#------------------------------------------------------------------------------
#$Date: 2019-11-26 06:00:13 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242777 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/29/4132902.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_4132902
loop_
_publ_author_name
'Yang, Huajun'
'Zhang, Jiaxu'
'Luo, Min'
'Wang, Wei'
'Lin, Haiping'
'Li, Youyong'
'Li, Dongsheng'
'Feng, Pingyun'
'Wu, Tao'
_publ_section_title
;
 The Largest Supertetrahedral Oxychalcogenide Nanocluster and Its Unique
 Assembly.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11189
_journal_page_last               11192
_journal_paper_doi               10.1021/jacs.8b07349
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C9 H3 Fe12 In48 N0 O15 S93'
_chemical_formula_weight         9514.26
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   37.421(3)
_cell_length_b                   37.421(3)
_cell_length_c                   20.6962(17)
_cell_measurement_reflns_used    6702
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      17.369
_cell_measurement_theta_min      2.336
_cell_volume                     25099(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CPAD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            5459
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        17.447
_diffrn_reflns_theta_max         17.447
_diffrn_reflns_theta_min         2.266
_exptl_absorpt_coefficient_mu    2.886
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       rod
_exptl_crystal_F_000             20385
_platon_squeeze_details
;
;
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5459
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0792
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2633
_reflns_number_total             5459
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b07349_si_007.cif
_cod_data_source_block           FIS-1
_cod_database_code               4132902
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
S1 S 0.3600(2) 0.3855(2) 0.2500 0.158(4) Uani 1 2 d S T P
C1 C 0.6301(7) 0.3290(8) 0.2500 0.129(13) Uani 1 2 d S TU P
In1 In 0.30008(7) 0.39615(8) 0.44136(19) 0.300(2) Uani 1 1 d . . .
O1 O 0.5903(5) 0.3610(6) 0.2500 0.210(13) Uani 1 2 d DS T P
Fe1 Fe 0.39973(8) 0.41689(8) 0.34564(18) 0.1311(14) Uani 1 1 d . . .
C2 C 0.6628(8) 0.3665(6) 0.2500 0.157(16) Uani 1 2 d S TU P
H2A H 0.6598 0.3903 0.2500 0.188 Uiso 1 2 calc R U P
S2 S 0.45969(15) 0.41023(15) 0.3498(4) 0.180(4) Uani 1 1 d . . .
O2 O 0.2051(6) 0.2618(7) 0.6226(10) 0.307(12) Uani 1 1 d D U .
Fe2 Fe 0.30043(13) 0.39447(15) 0.2500 0.179(3) Uani 1 2 d S T P
In2 In 0.42380(17) 0.59407(12) 0.2500 0.408(4) Uani 1 2 d DS TU P
S3 S 0.3946(2) 0.3029(2) 0.2500 0.153(4) Uani 1 2 d S T P
In3 In 0.52763(6) 0.35621(6) 0.2500 0.1862(16) Uani 1 2 d DS T P
O3 O 0.5563(5) 0.2917(6) 0.2500 0.194(12) Uani 1 2 d S T P
Fe3 Fe 0.33651(9) 0.31302(10) 0.2500 0.1090(17) Uani 1 2 d S T P
S4 S 0.49519(18) 0.3249(2) 0.3488(4) 0.187(4) Uani 1 1 d . . .
In4 In 0.24051(8) 0.29339(11) 0.5257(2) 0.329(2) Uani 1 1 d D . .
O4 O 0.4436(9) 0.6655(6) 0.2500 0.41(3) Uani 1 2 d DS TU P
C4 C 0.5851(9) 0.3246(10) 0.2500 0.122(10) Uani 1 2 d S TU P
S5 S 0.5608(2) 0.4317(2) 0.2500 0.203(6) Uani 1 2 d S T P
S6 S 0.4889(4) 0.5943(3) 0.2500 0.367(12) Uani 1 2 d S T P
In6 In 0.23466(6) 0.28900(8) 0.34332(16) 0.2637(17) Uani 1 1 d . . .
S7 S 0.3620(2) 0.3871(2) 0.4391(5) 0.214(4) Uani 1 1 d . . .
In7 In 0.33703(6) 0.31131(6) 0.44103(14) 0.2172(13) Uani 1 1 d . . .
In09 In 0.36251(8) 0.49833(8) 0.3473(2) 0.317(2) Uani 1 1 d . . .
S9 S 0.5270(3) 0.5150(2) 0.2500 0.247(7) Uani 1 2 d S T P
In9 In 0.50139(6) 0.44154(6) 0.2500 0.1903(16) Uani 1 2 d S T P
S8 S 0.3965(2) 0.3016(2) 0.4416(4) 0.193(4) Uani 1 1 d . . .
In8 In 0.43612(4) 0.33495(5) 0.34828(11) 0.1731(11) Uani 1 1 d . . .
S14 S 0.1924(3) 0.2544(4) 0.4335(8) 0.370(8) Uani 1 1 d . . .
