#------------------------------------------------------------------------------
#$Date: 2023-07-10 11:54:09 +0300 (Mon, 10 Jul 2023) $
#$Revision: 285115 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/74/8107449.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_8107449
loop_
_publ_author_name
'Kim, Kang-Woo'
'Kim, Sunghyeon'
_publ_section_title
;
 Crystal structure of bis(trimethylphenylammonium)
 aqua-oxido-octathiotritungstate, (Me3PhN)2[W3OS8(H2O)]
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              389
_journal_page_last               390
_journal_paper_doi               10.1515/ncrs-2023-0027
_journal_volume                  238
_journal_year                    2023
_chemical_formula_sum            'C18 H30 N2 O2 S8 W3'
_chemical_formula_weight         1114.47
_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   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0254(13)
_cell_length_b                   15.2534(10)
_cell_length_c                   11.8789(9)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.48
_cell_volume                     3084.9(4)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2012)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2012)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2012)'
_computing_molecular_graphics    'Diamond 4.6 (Brandenburg, 2015)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  SHELXL-2019/2
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26108
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.339
_diffrn_reflns_theta_min         2.393
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    11.720
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.2835
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.400
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.050
_refine_diff_density_max         5.510
_refine_diff_density_min         -2.381
_refine_diff_density_rms         0.373
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         3972
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0342
_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)+(0.0366P)²+16.1059P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3521
_reflns_number_total             3972
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0027_suppl.cif
_cod_data_source_block           (PhMe3N)2[W3OS8(H2O)]
_cod_database_code               8107449
_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.
;
_shelx_estimated_absorpt_t_min   0.149
_shelx_estimated_absorpt_t_max   0.592
_publcif_funding_html
;
;
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
W1 W 0.46330(2) 0.750000 0.49610(3) 0.02793(9) Uani 1 2 d S T P . .
W2 W 0.59309(2) 0.750000 0.66154(3) 0.03030(10) Uani 1 2 d S T P . .
W3 W 0.37085(2) 0.750000 0.28474(3) 0.03769(11) Uani 1 2 d S T P . .
S1 S 0.54165(9) 0.63188(9) 0.57475(13) 0.0338(3) Uani 1 1 d . . . . .
S2 S 0.42154(10) 0.63197(10) 0.37335(13) 0.0360(3) Uani 1 1 d . . . . .
S3 S 0.56166(18) 0.750000 0.8372(2) 0.0477(6) Uani 1 2 d S T P . .
S4 S 0.71846(16) 0.750000 0.6402(3) 0.0509(6) Uani 1 2 d S T P . .
S5 S 0.2443(2) 0.750000 0.2966(3) 0.0708(9) Uani 1 2 d S T P . .
S6 S 0.4089(2) 0.750000 0.1126(2) 0.0682(9) Uani 1 2 d S T P . .
O1 O 0.3868(4) 0.750000 0.5898(5) 0.0384(14) Uani 1 2 d S T P . .
O2 O 0.5754(8) 0.750000 0.3583(9) 0.083(3) Uani 1 2 d DS T P . .
H2W H 0.587(7) 0.7943(13) 0.321(6) 0.125 Uiso 1 1 d D U . . .
N1 N 0.2213(4) 0.5250(4) 0.5778(4) 0.0405(12) Uani 1 1 d . . . . .
C1 C 0.1646(4) 0.5118(4) 0.4834(5) 0.0385(14) Uani 1 1 d . . . . .
C2 C 0.1579(5) 0.4309(5) 0.4328(8) 0.060(2) Uani 1 1 d . . . . .
H2 H 0.190023 0.384154 0.455949 0.072 Uiso 1 1 calc R U . . .
C3 C 0.1034(6) 0.4187(7) 0.3474(9) 0.074(3) Uani 1 1 d . . . . .
H3 H 0.099155 0.363888 0.311695 0.088 Uiso 1 1 calc R U . . .
C4 C 0.0563(6) 0.4856(7) 0.3157(8) 0.070(3) Uani 1 1 d . . . . .
H4 H 0.019440 0.477068 0.257812 0.083 Uiso 1 1 calc R U . . .
C5 C 0.0617(6) 0.5641(7) 0.3662(8) 0.078(3) Uani 1 1 d . . . . .
H5 H 0.028100 0.609860 0.343901 0.094 Uiso 1 1 calc R U . . .
C6 C 0.1162(6) 0.5785(6) 0.4509(8) 0.067(2) Uani 1 1 d . . . . .
H6 H 0.119856 0.633742 0.485584 0.081 Uiso 1 1 calc R U . . .
C7 C 0.1786(6) 0.5098(6) 0.6873(6) 0.071(3) Uani 1 1 d . . . . .
H7A H 0.134549 0.550006 0.692709 0.106 Uiso 1 1 calc R U . . .
H7B H 0.214189 0.519804 0.749704 0.106 Uiso 1 1 calc R U . . .
H7C H 0.159427 0.449965 0.689881 0.106 Uiso 1 1 calc R U . . .
C8 C 0.2532(5) 0.6171(5) 0.5807(7) 0.0529(19) Uani 1 1 d . . . . .
H8A H 0.276571 0.631189 0.508490 0.079 Uiso 1 1 calc R U . . .
H8B H 0.292748 0.621692 0.639237 0.079 Uiso 1 1 calc R U . . .
H8C H 0.210814 0.657847 0.596393 0.079 Uiso 1 1 calc R U . . .
