Family of Lanthanide Metal-Organic Frameworks Based on Redox-Active Tetrathiafulvalene-Dicarboxylic Ligand Showing Slow Relaxation of Magnetisation and Electronic Conductivity
Hu, Jun-Jie; Li, Yu-Guang; Wen, He-Rui; Liu, Sui-Jun; Peng, Yan; Liu, Cai-Ming; Dalton Transactions  (2021) –; doi:10.1039/D1DT01851E

data_7708269
_publ_section_title
;
 Family of Lanthanide Metal-Organic Frameworks Based on Redox-Active
 Tetrathiafulvalene-Dicarboxylic Ligand Showing Slow Relaxation of
 Magnetisation and Electronic Conductivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01851E
_journal_year                    2021
_chemical_formula_moiety         'C60 H41 N4 O30 S24 Tb4, 4(C3 H7 N O)'
_chemical_formula_sum            'C72 H67 N8 O34 S24 Tb4'
_chemical_formula_weight         2993.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-09-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-09 deposited with the CCDC.	2021-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.037(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6786(6)
_cell_length_b                   23.0569(8)
_cell_length_c                   26.3088(8)
_cell_measurement_reflns_used    11894
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4690
_cell_measurement_theta_min      3.8720
_cell_volume                     10447.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.849
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.849
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56426
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.447
_diffrn_reflns_theta_min         3.254
_exptl_absorpt_coefficient_mu    3.235
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_description       block
_exptl_crystal_F_000             5884
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         5.158
_refine_diff_density_min         -2.795
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1296
_refine_ls_number_reflns         24595
_refine_ls_number_restraints     3972
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1281
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+10.2861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1829
_refine_ls_wR_factor_ref         0.2200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13864
_reflns_number_total             24595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01851e2.cif
_cod_data_source_block           1-Tb
_cod_database_code               7708269
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
N6 \\sim C2 \\sim C63 \\sim C3: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N3 \\sim C65 \\sim C1 \\sim C64: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N5 \\sim C67 \\sim C5 \\sim C66: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N7 \\sim C4 \\sim C62 \\sim C61: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C1 \\sim C2 \\sim C29 \\sim C28 \\sim C27 \\sim C26 \\sim C3 \\sim C39 \\sim C4
\\sim C49 \\sim C48 \\sim C47 \\sim C46 \\sim C45 \\sim C44 \\sim C43 \\sim C42
\\sim C41 \\sim C40 \\sim C59 \\sim C58 \\sim C57 \\sim C56 \\sim C55 \\sim C54
\\sim C53 \\sim C52 \\sim C51 \\sim C50 \\sim C5 \\sim C67 \\sim C66 \\sim C65
\\sim C64 \\sim C63 \\sim C62 \\sim C61 \\sim C60 \\sim C6 \\sim C9 \\sim C7
\\sim C8 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16
\\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24
\\sim C25 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C35 \\sim C34 \\sim C37
\\sim C36 \\sim C38 \\sim C69 \\sim C72 \\sim C70 \\sim C71 \\sim C68: within
10A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 10A
Uanis(C62) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(O8) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C3) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Rotating group:
 O5(H5A,H5B), O17(H17A,H17B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C27(H27), C3(H3), C39(H39), C47(H47), C42(H42), C58(H58), C55(H55),
 C50(H50), C5(H5), C61(H61), C6(H6), C11(H11), C14(H14), C19(H19), C22(H22),
 C30(H30), C35(H35), C69(H69), C72(H72)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C67(H67A,H67B,H67C), C66(H66A,H66B,H66C),
 C65(H65A,H65B,H65C), C64(H64A,H64B,H64C), C62(H62A,H62B,H62C), C9(H9A,H9B,H9C),
  C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              60590
_olex2_submission_special_instructions 'No special instructions were received'