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_7126502
_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         '2(C42 H24 N6 O19 Th3)'
_chemical_formula_sum            'C84 H48 N12 O38 Th6'
_chemical_formula_weight         3225.58
_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.cc24hz8x
_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            4
_cell_length_a                   30.4822(15)
_cell_length_b                   30.4822(15)
_cell_length_c                   30.4822(15)
_cell_measurement_reflns_used    2460
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.743
_cell_measurement_theta_min      2.216
_cell_volume                     28323(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1773
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            29843
_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         27.445
_diffrn_reflns_theta_min         2.216
_exptl_absorpt_coefficient_mu    3.170
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7051
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.756
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             5920
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.871
_refine_diff_density_min         -2.303
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.00029(6)
_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   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         1658
_refine_ls_number_restraints     364
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1527
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1684P)^2^+700.5977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.3077
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1025
_reflns_number_total             1658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc02841j2.cif
_cod_data_source_block           Th-SINAP-14_sq
_cod_depositor_comments
'Adding full bibliography for 7126502--7126508.cif.'
_cod_original_cell_volume        28323(4)
_cod_database_code               7126502
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.702
_shelx_estimated_absorpt_t_min   0.702
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N1-C9 = N2-C6
 2.9 with sigma of 0.02
 C1-O1 = C14-O3 = C1-O2 = C14-O4
 1.22 with sigma of 0.01
 C1-C2 = C11-C14
 1.5 with sigma of 0.02
 C5-N1 = C8-N2
 1.4 with sigma of 0.02
 N1-N2
 1.25 with sigma of 0.01
 N1-C4 \\sim N1-C6 \\sim N2-C9 \\sim N2-C13
 with sigma of 0.02
 C1-C3 \\sim C1-C7 \\sim C14-C10 \\sim C14-C12
 with sigma of 0.01
 C2-O1 \\sim C2-O2 \\sim C11-O3 \\sim C11-O4
 with sigma of 0.02
 O1-Th1 \\sim O2-Th1_$1 \\sim O4-Th1_$2 \\sim O3-Th1_$3
 with sigma of 0.01
3. Restrained planarity
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, N1, N2, 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
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(N1)
\\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq,
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
6. Others
 Fixed Sof: C1(0.125) C2(0.125) C3(0.125) H3(0.125) C4(0.125) H4(0.125)
 C5(0.125) C6(0.125) H6(0.125) C7(0.125) H7(0.125) C8(0.125) C9(0.125)
 H9(0.125) C10(0.125) H10(0.125) C11(0.125) C12(0.125) H12(0.125) C13(0.125)
 H13(0.125) C14(0.125) N1(0.125) N2(0.125) O1(0.125) O2(0.125) O3(0.125)
 O4(0.125)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13)
7.b Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C8(C9,C10,C11,C12,C13)
;
_shelx_res_checksum              86176
_shelx_hkl_checksum              93029
_shelx_fab_checksum              64822
_olex2_submission_special_instructions 'No special instructions were received'