C9 C 0.2903(6) 0.4645(7) 0.5694(10) 0.089(4) Uani 1 1 d . . . . .
H9A H 0.272783 0.404367 0.578566 0.134 Uiso 1 1 calc R U . . .
H9B H 0.327932 0.478605 0.628025 0.134 Uiso 1 1 calc R U . . .
H9C H 0.314951 0.471202 0.496326 0.134 Uiso 1 1 calc R U . . .
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'
W W -0.8490 6.8722 '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
O1 W1 S2 99.68(15) . 7_575
O1 W1 S2 99.68(15) . .
S2 W1 S2 95.96(8) 7_575 .
O1 W1 S1 99.64(15) . 7_575
S2 W1 S1 80.88(5) 7_575 7_575
S2 W1 S1 160.68(6) . 7_575
O1 W1 S1 99.64(15) . .
S2 W1 S1 160.68(6) 7_575 .
S2 W1 S1 80.88(5) . .
S1 W1 S1 95.78(7) 7_575 .
O1 W1 O2 179.9(4) . .
S2 W1 O2 80.3(2) 7_575 .
S2 W1 O2 80.3(2) . .
S1 W1 O2 80.4(2) 7_575 .
S1 W1 O2 80.4(2) . .
O1 W1 W2 97.8(2) . .
S2 W1 W2 128.25(4) 7_575 .
S2 W1 W2 128.25(4) . .
S1 W1 W2 48.24(4) 7_575 .
S1 W1 W2 48.24(4) . .
O2 W1 W2 82.3(3) . .
O1 W1 W3 98.5(2) . .
S2 W1 W3 48.27(4) 7_575 .
S2 W1 W3 48.27(4) . .
S1 W1 W3 128.15(4) 7_575 .
S1 W1 W3 128.15(4) . .
O2 W1 W3 81.5(3) . .
W2 W1 W3 163.731(17) . .
S4 W2 S3 111.15(12) . .
S4 W2 S1 109.40(6) . 7_575
S3 W2 S1 110.29(6) . 7_575
S4 W2 S1 109.39(6) . .
S3 W2 S1 110.29(6) . .
S1 W2 S1 106.20(8) 7_575 .
S4 W2 W1 131.58(8) . .
S3 W2 W1 117.26(8) . .
S1 W2 W1 53.52(4) 7_575 .
S1 W2 W1 53.52(4) . .
S6 W3 S5 111.32(15) . .
S6 W3 S2 109.21(7) . 7_575
S5 W3 S2 110.56(7) . 7_575
S6 W3 S2 109.21(7) . .
S5 W3 S2 110.56(7) . .
S2 W3 S2 105.81(8) 7_575 .
S6 W3 W1 130.33(11) . .
S5 W3 W1 118.35(10) . .
S2 W3 W1 53.25(4) 7_575 .
S2 W3 W1 53.25(4) . .
W2 S1 W1 78.25(5) . .
W3 S2 W1 78.47(5) . .
W1 O2 H2W 122(6) . .
W1 O2 H2W 122(6) . 7_575
H2W O2 H2W 108(6) . 7_575
C1 N1 C9 112.0(6) . .
C1 N1 C8 112.1(5) . .
C9 N1 C8 107.1(7) . .
C1 N1 C7 108.4(6) . .
C9 N1 C7 110.0(7) . .
C8 N1 C7 107.3(6) . .
C6 C1 C2 119.6(8) . .
C6 C1 N1 120.1(6) . .
C2 C1 N1 120.2(7) . .
C1 C2 C3 119.7(8) . .
C1 C2 H2 120.1 . .
C3 C2 H2 120.1 . .
C4 C3 C2 120.0(8) . .
C4 C3 H3 120.0 . .
C2 C3 H3 120.0 . .
C5 C4 C3 120.6(9) . .
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
C4 C5 C6 120.7(9) . .
C4 C5 H5 119.6 . .
C6 C5 H5 119.6 . .
C1 C6 C5 119.4(8) . .
C1 C6 H6 120.3 . .
C5 C6 H6 120.3 . .
N1 C7 H7A 109.5 . .
N1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N1 C8 H8A 109.5 . .
N1 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N1 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N1 C9 H9A 109.5 . .
N1 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N1 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 1.713(6) .
W1 S2 2.4233(15) 7_575
W1 S2 2.4234(15) .
W1 S1 2.4287(15) 7_575
W1 S1 2.4288(15) .
W1 O2 2.515(11) .
W1 W2 2.9574(5) .
W1 W3 2.9633(5) .
W2 S4 2.149(3) .
W2 S3 2.154(2) .
W2 S1 2.2531(15) 7_575
W2 S1 2.2531(15) .
W3 S6 2.145(3) .
W3 S5 2.158(4) .
W3 S2 2.2570(16) 7_575
W3 S2 2.2570(16) .
O2 H2W 0.83(2) .
O2 H2W 0.83(2) 7_575
N1 C1 1.493(9) .
N1 C9 1.497(10) .
N1 C8 1.508(9) .
N1 C7 1.508(9) .
C1 C6 1.366(10) .
C1 C2 1.378(10) .
C2 C3 1.387(13) .
C2 H2 0.9400 .
C3 C4 1.351(14) .
C3 H3 0.9400 .
C4 C5 1.343(13) .
C4 H4 0.9400 .
C5 C6 1.386(12) .
C5 H5 0.9400 .
C6 H6 0.9400 .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C7 H7C 0.9700 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C8 H8C 0.9700 .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C9 H9C 0.9700 .
