Modulated synthesis and isoreticular expansion of Th-MOFs with record high pore volume and surface area for iodine adsorption.
Li, Zi-Jian; Ju, Yu; Yu, Bowen; Wu, Xiaoling; Lu, Huangjie; Li, Yongxin; Zhou, Jing; Guo, Xiaofeng; Zhang, Zhi-Hui; Lin, Jian; Wang, Jian-Qiang; Wang, Shuao; Chemical communications (Cambridge, England) 56 (2020) 6715–6718; doi:10.1039/d0cc02841j

data_7126506
_publ_section_title
;
 Modulated synthesis and isoreticular expansion of Th-MOFs with record
 high pore volume and surface area for iodine adsorption.
;
_journal_issue                   49
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6715
_journal_page_last               6718
_journal_paper_doi               10.1039/d0cc02841j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '4(C36 H24 O19 Th3)'
_chemical_formula_sum            'C144 H96 O76 Th12'
_chemical_formula_weight         5826.68
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-10 deposited with the CCDC.	2020-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.2063(13)
_cell_length_b                   28.2063(13)
_cell_length_c                   28.2063(13)
_cell_measurement_reflns_used    5417
_cell_measurement_temperature    120
_cell_measurement_theta_max      20.802
_cell_measurement_theta_min      2.399
_cell_volume                     22440.8(18)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1221
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            10639
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        20.767
_diffrn_reflns_theta_max         20.767
_diffrn_reflns_theta_min         2.395
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.994
_exptl_absorpt_correction_T_max  0.7230
_exptl_absorpt_correction_T_min  0.6242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1185 before and 0.1129 after correction. The Ratio of minimum to maximum transmission is 0.8633. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.862
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             5296
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.730
_refine_diff_density_min         -2.015
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         647
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1461P)^2^+3016.3293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2128
_refine_ls_wR_factor_ref         0.2203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                587
_reflns_number_total             647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02841j2.cif
_cod_data_source_block           Th-SINAP-12_sq
_cod_depositor_comments
'Adding full bibliography for 7126502--7126508.cif.'
_cod_original_cell_volume        22441(3)
_cod_database_code               7126506
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.605
_shelx_estimated_absorpt_t_min   0.605
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-C3 = C10-C11
 1.33 with sigma of 0.02
 C3-C5 \\sim C3-C9 \\sim C10-C6 \\sim C10-C8
 with sigma of 0.02
 C2-O1 \\sim C2-O2 \\sim C11-O3 \\sim C11-O4
 with sigma of 0.02
 C1-O1 \\sim C1-O2 \\sim C12-O3 \\sim C12-O4
 with sigma of 0.02
 C2-C9 \\sim C4-C7 \\sim C8-C11
 with sigma of 0.02
 C1-C2 \\sim C11-C12
 with sigma of 0.02
3. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, O1, O2, O3, O4, Th1,
 Th1_$1, Th1_$2, Th1_$3
 with sigma of 0.01
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.02 and sigma
for terminal atoms of 0.04
6. Others
 Fixed Sof: C1(0.125) C2(0.125) H2(0.125) C3(0.125) H3(0.125) C4(0.125)
 C5(0.125) H5(0.125) C6(0.125) H6(0.125) C7(0.125) C8(0.125) H8(0.125)
 C9(0.125) H9(0.125) C10(0.125) H10(0.125) C11(0.125) H11(0.125) C12(0.125)
 O1(0.125) O2(0.125) O3(0.125) O4(0.125)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11)
7.b Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C8,C9)
;
_shelx_res_checksum              52679
_shelx_hkl_checksum              68183
_shelx_fab_checksum              95766
_olex2_submission_special_instructions 'No special instructions were received'