S13 S 0.4252(2) 0.49003(19) 0.3470(5) 0.213(5) Uani 1 1 d . . .
S15 S 0.2952(3) 0.2785(3) 0.5350(6) 0.280(5) Uani 1 1 d . . .
S16 S 0.2582(2) 0.3644(3) 0.3406(5) 0.251(5) Uani 1 1 d . . .
S17 S 0.1916(3) 0.2564(4) 0.2500 0.292(8) Uani 1 2 d S T P
S18 S 0.29516(18) 0.27866(19) 0.3415(4) 0.189(4) Uani 1 1 d . . .
S19 S 0.3832(4) 0.5697(3) 0.3494(8) 0.394(10) Uani 1 1 d . . .
S12 S 0.2598(3) 0.3669(4) 0.5339(7) 0.358(8) Uani 1 1 d . . .
S11 S 0.3185(3) 0.4642(4) 0.2500 0.278(8) Uani 1 2 d S T P
S10 S 0.3232(3) 0.4695(3) 0.0604(7) 0.337(8) Uani 1 1 d . . .
In10 In 0.46622(9) 0.52214(8) 0.2500 0.243(2) Uani 1 2 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
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'
N N 0.0061 0.0033 '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'
S S 0.1246 0.1234 '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'
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
Fe3 S1 Fe1 109.91(19) . 10_556
Fe3 S1 Fe1 109.91(19) . .
Fe1 S1 Fe1 111.0(3) 10_556 .
Fe3 S1 Fe2 108.5(3) . .
Fe1 S1 Fe2 108.73(19) 10_556 .
Fe1 S1 Fe2 108.73(19) . .
C2 C1 C2 122(2) 2_655 .
C2 C1 C4 120(2) 2_655 .
C2 C1 C4 118(2) . .
S12 In1 S10 108.8(5) . 10_556
S12 In1 S7 112.0(4) . .
S10 In1 S7 108.7(3) 10_556 .
S12 In1 S16 110.7(4) . .
S10 In1 S16 107.8(4) 10_556 .
S7 In1 S16 108.7(3) . .
C4 O1 In3 108.3(18) . .
S7 Fe1 S2 107.4(3) . .
S7 Fe1 S1 111.8(3) . .
S2 Fe1 S1 111.4(3) . .
S7 Fe1 S13 109.6(3) . .
S2 Fe1 S13 105.1(2) . .
S1 Fe1 S13 111.3(3) . .
C1 C2 C1 118(2) 3_665 .
C1 C2 H2A 121.0 3_665 .
C1 C2 H2A 121.0 . .
Fe1 S2 In8 107.3(2) . .
Fe1 S2 In9 108.8(3) . .
In8 S2 In9 107.7(3) . .
S16 Fe2 S16 106.1(5) . 10_556
S16 Fe2 S11 106.5(3) . .
S16 Fe2 S11 106.5(3) 10_556 .
S16 Fe2 S1 112.4(2) . .
S16 Fe2 S1 112.4(2) 10_556 .
S11 Fe2 S1 112.5(3) . .
O4 In2 S6 104.2(8) . .
O4 In2 S19 101.8(4) . .
S6 In2 S19 115.8(3) . .
O4 In2 S19 101.8(4) . 10_556
S6 In2 S19 115.8(3) . 10_556
S19 In2 S19 114.5(7) . 10_556
Fe3 S3 In8 108.86(19) . .
Fe3 S3 In8 108.87(19) . 10_556
In8 S3 In8 110.5(3) . 10_556
O1 In3 S4 107.1(3) . 10_556
O1 In3 S4 107.1(3) . .
S4 In3 S4 119.4(3) 10_556 .
O1 In3 S5 90.0(5) . .
S4 In3 S5 114.16(18) 10_556 .
S4 In3 S5 114.16(18) . .
S18 Fe3 S18 105.7(3) 10_556 .
S18 Fe3 S3 108.2(2) 10_556 .
S18 Fe3 S3 108.2(2) . .
S18 Fe3 S1 112.5(2) 10_556 .
S18 Fe3 S1 112.5(2) . .
S3 Fe3 S1 109.4(3) . .
In3 S4 In8 101.6(3) . .
O2 In4 S15 98.4(5) . .
O2 In4 S12 106.0(7) . .
S15 In4 S12 116.5(3) . .
O2 In4 S14 106.9(6) . .
S15 In4 S14 111.9(4) . .
S12 In4 S14 115.0(5) . .
O3 C4 O1 134(3) . .
O3 C4 C1 118(3) . .
O1 C4 C1 107(2) . .
In9 S5 In3 101.6(3) . .
In10 S6 In2 101.9(5) . .
S14 In6 S17 105.0(4) . .
S14 In6 S18 109.8(4) . .
S17 In6 S18 109.8(3) . .
S14 In6 S16 113.4(4) . .
S17 In6 S16 108.7(4) . .
S18 In6 S16 110.0(2) . .
Fe1 S7 In1 109.4(4) . .
Fe1 S7 In7 110.5(3) . .
