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_1574099
_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 N40 Pd4, (O40 Si Mo12), 8(N O3), 74 (H2 O)'
_chemical_formula_sum            'C112 H276 Mo12 N40 O138 Pd4 Si'
_chemical_formula_weight         5996.68
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   55.438(4)
_cell_length_b                   55.438(4)
_cell_length_c                   34.467(2)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.45
_cell_measurement_theta_min      2.20
_cell_volume                     91738(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1551
_diffrn_reflns_av_unetI/netI     0.1007
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            284618
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        17.999
_diffrn_reflns_theta_max         17.999
_diffrn_reflns_theta_min         2.182
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5834
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       block
_exptl_crystal_F_000             54612
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.333
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.57(8)
_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     4560
_refine_ls_number_reflns         41961
_refine_ls_number_restraints     11704
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.0935
_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^)+(0.1492P)^2^+1609.0101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2345
_refine_ls_wR_factor_ref         0.2746
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                27259
_reflns_number_total             41961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08729a2.cif
_cod_data_source_block           p63_sq
_cod_depositor_comments
'Adding full bibliography for 1574099--1574101.cif.'
_cod_original_cell_volume        91736(13)
_cod_database_code               1574099
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              77625
_shelx_hkl_checksum              62027
_shelx_fab_checksum              8261