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_1573450
_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         'C348 H288 N156 O118.8 Zn54, 4.8(I2), 23.5[I2]'
_chemical_formula_sum            'C348 H288 I56.6 N156 O118.8 Zn54'
_chemical_formula_weight         19268.65
_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.cc2j05wm
_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                   58.9792(3)
_cell_length_b                   58.9792(3)
_cell_length_c                   58.9792(3)
_cell_measurement_reflns_used    16437
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      66.6360
_cell_measurement_theta_min      2.4760
_cell_volume                     205161.9(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (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 0.985
_diffrn_measured_fraction_theta_max 0.914
_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    -28.00  27.00   0.50   30.00    --   43.30 -19.00  90.00  110
  2  \w     36.00  66.00   0.50   70.00    --  109.26 -61.00  76.00   60
  3  \w     35.00  71.00   0.50   70.00    --  109.26 -61.00  30.00   72
  4  \w    -76.00 -18.00   0.50   70.00    --  -90.25 113.00  14.00  116
  5  \w    -39.00 -14.00   0.50   70.00    --  -90.25  45.00  30.00   50
;
_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      -0.0015124000
_diffrn_orient_matrix_UB_12      0.0209815000
_diffrn_orient_matrix_UB_13      -0.0154550000
_diffrn_orient_matrix_UB_21      0.0221093000
_diffrn_orient_matrix_UB_22      0.0092435000
_diffrn_orient_matrix_UB_23      0.0104055000
_diffrn_orient_matrix_UB_31      0.0138440000
_diffrn_orient_matrix_UB_32      -0.0124907000
_diffrn_orient_matrix_UB_33      -0.0183159000
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       74
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            63823
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.032
_diffrn_reflns_theta_min         2.485
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             72306
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         16367
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1631P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2336
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10617
_reflns_number_total             16367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04474f2.cif
_cod_data_source_block           zn54-i2
_cod_depositor_comments
'Adding full bibliography for 1573449--1573451.cif.'
_cod_original_cell_volume        205162(3)
_cod_original_sg_symbol_H-M      'F d -3'
_cod_original_formula_sum        'C348 H288 I56.60 N156 O118.80 Zn54'
_cod_database_code               1573450
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.111
_shelx_estimated_absorpt_t_min   0.093
_reflns_odcompleteness_completeness 98.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 I2-I1 = I1-I2'
 2.9 with sigma of 0.02
 C18-C17 = C18-C17A
 1.45 with sigma of 0.02
 C18-C17 \\sim C18-C17A
 with sigma of 0.02
 O5-C17 \\sim O5A-C17A \\sim O6-C17 \\sim O6A-C17A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(I2) \\sim Ueq, Uanis(I2') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(I3) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C17A)
\\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(I3) = Uanis(I3')
Uanis(I2) = Uanis(I2')
Uanis(O5) = Uanis(O5A)
Uanis(C17) = Uanis(C17A)
Uanis(O6) = Uanis(O6A)
4. Others
 Sof(O5A)=Sof(O6A)=Sof(C17A)=1-FVAR(1)
 Sof(O5)=Sof(O6)=Sof(C17)=FVAR(1)
 Fixed Sof: O9(0.9) H26A(0.5) H26B(0.5) C27(0.5) H27A(0.5) H27B(0.5) C28(0.5)
 H28A(0.5) H28B(0.5) C29(0.5) H29A(0.5) H29B(0.5) I1(0.26666) I2(0.13333)
 I2'(0.13333) I3(0.13333) I3'(0.13333)
 Fixed X: C28(0.52369)
 Fixed Y: C28(0.40525)
 Fixed Z: C28(0.628091)
5.a Rotating group:
 O10(H10A,H10B)
5.b Ternary CH refined with riding coordinates:
 N13(H13)
5.c Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13A), C14(H14), C19(H19), C20(H20),
 C21(H21)
5.e Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90428
_shelx_fab_checksum              19917
_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 1.329
_oxdiff_exptl_absorpt_empirical_full_min 0.775