) 11_577 6_466 ?
In3 In2 In3 62.805(19) 5_646 12_757 ?
In4 In2 In2 56.91(2) 9_667 9_667 ?
In4 In2 In2 56.91(2) . 9_667 ?
In4 In2 In3 78.131(14) . 6_466 ?
In4 In2 In3 78.131(14) 9_667 11_577 ?
In4 In2 In3 78.131(14) . 12_757 ?
In4 In2 In3 131.871(10) . 5_646 ?
In4 In2 In3 131.871(10) 9_667 6_466 ?
In4 In2 In3 78.131(14) 9_667 5_646 ?
In4 In2 In3 131.871(10) 9_667 12_757 ?
In4 In2 In3 131.871(10) . 11_577 ?
In4 In2 In4 113.83(4) . 9_667 ?
In4 In2 In5 73.672(17) 9_667 11_577 ?
In4 In2 In5 73.672(17) . 11_577 ?
In4 In2 In5 73.672(17) . 3_645 ?
In4 In2 In5 73.672(17) 9_667 3_645 ?
In5 In2 In2 59.003(19) 3_645 9_667 ?
In5 In2 In2 59.003(19) 11_577 9_667 ?
In5 In2 In3 65.313(16) 11_577 6_466 ?
In5 In2 In3 148.574(10) 3_645 11_577 ?
In5 In2 In3 148.574(10) 11_577 5_646 ?
In5 In2 In3 65.313(16) 11_577 11_577 ?
In5 In2 In3 65.313(15) 3_645 12_757 ?
In5 In2 In3 148.573(10) 11_577 12_757 ?
In5 In2 In3 148.574(10) 3_645 6_466 ?
In5 In2 In3 65.313(15) 3_645 5_646 ?
In5 In2 In5 118.01(4) 11_577 3_645 ?
Ir1 In3 Ir1 147.55(2) 11_677 . ?
Ir1 In3 In1 129.06(2) . 11_677 ?
Ir1 In3 In1 55.301(16) 11_677 11_677 ?
Ir1 In3 In2 95.217(17) . 11_677 ?
Ir1 In3 In2 54.412(11) 11_677 11_677 ?
Ir1 In3 In3 54.296(18) 11_677 11_677 ?
Ir1 In3 In3 54.145(17) . 12_757 ?
Ir1 In3 In3 132.00(2) . 11_677 ?
Ir1 In3 In3 134.24(2) 11_677 12_757 ?
Ir1 In3 In4 146.59(3) 11_677 . ?
Ir1 In3 In4 51.336(17) . . ?
Ir1 In3 S1 108.149(17) . . ?
Ir1 In3 S1 104.214(18) 11_677 . ?
In1 In3 In2 68.03(2) 11_677 11_677 ?
In1 In3 In4 91.36(2) 11_677 . ?
In3 In3 In1 98.63(3) 11_677 11_677 ?
In3 In3 In1 161.73(3) 12_757 11_677 ?
In3 In3 In2 98.44(2) 11_677 11_677 ?
In3 In3 In2 129.99(3) 12_757 11_677 ?
In3 In3 In3 82.737(14) 11_677 12_757 ?
In3 In3 In4 146.30(2) 11_677 . ?
In3 In3 In4 78.27(2) 12_757 . ?
In4 In3 In2 115.11(2) . 11_677 ?
S1 In3 In1 85.83(2) . 11_677 ?
S1 In3 In2 152.58(2) . 11_677 ?
S1 In3 In3 76.718(16) . 11_677 ?
S1 In3 In3 76.718(16) . 12_757 ?
S1 In3 In4 71.993(15) . . ?
Ir1 In4 Ir1 177.89(5) . 10_557 ?
Ir1 In4 In2 124.14(4) . 9_667 ?
Ir1 In4 In2 124.14(4) 10_557 . ?
Ir1 In4 In2 57.97(2) . . ?
Ir1 In4 In2 57.97(2) 10_557 9_667 ?
Ir1 In4 In3 126.29(3) . 7_557 ?
Ir1 In4 In3 126.29(3) 10_557 16 ?
Ir1 In4 In3 52.128(15) . 16 ?
Ir1 In4 In3 126.29(3) 10_557 . ?
Ir1 In4 In3 52.128(15) . . ?
Ir1 In4 In3 126.29(3) . 10_557 ?
