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_7708267
_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 H44 Gd4 N4 O30 S24, 4(C3 H7 N O)'
_chemical_formula_sum            'C72 H72 Gd4 N8 O34 S24'
_chemical_formula_weight         2991.81
_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             2020-10-29
_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                 102.869(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6826(7)
_cell_length_b                   23.109(5)
_cell_length_c                   26.232(9)
_cell_measurement_reflns_used    17757
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      3.5530
_cell_measurement_theta_min      29.0730
_cell_volume                     10450(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48831
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.388
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.066
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       block
_exptl_crystal_F_000             5888
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         5.679
_refine_diff_density_min         -3.194
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         18373
_refine_ls_number_restraints     4140
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+114.2579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.2037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13561
_reflns_number_total             18373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01851e2.cif
_cod_data_source_block           1-Gd
_cod_database_code               7708267
_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
N1 \\sim C03O \\sim C03H \\sim C033: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N7 \\sim C3 \\sim C03P \\sim C12: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C01K \\sim C01M \\sim C01O \\sim C01P \\sim
C01R \\sim C01S \\sim C01U \\sim C01V \\sim C01W \\sim C01X \\sim C01Y \\sim
C01Z \\sim C020 \\sim C021 \\sim C022 \\sim C023 \\sim C024 \\sim C025 \\sim
C026 \\sim C027 \\sim C028 \\sim C029 \\sim C02A \\sim C02B \\sim C02C \\sim
C02E \\sim C02F \\sim C02G \\sim C02H \\sim C02I \\sim C02J \\sim C02K \\sim
C02M \\sim C02N \\sim C02O \\sim C02P \\sim C02Q \\sim C02R \\sim C02S \\sim
C02U \\sim C02V \\sim C02Y \\sim C02Z \\sim C030 \\sim C031 \\sim C032 \\sim
C033 \\sim C034 \\sim C037 \\sim C03D \\sim C03E \\sim C03F \\sim C03H \\sim
C03I \\sim C03J \\sim C03K \\sim C03M \\sim C03N \\sim C03O \\sim C03P: within
10A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 10A
N3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
N4 \\sim C10 \\sim C031 \\sim C03M: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Rotating group:
 O01G(H01A,H01B), O01I(H01C,H01D)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C12(H12), C02E(H02E), C02I(H02I), C02J(H02J), C02O(H02O),
 C02P(H02P), C02Q(H02Q), C02U(H02U), C02V(H02V), C030(H030), C031(H031),
 C032(H032), C033(H033), C034(H034), C037(H037), C03D(H03X), C03F(H03Q),
 C03I(H03I)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C03E(H03Y,H,
 HA), C03H(H03A,H03B,H03C), C03J(H03R,H03S,H03T), C03K(H03U,H03V,H03W),
 C03M(H03D,H03E,H03F), C03N(H03K,H03L,H03M), C03O(H03G,H03H,H03J), C03P(H03N,
 H03O,H03P)
;
_shelx_res_checksum              12197
_olex2_submission_special_instructions 'No special instructions were received'