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_1573451
_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
'C385.2 H367.2 N165.6 O108 Zn54, 16[C3H8O2], 30[C3H7NO]'
_chemical_formula_sum            'C523.2 H705.2 N195.61 O170 Zn54'
_chemical_formula_weight         15985.07
_space_group_crystal_system      cubic
_space_group_IT_number           203
_space_group_name_Hall           '-F 2uv 2vw 3'
_space_group_name_H-M_alt        'F d -3 :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2j05vl
_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                90
_cell_formula_units_Z            8
_cell_length_a                   58.3017(2)
_cell_length_b                   58.3017(2)
_cell_length_c                   58.3017(2)
_cell_measurement_reflns_used    26694
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.7670
_cell_measurement_theta_min      2.5040
_cell_volume                     198172.6(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.80a (Rigaku OD, 2020)'
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -39.00  18.00   0.50   30.00    --  -46.87  48.00  79.00  114
  2  \w    -48.00 -15.00   0.50  100.00    --  -88.50  48.00  79.00   66
  3  \w   -120.00 -89.00   0.50   30.00    --  -46.87-125.00-150.00   62
  4  \w     44.00  69.00   0.50  100.00    --  108.56 -61.00-150.00   50
  5  \w     39.00  65.00   0.50  100.00    --  108.56 -61.00 -30.00   52
  6  \w     38.00  66.00   0.50  100.00    --  108.56 -61.00  90.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0192307000
_diffrn_orient_matrix_UB_12      -0.0161813000
_diffrn_orient_matrix_UB_13      -0.0082583000
_diffrn_orient_matrix_UB_21      -0.0177846000
_diffrn_orient_matrix_UB_22      0.0191477000
_diffrn_orient_matrix_UB_23      0.0038267000
_diffrn_orient_matrix_UB_31      0.0036404000
_diffrn_orient_matrix_UB_32      0.0083226000
_diffrn_orient_matrix_UB_33      -0.0247897000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       69
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            61406
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.068
_diffrn_reflns_theta_max         67.068
_diffrn_reflns_theta_min         2.514
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.908
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.80a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       Octahedron
_exptl_crystal_F_000             65550
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         14575
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0847P)^2^+263.6934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12642
_reflns_number_total             14575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04474f2.cif
_cod_data_source_block           20200607-hfp-ty-zn54_sq
_cod_depositor_comments
'Adding full bibliography for 1573449--1573451.cif.'
_cod_original_cell_volume        198173(2)
_cod_original_sg_symbol_H-M      'F d -3'
_cod_original_formula_sum        'C523.20 H705.20 N195.61 O170.00 Zn54'
_cod_database_code               1573451
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.598
_shelx_estimated_absorpt_t_min   0.539
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N14-C32 = N14-C33 = N14-C33'
 1.5 with sigma of 0.02
 N14-C32 \\sim N14-C33' \\sim N14-C33
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C33')
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(N14) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C33') = Uanis(C33)
4. Others
 Fixed Sof: N14(0.8) H14(0.4) H14a(0.4) C29(0.5) H29a(0.5) H29b(0.5) C32(0.8)
 H32a(0.8) H32b(0.8) H32c(0.8) C33(0.4) H33a(0.4) H33b(0.4) H33c(0.4) C33'(0.4)
 H33d(0.4) H33e(0.4) H33f(0.4)
 Fixed X: H28a(0.65534) H28b(0.63601)
 Fixed Y: H28a(0.56641) H28b(0.56624)
 Fixed Z: H28a(0.61363) H28b(0.59454)
5.a Ternary CH refined with riding coordinates:
 N13(H13), N14(H14), N14(H14a)
5.b Secondary CH2 refined with riding coordinates:
 C25(H25a,H25b), C26(H26a,H26b), C27(H27a,H27b), C29(H29a,H29b)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13a), C14(H14b), C19(H19), C20(H20),
 C21(H21)
5.d Idealised Me refined as rotating group:
 C30(H30a,H30b,H30c), C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C33(H33a,H33b,
 H33c), C33'(H33d,H33e,H33f)
;
_shelx_res_checksum              13381
_shelx_fab_checksum              69108
_platon_squeeze_special_details
;
A solvent mask was calculated and 14782 electrons were 
found in a volume of 103277\%A^3^ in 7 voids per unit cell. 
This is consistent with the presence of 
16[C3H8O2], 30[C3H7NO] per formula unit 
which account for 14976 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 1.746
_oxdiff_exptl_absorpt_empirical_full_min 0.812