A Cationic Thorium-Organic Framework with Triple Single-Crystal-to-Single-Crystal Transformation Peculiarities for Ultrasensitive Anion Recognition
Li, Zi-Jian; Lei, Min; Bao, Hong-liang; Yu, Ju; Lu, Huangjie; Li, Yongxin; Zhang, Zhi-Hui; Guo, Xiaofeng; Qian, Yuan; He, Mingyang; Wang, Jian-Qiang; Liu, Wei; Lin, Jian; Chemical Science  (2021) –; doi:10.1039/D1SC03709A

data_1565060
_publ_section_title
;
 A Cationic Thorium-Organic Framework with Triple
 Single-Crystal-to-Single-Crystal Transformation Peculiarities for
 Ultrasensitive Anion Recognition
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03709A
_journal_year                    2021
_chemical_formula_moiety         'C156 H96 N4 O37 Th6'
_chemical_formula_sum            'C156 H96 N4 O37 Th6'
_chemical_formula_weight         4010.60
_chemical_name_systematic        Th-SINAP-202
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.987(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   48.68(3)
_cell_length_b                   20.234(11)
_cell_length_c                   43.14(2)
_cell_measurement_reflns_used    9269
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      17.096
_cell_measurement_theta_min      2.201
_cell_volume                     39933(4)
_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      120.0
_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  0.2270
_diffrn_reflns_av_unetI/netI     0.1153
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            82872
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        16.516
_diffrn_reflns_theta_max         16.516
_diffrn_reflns_theta_min         1.873
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.510
_exptl_absorpt_correction_T_max  0.7441
_exptl_absorpt_correction_T_min  0.5213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1202 before and 0.0984 after correction. The Ratio of minimum to maximum transmission is 0.7006. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             15168
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         7.361
_refine_diff_density_min         -2.103
_refine_diff_density_rms         0.428
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.467
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1540
_refine_ls_number_reflns         10654
_refine_ls_number_restraints     3424
_refine_ls_restrained_S_all      1.342
_refine_ls_R_factor_all          0.2508
_refine_ls_R_factor_gt           0.2099
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.3700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5158
_refine_ls_wR_factor_ref         0.5659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6785
_reflns_number_total             10654
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03709a2.cif
_cod_data_source_block           Th-SINAP-202_sq
_cod_original_cell_volume        39938(38)
_cod_database_code               1565060
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.497
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O5-C39 = O6-C39
 1.25 with sigma of 0.02
 N4-C131 = N4-C128 = N4-C144
 1.48 with sigma of 0.02
 N3-C89 = N3-C92 = N3-C105
 1.48 with sigma of 0.02
 O10-C65 = O9-C65
 1.25 with sigma of 0.02
 O11-C78 = O12-C78
 1.25 with sigma of 0.02
 O26-Th1
 2.4 with sigma of 0.02
 O26-Th2
 2.4 with sigma of 0.02
 O26-Th6
 2.4 with sigma of 0.02
 O31-Th5
 2.4 with sigma of 0.02
 Th6-O31
 2.4 with sigma of 0.02