Ir1 In4 In3 52.129(15) 10_557 7_557 ?
Ir1 In4 In3 52.129(15) 10_557 10_557 ?
In2 In4 In2 66.17(4) . 9_667 ?
In2 In4 In3 146.186(18) . 7_557 ?
In2 In4 In3 146.186(18) . 10_557 ?
In2 In4 In3 99.93(2) 9_667 10_557 ?
In2 In4 In3 99.93(2) 9_667 7_557 ?
In2 In4 In3 99.93(2) . 16 ?
In2 In4 In3 99.93(2) . . ?
In2 In4 In3 146.186(18) 9_667 . ?
In2 In4 In3 146.186(18) 9_667 16 ?
In3 In4 In3 106.44(4) 7_557 . ?
In3 In4 In3 74.17(3) 10_557 . ?
In3 In4 In3 74.17(3) 7_557 16 ?
In3 In4 In3 63.63(2) 7_557 10_557 ?
In3 In4 In3 63.62(2) . 16 ?
In3 In4 In3 106.44(4) 10_557 16 ?
Ir1 In5 Ir1 113.93(4) . 10_556 ?
Ir1 In5 In2 154.03(3) . 3_654 ?
Ir1 In5 In2 92.04(2) 10_556 3_654 ?
Ir1 In5 In2 154.03(3) 10_556 11_677 ?
Ir1 In5 In2 92.04(2) . 11_677 ?
In1 In5 Ir1 56.97(2) . 10_556 ?
In1 In5 Ir1 56.97(2) . . ?
In1 In5 In2 149.00(2) . 11_677 ?
In1 In5 In2 149.00(2) . 3_654 ?
In2 In5 In2 61.99(4) 11_677 3_654 ?
In3 S1 In3 92.21(3) 10_557 9_767 ?
In3 S1 In3 92.21(3) 2_765 . ?
In3 S1 In3 180.0 9_767 . ?
In3 S1 In3 87.79(3) 2_765 9_767 ?
In3 S1 In3 180.0 10_557 2_765 ?
In3 S1 In3 87.79(3) 10_557 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 In1 2.7532(7) . ?
Ir1 In2 2.7993(6) . ?
Ir1 In3 2.6668(6) . ?
Ir1 In3 2.6618(6) 12_757 ?
Ir1 In3 2.6668(6) 16 ?
Ir1 In3 2.6618(6) 6_466 ?
Ir1 In4 2.6379(6) . ?
Ir1 In5 2.9016(8) . ?
In1 Ir1 2.7531(7) 10_556 ?
In1 In1 2.6843(19) 9_666 ?
In1 In3 3.1858(6) 6_466 ?
In1 In3 3.1858(6) 13_575 ?
In1 In3 3.1858(6) 12_757 ?
In1 In3 3.1858(6) 3_644 ?
In1 In5 2.8711(15) . ?
In2 Ir1 2.7992(6) 2_665 ?
In2 In2 3.366(2) 9_667 ?
In2 In3 3.3239(8) 6_466 ?
In2 In3 3.3239(8) 5_646 ?
In2 In3 3.3239(8) 11_577 ?
In2 In3 3.3239(8) 12_757 ?
In2 In4 3.0829(11) . ?
In2 In4 3.0829(11) 9_667 ?
In2 In5 3.2679(12) 11_577 ?
In2 In5 3.2679(12) 3_645 ?
In3 Ir1 2.6618(6) 11_677 ?
In3 In1 3.1857(6) 11_677 ?
In3 In2 3.3239(8) 11_677 ?
In3 In3 3.1156(9) 12_757 ?
In3 In3 3.1155(9) 11_677 ?
In3 In4 3.2855(9) . ?
In3 S1 2.8574(6) . ?
In4 Ir1 2.6379(6) 10_557 ?
In4 In2 3.0829(11) 9_667 ?
In4 In3 3.2855(9) 16 ?
In4 In3 3.2855(9) 10_557 ?
In4 In3 3.2855(9) 7_557 ?
In5 Ir1 2.9016(8) 10_556 ?
In5 In2 3.2680(12) 11_677 ?
In5 In2 3.2680(12) 3_654 ?
S1 In3 2.8574(6) 2_765 ?
S1 In3 2.8574(6) 9_767 ?
S1 In3 2.8574(6) 10_557 ?
