Isolation and characterization of a new polyoxometalate ligand, H<sub>3</sub>SbW<sub>14</sub>O<sub>50</sub><sup>10-</sup>, and its interactions with f-elements.
Colliard, Ian; Deblonde, Gauthier J.-P.; Chemical communications (Cambridge, England) 61 (2025) 941–944; doi:10.1039/d4cc05558f

data_7134043
_publ_section_title
;
 Isolation and characterization of a new polyoxometalate ligand,
 H<sub>3</sub>SbW<sub>14</sub>O<sub>50</sub><sup>10-</sup>, and its
 interactions with f-elements.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              941
_journal_page_last               944
_journal_paper_doi               10.1039/d4cc05558f
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'H3 O50 Sb W14, 10(Cs), 3(O)'
_chemical_formula_sum            'Cs10 H3 O53 Sb W14'
_chemical_formula_weight         4875.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-05-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-07 deposited with the CCDC.	2024-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2565(5)
_cell_length_b                   18.2879(5)
_cell_length_c                   22.2320(6)
_cell_measurement_reflns_used    28428
_cell_measurement_temperature    298
_cell_measurement_theta_max      31.7790
_cell_measurement_theta_min      3.6940
_cell_volume                     6609.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.00
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.883
_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    -69.00 -17.00   0.50    9.00    --    3.37 -60.00 -49.00  104
  2  \w    -16.00  71.00   0.50    9.00    --    3.37  60.00  90.00  174
  3  \w    -11.00  40.00   0.50    9.00    --    3.37 -99.00-120.00  102
  4  \w    -12.00  37.00   0.50    9.00    --    3.37 -99.00 150.00   98
  5  \w    -11.00  40.00   0.50    9.00    --    3.37 -99.00 -60.00  102
  6  \w    -12.00  35.00   0.50    9.00    --    3.37 -99.00-180.00   94
  7  \w      4.00  40.00   0.50    9.00    --    3.37 -99.00 -30.00   72
  8  \w      9.00  34.00   0.50    9.00    --    3.37  19.00   0.00   50
  9  \w     58.00  83.00   0.50    9.00    --    3.37  19.00   0.00   50
 10  \w     12.00  37.00   0.50    9.00    --    3.37  57.00  90.00   50
 11  \w     -2.00  23.00   0.50    9.00    --    3.37 -60.00 -49.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            108623
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.931
_diffrn_reflns_theta_min         3.465
_exptl_absorpt_coefficient_mu    30.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.898
_exptl_crystal_description       needle
_exptl_crystal_F_000             8248
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.674
_refine_diff_density_min         -5.283
_refine_diff_density_rms         0.500
_refine_ls_abs_structure_details
;
 Flack x determined using 6493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.183(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         19244
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0763P)^2^+108.1264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.795
_reflns_number_gt                16504
_reflns_number_total             19244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc05558f2.cif
_cod_data_source_block           sbw14-cs
_cod_depositor_comments          'Adding full bibliography for 7134043.cif.'
_cod_database_code               7134043
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.752
_shelx_estimated_absorpt_t_min   0.314
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: Cs9(0.25) Cs5(0.25) Cs11(0.25) Cs3(0.25)
3.a Ternary CH refined with riding coordinates:
 O8(H8)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              50605
_shelx_hkl_checksum              91690
_shelx_fab_checksum              94457
_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
;