Evolution from [Zn<sub>9</sub>] to a record-high [Zn<sub>54</sub>] subblock and engineering a hierarchical supramolecular framework for enhanced iodine uptake.
Tao, Ye; Dong, Qiubing; Wan, Jingmeng; Huang, Fu-Ping; Duan, Jingui; Zeng, Ming-Hua; Chemical science 16 (2025) 1730–1736; doi:10.1039/d4sc04474f

data_1573449
_publ_section_title
;
 Evolution from [Zn<sub>9</sub>] to a record-high [Zn<sub>54</sub>]
 subblock and engineering a hierarchical supramolecular framework for
 enhanced iodine uptake.
;
_journal_issue                   4
_journal_name_full               'Chemical science'
_journal_page_first              1730
_journal_page_last               1736
_journal_paper_doi               10.1039/d4sc04474f
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C60 H48 N24 O24 Zn9, 5.5[H2O]'
_chemical_formula_sum            'C60 H59 N24 O29.5 Zn9'
_chemical_formula_weight         2176.64
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2j05tk
_audit_creation_date             2024-11-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-25 deposited with the CCDC.	2024-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.31573(19)
_cell_length_b                   15.31573(19)
_cell_length_c                   56.9773(7)
_cell_measurement_reflns_used    15234
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6130
_cell_measurement_theta_min      3.4370
_cell_volume                     11574.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9784
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.949
_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    -20.00  26.00   0.50    7.50    --   17.77  93.00 -86.00   92
  2  \w    -93.00  25.00   0.50    7.50    --  -19.57 -19.00 150.00  236
  3  \w    -88.00   2.00   0.50    7.50    --  -19.57 -57.00   0.00  180
  4  \w    -88.00   2.00   0.50    7.50    --  -19.57 -57.00  90.00  180
  5  \w    -41.00  49.00   0.50    7.50    --  -19.57  57.00 -30.00  180
  6  \w    -50.00  51.00   0.50    7.50    --  -19.57  77.00-150.00  202
  7  \w    -51.00  38.00   0.50    7.50    --   17.77 -57.00  90.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0359290000
_diffrn_orient_matrix_UB_12      0.0386384000
_diffrn_orient_matrix_UB_13      0.0073489000
_diffrn_orient_matrix_UB_21      -0.0228213000
_diffrn_orient_matrix_UB_22      0.0296263000
_diffrn_orient_matrix_UB_23      -0.0022884000
_diffrn_orient_matrix_UB_31      -0.0323406000
_diffrn_orient_matrix_UB_32      -0.0221284000
_diffrn_orient_matrix_UB_33      0.0097815000
_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  0.0339
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       76
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            47231
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.957
_diffrn_reflns_theta_min         3.389
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.874
_exptl_crystal_description       block
_exptl_crystal_F_000             6558
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3247
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0509P)^2^+51.9232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2822
_reflns_number_total             3247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04474f2.cif
_cod_data_source_block           zn9_sq
_cod_depositor_comments
'Adding full bibliography for 1573449--1573451.cif.'
_cod_original_cell_volume        11574.6(3)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C60 H59 N24 O29.50 Zn9'
_cod_database_code               1573449
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.514
_shelx_estimated_absorpt_t_min   0.463
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O4-H4
 0.85 with sigma of 0.01
 C10-H4
 1.928692 with sigma of 0.02
 Zn1-H4
 2.943996 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C5(H5)
;
_shelx_res_checksum              80132
_shelx_fab_checksum              54558
_platon_squeeze_special_details
;
A solvent mask was calculated and 336 electrons were 
found in a volume of 1421\%A^3^ in 6 voids per unit cell. 
This is consistent with the presence of 
[5.5 H2O] per formula unit 
which account for 330 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_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 2.770
_oxdiff_exptl_absorpt_empirical_full_min 0.796