Crystal structure of bis(trimethylphenylammonium) aqua-oxido-octathiotritungstate, (Me3PhN)2[W3OS8(H2O)]
Kim, Kang-Woo; Kim, Sunghyeon; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 389–390; doi:10.1515/ncrs-2023-0027

data_8107449
_publ_section_title
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 Crystal structure of bis(trimethylphenylammonium)
 aqua-oxido-octathiotritungstate, (Me3PhN)2[W3OS8(H2O)]
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_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur 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       '\f and \w 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/[\s^2^(Fo^2^)+(0.0366P)^2^+16.1059P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_estimated_absorpt_t_min   0.149
_shelx_estimated_absorpt_t_max   0.592
_shelx_res_checksum              79162
_shelx_hkl_checksum              14934
_publcif_funding_html
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