Rational design and synthesis of a novel ternary metal-organic framework with a (3,5)-connected topology for iodine capture.
Yuan, Jingjing; Lei, Honghui; Song, Fahui; Tu, Binbin; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15856–15863; doi:10.1039/d5dt01722j

data_7719496
_publ_section_title
;
 Rational design and synthesis of a novel ternary metal-organic framework
 with a (3,5)-connected topology for iodine capture.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15856
_journal_page_last               15863
_journal_paper_doi               10.1039/d5dt01722j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C74 H44 N4 O16 Zn4, 13[C5H11NO]'
_chemical_formula_sum            'C139 H187 N17 O29 Zn4'
_chemical_formula_weight         2821.52
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-09-10
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-09-10 deposited with the CCDC.	2025-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.793(5)
_cell_length_b                   23.793(5)
_cell_length_c                   49.173(10)
_cell_measurement_reflns_used    9575
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.12
_cell_measurement_theta_min      2.43
_cell_volume                     24108(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            84373
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        37.590
_diffrn_reflns_theta_max         37.590
_diffrn_reflns_theta_min         2.434
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.5104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0912 before and 0.0676 after correction.
The Ratio of minimum to maximum transmission is 0.6829.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.583
_exptl_crystal_description       rod
_exptl_crystal_F_000             4476
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.171
_refine_diff_density_rms         0.012
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         12552
_refine_ls_number_restraints     271
_refine_ls_restrained_S_all      24.059
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0232P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.954
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                8474
_reflns_number_total             12552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01722j2.cif
_cod_data_source_block           ccnuf-7
_cod_depositor_comments          'Adding full bibliography for 7719496.cif.'
_cod_original_cell_volume        24107(11)
_cod_database_code               7719496
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.59(2)
 0.41(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C17-C20 = C34-C37 = C1-C2 = C29-C31 = C5-C8 = C12-C14 = C10-C21 = C25-C27
 1.5 with sigma of 0.01
 H11-H15
 2.2 with sigma of 0.01
 C1-C2 = C5-C8 = C17-C20
 1.5 with sigma of 0.003
 H9-H23
 2.2 with sigma of 0.005
 C24-C27 = C26-C27 = C9-C21 = C11-C21
 2.4 with sigma of 0.001
 C28-C31 = C30-C31 = C34-O7 = C17-O5 = C17-O6 = C28-C30
 2.4 with sigma of 0.01
 O6-O8
 3.2 with sigma of 0.01
 C27-O3 = C27-O4 = C37-O7 = C37-O8
 1.3 with sigma of 0.01
 C20-O6 = C20-O5
 1.26 with sigma of 0.01
 C25-O4 = C2-O1 = C17-O6 = C34-O8
 2.3 with sigma of 0.03
 C20-C18 = C33-C37 = O5-O6
 2.4 with sigma of 0.03
 Zn1-N2 = Zn2-C28
 3 with sigma of 0.01
4. Restrained planarity
 O3, O4, C21, C22, C26, C25, C24, C23, C27
 with sigma of 0.1
 O6, C20, C17, C16, C15, C14, C19, C18
 with sigma of 0.1
 O1, O2, C1, C2, C3, C4, C5, C6
 with sigma of 0.1
5. Rigid bond restraints
 O3, O4, C21, C22, C26, C25, C24, C23, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C15, C16, C17, C18, C19, C20, O5, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C28, C29, C30, N1, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C8, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C32, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C35, C36
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C14, C15, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1, N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C27, O3, O4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Zn1, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, Zn2, N2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C14) \\sim
Ueq, Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C22) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O4)
\\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C23) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.001
7.a :
 C29(C28,N2,N1,C30)
7.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C30(H30), C7(H7), C6(H6), C4(H4), C3(H3A), C11(H11), C13(H13),
 C9(H9), C22(H22), C26(H26), C24(H24), C23(H23), C32(H32), C33(H33), C35(H35),
 C36(H36), C16(H16), C15(H15), C19(H19), C18(H18)
7.c Fitted hexagon refined as free rotating group:
 C2(C7,C6,C5,C4,C3), C10(C11,C12,C13,C8,C9), C21(C22,C26,C25,C24,C23), C31(C32,
 C33,C34,C35,C36), C17(C16,C15,C14,C19,C18)
7.d Tetrahedral OH refined with riding coordinates:
 O3(H3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90151
_shelx_fab_checksum              74387
_olex2_submission_special_instructions 'No special instructions were received'