Ligand-directed top-down synthesis of trivacant lacunary polyoxomolybdates from plenary Keggin-type [α-XMo<sub>12</sub>O<sub>40</sub>]<sup>3-</sup> (X = P, As, V) in organic media.
Jimbo, Atsuhiro; Li, Chifeng; Yonesato, Kentaro; Yamaguchi, Kazuya; Suzuki, Kosuke; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8234–8240; doi:10.1039/d5dt00252d

data_7718139
_publ_section_title
;
 Ligand-directed top-down synthesis of trivacant lacunary
 polyoxomolybdates from plenary Keggin-type
 [&#x3b1;-XMo<sub>12</sub>O<sub>40</sub>]<sup>3-</sup> (X = P, As, V) in
 organic media.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8234
_journal_page_last               8240
_journal_paper_doi               10.1039/d5dt00252d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_sum            'C92 H162 As Mo9 N7 O34'
_chemical_formula_weight         2848.66
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-12-05 deposited with the CCDC.	2025-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   19.4803(2)
_cell_length_b                   19.4803(2)
_cell_length_c                   51.6719(6)
_cell_measurement_reflns_used    39253
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.0720
_cell_measurement_theta_min      1.9700
_cell_volume                     16981.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.121a 64-bit (release 24-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            71913
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.986
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.329
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55714
_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            Colorless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             8676
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         8317
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0876P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7935
_reflns_number_total             8317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00252d2.cif
_cod_data_source_block           shelx_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7718136--7718141.cif.'
_cod_original_cell_volume        16981.5(4)
_cod_database_code               7718139
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.879
_shelx_estimated_absorpt_t_max   0.974
_oxdiff_exptl_absorpt_empirical_full_min 0.607
_oxdiff_exptl_absorpt_empirical_full_max 1.702
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_shelx_res_checksum              43956
_shelx_hkl_checksum              75620