Post-synthetic linker installation: an unprecedented strategy to enhance iodine adsorption in metal-organic frameworks.
Li, Zi-Jian; Ju, Yu; Qiu, Jie; Zhang, Zhi-Hui; Zhang, Linjuan; He, Ming-Yang; Wang, Jian-Qiang; Lin, Jian; Chemical communications (Cambridge, England) 59 (2023) 4958–4961; doi:10.1039/d3cc00278k

data_7131492
_publ_section_title
;
 Post-synthetic linker installation: an unprecedented strategy to enhance
 iodine adsorption in metal-organic frameworks.
;
_journal_issue                   33
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4958
_journal_page_last               4961
_journal_paper_doi               10.1039/d3cc00278k
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C37 H28 N7 O19 Th3, 2[C3H7NO]'
_chemical_formula_sum            'C43 H42 N9 O21 Th3'
_chemical_formula_weight         1716.97
_space_group_crystal_system      tetragonal
_space_group_IT_number           132
_space_group_name_Hall           '-P 4c 2c'
_space_group_name_H-M_alt        'P 42/m c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-24 deposited with the CCDC.	2023-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.037(3)
_cell_length_b                   16.037(3)
_cell_length_c                   30.899(8)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      2.540
_cell_volume                     7947(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX4 v2022.1-1 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            71190
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         1.913
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.656
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1248 before and 0.0805 after correction.
The Ratio of minimum to maximum transmission is 0.6384.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             3204
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.560
_refine_diff_density_min         -1.524
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4890
_refine_ls_number_restraints     652
_refine_ls_restrained_S_all      3.751
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0519
_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^)+(0.1041P)^2^+23.8287P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3697
_reflns_number_total             4890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00278k2.cif
_cod_data_source_block           Th-BCPT-BDC-NH22
_cod_depositor_comments
'Adding full bibliography for 7131491--7131495.cif.'
_cod_original_cell_volume        7947(4)
_cod_database_code               7131492
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.693
_shelx_estimated_absorpt_t_min   0.550
_olex2_refinement_description
;
1. Restrained distances
 C9-C10
 1.51 with sigma of 0.02
 O8-C9
 1.25 with sigma of 0.02
 C11-C9
 2.47 with sigma of 0.02
 C9-C15
 2.47 with sigma of 0.02
 N3-C10
 2.45 with sigma of 0.02
 N4-C15
 2.45 with sigma of 0.02
 C14-N4
 1.45 with sigma of 0.02
 C1-C7 \\sim C1-C3
 with sigma of 0.02
 C9-C11 \\sim C9-C15 \\sim C9-C12 \\sim C9-C14
 with sigma of 0.01
 C10-N3 \\sim N3-C12
 with sigma of 0.02
 C15-N4 \\sim N4-C13
 with sigma of 0.02
2. Restrained planarity
 C9, C10, C11, C12, C13, C14, C15, C9
 with sigma of 0.01
 C9, C10, C11, C12, C13, C14, C15
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, N3
 with sigma of 0.1
 C10, C11, C12, C13, C14, C15, N3, N4
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O1B)=0.5*(1-FVAR(2))
 Sof(O1A)=0.5*FVAR(2)
 Fixed Sof: C10(0.125) C11(0.125) C12(0.125) H12(0.125) C13(0.125) C14(0.125)
 C15(0.125) H15(0.125) H3A(0.25) H3B(0.25) N3(0.125) H3C(0.125) H3D(0.125)
 N4(0.125) H4C(0.125) H4D(0.125)
 Fixed X: C8(0.6752) C9(0.5)
 Fixed Y: C8(0.963) C9(0.5)
 Fixed Z: C8(0.7204) C9(0.6566)
6.a Riding coordinates:
 O4(H4A,H4B), O3(H3A,H3B)
6.b Aromatic/amide H refined with riding coordinates:
 C16(H16), N1(H1), C3(H3), C4(H4), C6(H6), C7(H7), C12(H12), C15(H15)
6.c Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C10(C11,C12,C13,C14,C15)
6.d X=CH2 refined with riding coordinates:
 N3(H3C,H3D), N4(H4C,H4D)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              72180
_shelx_hkl_checksum              81372
_shelx_fab_checksum              1485
_olex2_submission_special_instructions 'No special instructions were received'