In1 S7 In7 107.8(3) . .
S15 In7 S8 109.3(3) . .
S15 In7 S18 109.0(3) . .
S8 In7 S18 109.1(3) . .
S15 In7 S7 111.7(3) . .
S8 In7 S7 108.6(2) . .
S18 In7 S7 109.1(3) . .
S10 In09 S19 106.3(4) 10_556 .
S10 In09 S11 108.8(4) 10_556 .
S19 In09 S11 110.4(5) . .
S10 In09 S13 111.0(3) 10_556 .
S19 In09 S13 109.7(3) . .
S11 In09 S13 110.6(3) . .
In9 S9 In10 105.4(3) . .
S9 In9 S5 107.5(3) . .
S9 In9 S2 109.43(16) . .
S5 In9 S2 109.47(16) . .
S9 In9 S2 109.43(16) . 10_556
S5 In9 S2 109.48(16) . 10_556
S2 In9 S2 111.5(3) . 10_556
In8 S8 In7 107.1(3) . .
S8 In8 S4 107.0(3) . .
S8 In8 S3 109.8(2) . .
S4 In8 S3 109.2(2) . .
S8 In8 S2 111.1(2) . .
S4 In8 S2 109.9(2) . .
S3 In8 S2 109.9(2) . .
In6 S14 In4 101.0(4) . .
Fe1 S13 In10 110.1(3) . .
Fe1 S13 In09 106.1(3) . .
In10 S13 In09 109.6(3) . .
In4 S15 In7 103.3(4) . .
Fe2 S16 In6 109.4(4) . .
Fe2 S16 In1 108.9(3) . .
In6 S16 In1 107.3(4) . .
In6 S17 In6 106.0(4) . 10_556
Fe3 S18 In6 109.0(3) . .
Fe3 S18 In7 108.2(2) . .
In6 S18 In7 108.0(3) . .
In09 S19 In2 101.3(5) . .
In1 S12 In4 103.0(5) . .
Fe2 S11 In09 108.5(2) . .
Fe2 S11 In09 108.5(2) . 10_556
In09 S11 In09 106.7(5) . 10_556
In09 S10 In1 108.7(4) 10_556 10_556
S6 In10 S9 107.6(4) . .
S6 In10 S13 109.6(2) . .
S9 In10 S13 109.83(18) . .
S6 In10 S13 109.6(2) . 10_556
S9 In10 S13 109.83(18) . 10_556
S13 In10 S13 110.3(4) . 10_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 Fe3 2.396(8) .
S1 Fe1 2.401(5) 10_556
S1 Fe1 2.401(5) .
S1 Fe2 2.413(7) .
C1 C2 1.29(2) 2_655
C1 C2 1.32(2) .
C1 C4 1.61(3) .
In1 S12 2.343(14) .
In1 S10 2.432(10) 10_556
In1 S7 2.504(6) .
In1 S16 2.521(10) .
O1 C4 1.28(3) .
O1 In3 2.261(14) .
Fe1 S7 2.323(9) .
Fe1 S2 2.380(5) .
Fe1 S13 2.407(6) .
C2 C1 1.29(2) 3_665
C2 H2A 0.9500 .
S2 In8 2.496(5) .
S2 In9 2.499(8) .
O2 In4 2.369(17) .
Fe2 S16 2.345(10) .
Fe2 S16 2.346(10) 10_556
Fe2 S11 2.346(12) .
In2 O4 2.391(17) .
In2 S6 2.433(14) .
In2 S19 2.446(16) .
In2 S19 2.446(16) 10_556
S3 Fe3 2.387(7) .
S3 In8 2.475(4) .
S3 In8 2.475(4) 10_556
In3 S4 2.367(8) 10_556
In3 S4 2.367(8) .
In3 S5 2.453(8) .
O3 C4 1.16(3) .
Fe3 S18 2.376(8) 10_556
Fe3 S18 2.376(8) .
S4 In8 2.421(5) .
In4 S15 2.382(10) .
In4 S12 2.475(12) .
In4 S14 2.526(14) .
S5 In9 2.427(7) .
S6 In10 2.392(10) .
In6 S14 2.371(13) .
In6 S17 2.418(7) .
In6 S18 2.480(7) .
In6 S16 2.501(10) .
S7 In7 2.505(7) .
In7 S15 2.412(10) .
In7 S8 2.429(6) .
In7 S18 2.505(8) .
In09 S10 2.322(14) 10_556
In09 S19 2.381(9) .
In09 S11 2.508(7) .
In09 S13 2.516(6) .
S9 In9 2.417(7) .
S9 In10 2.418(8) .
In9 S2 2.499(8) 10_556
S8 In8 2.375(9) .
S13 In10 2.447(9) .
S17 In6 2.418(7) 10_556
S11 In09 2.508(7) 10_556
S10 In09 2.322(14) 10_556
S10 In1 2.433(10) 10_556
In10 S13 2.447(9) 10_556
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.007 -0.004 -0.003 17353 4934 ' '
