Synthesis of luminescent thorium-based metal‒organic frameworks with 1,2,4,5-tetrakis(4-carboxyphenyl)benzene
Yu, Ting; Qian, Zheng-hua; Li, Lin; Wu, Xiao-ling; He, Hui; Qiao, Yan-bo; Ye, Guo-an; RSC Advances 11 (2021) 17431–17436; doi:10.1039/D1RA01742J

data_7242823
_publ_section_title
;
 Synthesis of luminescent thorium-based metal--organic frameworks with
 1,2,4,5-tetrakis(4-carboxyphenyl)benzene
;
_journal_issue                   28
_journal_name_full               'RSC Advances'
_journal_page_first              17431
_journal_page_last               17436
_journal_paper_doi               10.1039/D1RA01742J
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         '0.5(C68 H36 O16 Th2)'
_chemical_formula_sum            'C34 H18 O8 Th'
_chemical_formula_weight         786.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-04 deposited with the CCDC.	2021-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.102(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.640(3)
_cell_length_b                   11.024(6)
_cell_length_c                   28.315(15)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.911
_cell_measurement_theta_min      3.063
_cell_volume                     1759.3(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_unetI/netI     0.1094
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3260
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.186
_diffrn_reflns_theta_min         7.837
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.221
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1585 before and 0.1031 after correction. The Ratio of minimum to maximum transmission is 0.6103. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.006
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.003
_refine_diff_density_max         4.030
_refine_diff_density_min         -3.269
_refine_diff_density_rms         0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3260
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0970
_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^)+(0.1410P)^2^+18.4174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2586
_refine_ls_wR_factor_ref         0.2768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2367
_reflns_number_total             3260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra01742j2.cif
_cod_data_source_block           200716qzh_3_0m_sq
_cod_database_code               7242823
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.617(5)
 0.383(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 C17-C14
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim O1 \\sim O2:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim O4: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
O3 \\sim C17 \\sim O4 \\sim C14: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C7(H7), C6(H6), C9(H9), C12(H12), C13(H13), C15(H15), C16(H16)
5.b Fitted hexagon refined as free rotating group:
 C5(C4,C3,C2,C7,C6), C11(C12,C13,C14,C15,C16)
;
_shelx_res_checksum              20573
_shelx_fab_checksum              8992
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'