Synthesis of a Keggin-type polyoxoselenidotungstate <i>via</i> site-selective oxygen-to-selenium substitution.
Yonesato, Kentaro; Watanabe, Yota; Pascual-Borràs, Magda; Errington, R. John; Yamaguchi, Kazuya; Suzuki, Kosuke; Chemical science 16 (2025) 13183–13188; doi:10.1039/d5sc03340c

data_1574880
_publ_section_title
;
 Synthesis of a Keggin-type polyoxoselenidotungstate <i>via</i>
 site-selective oxygen-to-selenium substitution.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              13183
_journal_page_last               13188
_journal_paper_doi               10.1039/d5sc03340c
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'O40 Si1 W12, 4(C24 H20 P), 4(C2 H3 N)'
_chemical_formula_sum            'C104 H92 N4 O40 P4 Si W12'
_chemical_formula_weight         4395.98
_chemical_name_systematic        I-Si
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7181)
;
_audit_update_record
;
2025-04-02 deposited with the CCDC.	2025-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                112.3714(8)
_cell_angle_beta                 104.2936(7)
_cell_angle_gamma                100.2025(7)
_cell_formula_units_Z            1
_cell_length_a                   13.90582(11)
_cell_length_b                   15.07813(13)
_cell_length_c                   15.90307(14)
_cell_measurement_reflns_used    71292
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      38.9020
_cell_measurement_theta_min      2.1920
_cell_volume                     2848.02(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 44.93a 64-bit (release 10-02-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      178(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -29.00  -3.00   0.50    0.50    --   26.00 -92.00 -36.55   52
  2  \w      4.00  55.00   0.50    0.50    --   26.00 -92.00 -36.55  102
  3  \w     27.00  83.00   0.50    0.50    --   26.00-142.00 -19.23  112
  4  \w    -38.00  52.00   0.50    0.50    --   26.00 -86.00  62.82  180
  5  \w    -38.00 -11.00   0.50    0.50    --   26.00 -90.00 145.32   54
  6  \w      6.00  57.00   0.50    0.50    --   24.14-101.00 108.68  102
  7  \w     -8.00  54.00   0.50    0.50    --   26.00 -90.00 145.32  124
  8  \w    -45.00  38.00   0.50    0.50    --   24.14 -58.00 159.00  166
  9  \w     12.00  95.00   0.50    0.50    --   24.14  58.00 -59.00  166
 10  \w    -33.00  52.00   0.50    0.50    --   26.00 -87.00-115.52  170
 11  \w    -94.00  -2.00   0.50    0.50    --  -22.82 -77.00 -60.00  184
 12  \w    -71.00 -11.00   0.50    0.50    --  -22.82 -57.00 -30.00  120
 13  \w    -95.00 -28.00   0.50    0.50    --  -22.82 -57.00  30.00  134
 14  \w    -95.00 -24.00   0.50    0.50    --  -22.82 -38.00  90.00  142
 15  \w    -94.00 -13.00   0.50    0.50    --  -22.82 -19.00 150.00  162
 16  \w    -85.00  -9.00   0.50    0.50    --  -22.82 -58.00 159.00  152
 17  \w    -94.00  -1.00   0.50    0.50    --  -22.82 -77.00  90.00  186
 18  \w     -2.00  42.00   0.50    0.50    --  -22.82  58.00 -59.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0243753000
_diffrn_orient_matrix_UB_12      0.0350127000
_diffrn_orient_matrix_UB_13      0.0227576000
_diffrn_orient_matrix_UB_21      -0.0101385000
_diffrn_orient_matrix_UB_22      -0.0263467000
_diffrn_orient_matrix_UB_23      0.0270587000
_diffrn_orient_matrix_UB_31      0.0485058000
_diffrn_orient_matrix_UB_32      0.0304705000
_diffrn_orient_matrix_UB_33      0.0372990000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            148727
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.318
_diffrn_reflns_theta_min         1.842
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.563
_exptl_crystal_description       block
_exptl_crystal_F_000             2026
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.139
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.251(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1969
_refine_ls_number_reflns         54553
_refine_ls_number_restraints     841
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0157P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0518
_reflns_Friedel_coverage         0.978
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                47155
_reflns_number_total             54553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03340c2.cif
_cod_data_source_block           I-Si
_cod_depositor_comments
'Adding full bibliography for 1574880--1574881.cif.'
_cod_database_code               1574880
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C104H92N4P4SiW12O40
_shelx_estimated_absorpt_t_max   0.442
_shelx_estimated_absorpt_t_min   0.442
_shelx_res_checksum              80796
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.904
_oxdiff_exptl_absorpt_empirical_full_min 0.769