 O31-Th4
 2.4 with sigma of 0.02
 C80-C81 = O4-C26
 1.25 with sigma of 0.02
 C26-O3
 1.25 with sigma of 0.02
 C156-O24
 1.25 with sigma of 0.02
 C156-O23
 1.25 with sigma of 0.02
 C150-C146
 2.5 with sigma of 0.02
 C56-C59
 1.51 with sigma of 0.02
 C153-C156
 1.51 with sigma of 0.02
 H82-C82
 1.48 with sigma of 0.02
 N4-C131 = N4-C144 = N4-C128
 1.48 with sigma of 0.02
 C45-C44 = C45-H45 = C45-C46
 1.51 with sigma of 0.02
 C128-C136
 3 with sigma of 0.02
 C137-C134 = C147-C150 = C118-C119 = C122-C125 = C140-C143 = C117-C114 = C108-
 C111 = C83-C86 = C80-C79 = C95-C98 = C101-C104 = C2-C1 = C5-C8 = C26-C23 = C20-
 C17 = C33-C30 = C39-C36 = C44-C47 = C40-C41 = C65-C62 = C59-C56 = C69-C72 =
 C75-C78
 1.51 with sigma of 0.02
 C26-C23
 1.51 with sigma of 0.02
 C138-C134 \\sim C134-C142
 with sigma of 0.02
 C13-C5 \\sim C5-C9
 with sigma of 0.02
 C6-C8 \\sim C8-C4
 with sigma of 0.02
 C133-C137 \\sim C137-C135
 with sigma of 0.02
 C142-C134 \\sim C134-C138
 with sigma of 0.02
 C139-C143 \\sim C143-C141
 with sigma of 0.02
3. Restrained planarity
 C111, C112, C113, C114, C115, C116, C117
 with sigma of 0.1
 C4, C5, C6, C8
 with sigma of 0.1
 C5, C8, C9, C13
 with sigma of 0.1
 C131, C132, C133, C134, C135, C136, C137
 with sigma of 0.1
4. 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
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 O4, C26
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.004
 C24, C23, C25
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C13(H13), C12(H12), C10(H10), C9(H9),
 C15(H15), C16(H16), C18(H18), C19(H19), C24(H24), C25(H25), C21(H21), C22(H22),
  C28(H28), C29(H29), C31(H31), C32(H32), C37(H37), C38(H38), C34(H34),
 C35(H35), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51),
  C52(H52), C57(H57), C55(H55), C54(H54), C58(H58), C60(H60), C61(H61),
 C63(H63), C64(H64), C71(H71), C67(H67), C68(H68), C70(H70), C73(H73), C74(H74),
  C76(H76), C77(H77), C85(H85), C84(H84), C82(H82), C81(H81), C87(H87),
 C88(H88), C90(H90), C91(H91), C96(H96), C97(H97), C93(H93), C94(H94), C99(H99),
  C100(H100), C102(H102), C103(H103), C109(H109), C107(H107), C106(H106),
 C110(H110), C116(H116), C115(H115), C113(H113), C112(H112), C124(H124),
 C123(H123), C121(H121), C120(H120), C127(H127), C126(H126), C130(H130),
 C129(H129), C132(H132), C133(H133), C135(H135), C136(H136), C139(H139),
 C138(H138), C142(H142), C141(H141), C149(H149), C148(H148), C146(H146),
 C145(H145), C152(H152), C151(H151), C155(H155), C154(H154)
6.b Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C8(C13,C12,C11,C10,C9), C15(C16,C17,C18,C19,C14), C24(C25,
 C20,C21,C22,C23), C27(C28,C29,C30,C31,C32), C36(C37,C38,C33,C34,C35), C41(C42,
 C43,C44,C45,C46), C47(C48,C49,C50,C51,C52), C57(C56,C55,C54,C53,C58), C59(C60,
 C61,C62,C63,C64), C71(C66,C67,C68,C69,C70), C72(C73,C74,C75,C76,C77), C85(C84,
 C83,C82,C81,C80), C86(C87,C88,C89,C90,C91), C95(C96,C97,C92,C93,C94), C98(C99,
 C100,C101,C102,C103), C109(C108,C107,C106,C105,C110), C111(C116,C115,C114,C113,
 C112), C124(C123,C122,C121,C120,C119), C128(C127,C126,C125,C130,C129),
 C132(C133,C134,C135,C136,C131), C139(C138,C137,C142,C141,C140), C149(C148,C147,
 C146,C145,C144), C153(C152,C151,C150,C155,C154)
;
_shelx_res_checksum              20964
_shelx_hkl_checksum              32761
_shelx_fab_checksum              28913
_olex2_submission_special_instructions 'No special instructions were received'