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_7126507
_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         '8(C49.92 H31.2 O19.48 Th3)'
_chemical_formula_sum            'C399.36 H249.6 O155.84 Th24'
_chemical_formula_weight         13110.29
_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_block_doi                 10.5517/ccdc.csd.cc24hz9y
_audit_creation_date             2020-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-20 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            1
_cell_length_a                   30.976(4)
_cell_length_b                   30.976(4)
_cell_length_c                   30.976(4)
_cell_measurement_reflns_used    7807
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.18
_cell_volume                     29722(7)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0881
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            23613
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.181
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.021
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1359 before and 0.0800 after correction. The Ratio of minimum to maximum transmission is 0.7332. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.732
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             6052
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.019
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.00016(4)
_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   1.234
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1424
_refine_ls_number_restraints     357
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0573
_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^)+(0.1138P)^2^+168.1586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.2038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1036
_reflns_number_total             1424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02841j2.cif
_cod_data_source_block           Th-SINAP-15_sq
_cod_depositor_comments
'Adding full bibliography for 7126502--7126508.cif.'
_cod_original_cell_volume        29722(10)
_cod_original_formula_sum        'C399.36 H249.60 O155.84 Th24'
_cod_database_code               7126507
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.677
_shelx_estimated_absorpt_t_min   0.677
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-O1 = C1-O2 = C16-O3 = C16-O4
 1.22 with sigma of 0.02
 C1-C2 = C13-C16 = C5-C8 = C9-C10
 1.46 with sigma of 0.02
 C8-C9
 1.33 with sigma of 0.02
 C8-C4 \\sim C8-C6 \\sim C9-C11 \\sim C9-C15
 with sigma of 0.02
 C2-O1 \\sim C2-O2 \\sim C13-O3 \\sim C13-O4
 with sigma of 0.02
 C8-C11 \\sim C9-C6
 with sigma of 0.02
 C1-C3 \\sim C1-C7 \\sim C16-C12 \\sim C16-C14
 with sigma of 0.02
 O1-Th1 \\sim O2-Th1_$1 \\sim O3-Th1_$2 \\sim O4-Th1_$3
 with sigma of 0.02
3. Restrained planarity
 O1, O2, O3, O4, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14,
 C15, C16, Th1, Th1_$3, Th1_$2, Th1_$1
 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
O1 \\sim O2 \\sim O3 \\sim O4 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5
\\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13
\\sim C14 \\sim C15 \\sim C16: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O1) = Uanis(O2) = Uanis(O3) = Uanis(O4)
6. Others
 Fixed Sof: O1(0.13) O2(0.13) O3(0.13) O4(0.13) C1(0.13) C2(0.13) C3(0.13)
 H3(0.13) C4(0.13) H4(0.13) C5(0.13) C6(0.13) H6(0.13) C7(0.13) H7(0.13)
 C8(0.13) H8(0.13) C9(0.13) H9(0.13) C10(0.13) C11(0.13) H11(0.13) C12(0.13)
 H12(0.13) C13(0.13) C14(0.13) H14(0.13) C15(0.13) H15(0.13) C16(0.13)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15)
7.b Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C10(C11,C12,C13,C14,C15)
;
_shelx_res_checksum              36195
_shelx_hkl_checksum              86136
_shelx_fab_checksum              75731
_olex2_submission_special_instructions 'No special instructions were received'