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_7131491
_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         'C34 H24 N6 O18 Th3, 6[C3H7NO]'
_chemical_formula_sum            'C52 H68 N12 O25 Th3'
_chemical_formula_weight         1957.30
_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             2023-02-22
_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                   16.4434(13)
_cell_length_b                   16.4434(13)
_cell_length_c                   29.878(2)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    120
_cell_measurement_theta_max      31.00
_cell_measurement_theta_min      2.48
_cell_volume                     8078.6(11)
_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 0.998
_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  0.0434
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            72921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         2.477
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.580
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.4244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1558 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.5686.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             3736
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.620
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.00071(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4724
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+103.1838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1416
_refine_ls_wR_factor_ref         0.1437
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4353
_reflns_number_total             4724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00278k2.cif
_cod_data_source_block           Th-BCPT
_cod_depositor_comments
'Adding full bibliography for 7131491--7131495.cif.'
_cod_original_cell_volume        8078.5(14)
_cod_database_code               7131491
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.605
_shelx_estimated_absorpt_t_min   0.402
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O10-O11
 2.27 with sigma of 0.001
 O10-C10 \\sim O11-C10
 with sigma of 0.001
 O10-O11 \\sim O5A-O5B
 with sigma of 0.001
 O10-C10 \\sim O11-C10 \\sim O5A-C9B \\sim O5B-C9B
 with sigma of 0.001
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
Uanis(C9B) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
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(O3B)=Sof(O4B)=0.5*(1-FVAR(2))
 Sof(O4A)=Sof(O3A)=0.5*FVAR(2)
 Fixed Sof: Th1B(0.25) H8A(0.25) H8B(0.25) O5B(0.25) O7B(0.25) H7BA(0.25)
 H7BB(0.25) C9B(0.25) H9B(0.25) Th1A(0.25) O7A(0.25) H7AA(0.25) H7AB(0.25)
 O11(0.25) C10(0.25) H10(0.25) O10(0.25) O5A(0.25)
6.a Riding coordinates:
 O8(H8A,H8B), O7B(H7BA,H7BB), O7A(H7AA,H7AB)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C3(H3), C6(H6), C7(H7), C9B(H9B), C10(H10)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 954 electrons were 
found in a volume of 4741\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
6[C3H7NO] per Formula Unit 
which account for 960 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9122
_shelx_hkl_checksum              27403
_shelx_fab_checksum              19804
_olex2_submission_special_instructions 'No special instructions were received'