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_1574881
_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         '1(O28 Se12 Si W12), 4(C24 H20 P), 2(C2 H3 N)'
_chemical_formula_sum            'C100 H86 N2 O28 P4 Se12 Si W12'
_chemical_formula_weight         5069.39
_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             2024-11-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-02 deposited with the CCDC.	2025-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                68.0094(7)
_cell_angle_beta                 68.5531(7)
_cell_angle_gamma                89.6202(6)
_cell_formula_units_Z            1
_cell_length_a                   13.76778(10)
_cell_length_b                   14.64503(10)
_cell_length_c                   17.18784(13)
_cell_measurement_reflns_used    67479
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.7130
_cell_measurement_theta_min      0.9210
_cell_volume                     2956.65(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'RAPID AUTO'
_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, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector
'PILATUS3 X CdTe 1M Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.809
_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      0.00 180.00   0.50    1.00    --    0.00  45.00   0.00  360
  2  \w      0.00 180.00   0.50    1.00    --    0.00  45.00 -90.00  360
  3  \w      0.00 180.00   0.50    1.00    --    0.00  45.00-180.00  360
  4  \w      0.00 180.00   0.50    1.00    --    0.00  45.00-270.00  360
;
_diffrn_measurement_device       'SPring-8 BL02B1'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0254840000
_diffrn_orient_matrix_UB_12      0.0150024000
_diffrn_orient_matrix_UB_13      -0.0242459000
_diffrn_orient_matrix_UB_21      0.0181559000
_diffrn_orient_matrix_UB_22      0.0008256000
_diffrn_orient_matrix_UB_23      0.0143285000
_diffrn_orient_matrix_UB_31      0.0091586000
_diffrn_orient_matrix_UB_32      -0.0268476000
_diffrn_orient_matrix_UB_33      -0.0002072000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.413
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.809
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            155649
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.755
_diffrn_reflns_theta_full        14.347
_diffrn_reflns_theta_max         21.855
_diffrn_reflns_theta_min         0.807
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    3.703
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75428
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.847
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2294
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.836
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.385(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1913
_refine_ls_number_reflns         54759
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.701
_reflns_number_gt                51551
_reflns_number_total             54759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03340c2.cif
_cod_data_source_block           III-Si
_cod_depositor_comments
'Adding full bibliography for 1574880--1574881.cif.'
_cod_database_code               1574881
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C64H144N4SiW12O28Se12
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.756
_shelx_res_checksum              37227
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.398
_oxdiff_exptl_absorpt_empirical_full_min 0.697