Polyoxometalate condensation and transformation mediated by adaptive coordination-assembled molecular flasks
Cai, Li-Xuan; Hu, Yu-Hang; Zhou, Li-Peng; Cheng, Pei-Ming; Guo, Xiao-Qing; Chan, Yi-Tsu; Sun, Qing-Fu; Chemical Science 16 (2025) 7956–7962; doi:10.1039/D4SC08729A

data_1574100
_publ_section_title
;
 Polyoxometalate condensation and transformation mediated by adaptive
 coordination-assembled molecular flasks
;
_journal_issue                   18
_journal_name_full               'Chemical Science'
_journal_page_first              7956
_journal_page_last               7962
_journal_paper_doi               10.1039/D4SC08729A
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C112 H128 N32 Pd4,  W10 O32, 8(N O3), 95.5(H2 O) '
_chemical_formula_sum            'C112 H319 N40 O151.5 Pd4 W10'
_chemical_formula_weight         6915.15
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-02-25 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   57.774(8)
_cell_length_b                   57.774(8)
_cell_length_c                   36.483(7)
_cell_measurement_reflns_used    241430
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.84
_cell_measurement_theta_min      0.39
_cell_volume                     121774(3)
_computing_cell_refinement       HKL-3000
_computing_data_collection       SSRF_BL17B
_computing_data_reduction        HKL-3000
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68875
_diffrn_reflns_av_R_equivalents  0.09
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       67
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31850
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        20.142
_diffrn_reflns_theta_max         20.142
_diffrn_reflns_theta_min         0.966
_diffrn_source                   'SSRF BL17B Beamline'
_exptl_absorpt_coefficient_mu    3.736
_exptl_absorpt_correction_T_max  0.7444
_exptl_absorpt_correction_T_min  0.4396
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       sheet
_exptl_crystal_F_000             54512
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.506
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1643
_refine_ls_number_reflns         31850
_refine_ls_number_restraints     1917
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0762
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2604
_refine_ls_wR_factor_ref         0.2908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20091
_reflns_number_total             31850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08729a3.cif
_cod_data_source_block           output_sq_s
_cod_depositor_comments
'Adding full bibliography for 1574099--1574101.cif.'
_cod_original_cell_volume        121774(42)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_original_formula_sum        'C112 H319 N40 O151.50 Pd4 W10'
_cod_database_code               1574100
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              87825
_shelx_fab_checksum              78893