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_1574101
_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, O40 Si W12, 8(N O3) , 50(H2 O) '
_chemical_formula_sum            'C112 H228 N40 O114 Pd4 Si W12'
_chemical_formula_weight         6619.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-02-24 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.8996(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   33.1786(3)
_cell_length_b                   35.0845(4)
_cell_length_c                   58.0136(6)
_cell_measurement_reflns_used    56816
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.6380
_cell_measurement_theta_min      2.0840
_cell_volume                     67530.9(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.961
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            96650
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        33.980
_diffrn_reflns_theta_max         33.980
_diffrn_reflns_theta_min         2.072
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    9.843
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.384
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_description       sheet
_exptl_crystal_F_000             38136
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         6.718
_refine_diff_density_min         -1.417
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     4877
_refine_ls_number_reflns         39350
_refine_ls_number_restraints     6195
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.1094
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3409
_refine_ls_wR_factor_ref         0.3538
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32879
_reflns_number_total             39350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08729a3.cif
_cod_data_source_block           p21n-a_sq_s
_cod_depositor_comments
'Adding full bibliography for 1574099--1574101.cif.'
_cod_original_cell_volume        67530.9(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1574101
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              16656
_shelx_fab_checksum              9486