Real-Time Tracking of Molecular Cluster Assembly and Precise Hierarchical Reassembly into Pure POM Host-Guest Architecture
Zhu, Kai-Ling; Li, Ke; Feng, Liubin; Yang, Le; Chen, Jiajia; Chemical Science  (2025) –; doi:10.1039/D5SC07121F

data_1576257
_publ_section_title
;
 Real-Time Tracking of Molecular Cluster Assembly and Precise Hierarchical
 Reassembly into Pure POM Host-Guest Architecture
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC07121F
_journal_year                    2025
_chemical_formula_moiety
'K52 Na14 O350 P8 W72, 3(O22.667 P0.667 W6), 16(O), 14[KH4O2]'
_chemical_formula_sum            'H56 K66 Na14 O462 P10 W90'
_chemical_formula_weight         27207.11
_chemical_name_systematic        {PW9}2@{PW9}8
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-07
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-07 deposited with the CCDC.	2025-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   29.9535(4)
_cell_length_b                   29.9535(4)
_cell_length_c                   29.9535(4)
_cell_measurement_reflns_used    7507
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.1300
_cell_measurement_theta_min      2.1220
_cell_volume                     26874.6(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_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    -44.00   0.00   0.50   22.60    --   -5.10 -38.00 118.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0089629000
_diffrn_orient_matrix_UB_12      -0.0206823000
_diffrn_orient_matrix_UB_13      -0.0072787000
_diffrn_orient_matrix_UB_21      -0.0117626000
_diffrn_orient_matrix_UB_22      -0.0111724000
_diffrn_orient_matrix_UB_23      0.0173006000
_diffrn_orient_matrix_UB_31      -0.0185087000
_diffrn_orient_matrix_UB_32      -0.0028595000
_diffrn_orient_matrix_UB_33      -0.0144199000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21042
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         1.665
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    19.826
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.362
_exptl_crystal_description       cube
_exptl_crystal_F_000             23940
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.387
_refine_diff_density_min         -2.994
_refine_diff_density_rms         0.535
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2919
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0904P)^2^+2597.0886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2349
_reflns_number_total             2919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07121f2.cif
_cod_data_source_block           compound-1
_cod_original_cell_volume        26874.6(11)
_cod_database_code               1576257
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'W9 P1 K12 O60 H40'
_cell_oxdiff_angle_alpha         89.845(2)
_cell_oxdiff_angle_beta          89.811(2)
_cell_oxdiff_angle_gamma         89.894(2)
_cell_oxdiff_length_a            29.9398(9)
_cell_oxdiff_length_b            29.9534(8)
_cell_oxdiff_length_c            29.9677(9)
_cell_oxdiff_measurement_reflns_used 7507
_cell_oxdiff_volume              26875(1)
_shelx_estimated_absorpt_t_max   0.383
_shelx_estimated_absorpt_t_min   0.383
_olex2_refinement_description
;
1. Shared sites
{K4, Na1}
2. Uiso/Uaniso restraints and constraints
O3 \\sim O5 \\sim O1 \\sim O4 \\sim O6 \\sim O7 \\sim O2 \\sim O13 \\sim O8
\\sim O9 \\sim O15 \\sim O11 \\sim O10 \\sim O16 \\sim O21 \\sim O19 \\sim O20
\\sim O17 \\sim O18 \\sim O12 \\sim O2W \\sim O1W \\sim O14: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
Uiso(K4) = Uiso(Na1)
3. Others
 Fixed Sof: W3(0.24933) W4(0.12567) P2(0.041667) K4(0.20834) O8(0.125)
 O10(0.25) O16(0.125) O21(0.23333) O19(0.46667) O20(0.11667) O17(0.25)
 O18(0.35) O12(0.125) Na1(0.29166) O2W(0.083333) O1W(0.25) O14(0.25)
;
_shelx_res_checksum              3297
_shelx_fab_checksum              90962
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.145
_oxdiff_exptl_absorpt_empirical_full_min 0.868