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_7708268
_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 Dy4 N4 O30 S24, 4(C3 H7 N O)'
_chemical_formula_sum            'C72 H74 Dy4 N8 O34 S24'
_chemical_formula_weight         3014.83
_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                 103.218(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6503(5)
_cell_length_b                   23.0251(6)
_cell_length_c                   26.1975(7)
_cell_measurement_reflns_used    13747
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9710
_cell_measurement_theta_min      3.5760
_cell_volume                     10364.6(5)
_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 0.845
_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  0.0264
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            51030
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.365
_diffrn_reflns_theta_min         3.315
_exptl_absorpt_coefficient_mu    3.416
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_description       block
_exptl_crystal_F_000             5928
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.165
_refine_diff_density_min         -3.070
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         24102
_refine_ls_number_restraints     5814
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+76.6154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17037
_reflns_number_total             24102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01851e2.cif
_cod_data_source_block           1-Dy
_cod_database_code               7708268
_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
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C8 \\sim C7 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C15 \\sim C14 \\sim C16 \\sim C18
\\sim C17 \\sim C19 \\sim C01K \\sim C01O \\sim C01P \\sim C01Q \\sim C01S
\\sim C01T \\sim C01U \\sim C01V \\sim C01W \\sim C01X \\sim C01Y \\sim C01Z
\\sim C020 \\sim C20 \\sim C021 \\sim C21 \\sim C022 \\sim C023 \\sim C024
\\sim C025 \\sim C026 \\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 C02L \\sim C02M \\sim C02O \\sim C02P \\sim C02Q \\sim C02R \\sim C02T
\\sim C02U \\sim C02V \\sim C02X \\sim C02Z \\sim C031 \\sim C032 \\sim C033
\\sim C034 \\sim C035 \\sim C036 \\sim C037 \\sim C03A \\sim C03G: within 10A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 10A
Uanis(C1) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C2) \\sim Ueq, Uanis(C03G) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N7)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C5) \\sim Ueq, Uanis(C03A) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N6)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
3.a Rotating group:
 O01H(H01A,H01B), O01J(H01C,H01D)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C15(H15), C19(H19), C21(H21), C02B(H02B), C02H(H02H), C02M(H02M),
 C02O(H02O), C02P(H02P), C02R(H02R), C02U(H02U), C02V(H02V), C031(H031),
 C033(H033), C034(H034), C035(H035), C036(H036), C037(H037), C03A(H03A),
 C03G(H03G)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,
 H10C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,
 H16B,H16C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              67813
_olex2_submission_special_instructions 'No special instructions were received'