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_7708270
_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 Er4 N4 O30 S24, 4(C3 H7 N O)'
_chemical_formula_sum            'C72 H72 Er4 N8 O34 S24'
_chemical_formula_weight         3031.85
_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
_atom_sites_solution_primary     dual
_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                 103.314(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6348(5)
_cell_length_b                   23.0268(5)
_cell_length_c                   26.0963(6)
_cell_measurement_reflns_used    20456
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0840
_cell_measurement_theta_min      3.5780
_cell_volume                     10312.2(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0894
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -59.00  14.00   1.00   14.00    --  -16.10 106.00 -67.00   73
  2  \w    -86.00 -38.00   1.00   14.00    --  -16.10-178.00   0.00   48
  3  \w    -83.00   1.00   1.00   14.00    --  -16.10 -57.00-180.00   84
  4  \w     36.00  89.00   1.00   14.00    --   17.35 178.00 120.00   53
  5  \w    -25.00  26.00   1.00   14.00    --   17.35 -19.00 -90.00   51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0131245000
_diffrn_orient_matrix_UB_12      0.0136682000
_diffrn_orient_matrix_UB_13      0.0248314000
_diffrn_orient_matrix_UB_21      0.0047783000
_diffrn_orient_matrix_UB_22      0.0264647000
_diffrn_orient_matrix_UB_23      -0.0127922000
_diffrn_orient_matrix_UB_31      -0.0389054000
_diffrn_orient_matrix_UB_32      0.0078614000
_diffrn_orient_matrix_UB_33      -0.0000598000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0425
_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       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            58392
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.413
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_description       block
_exptl_crystal_F_000             5952
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.740
_refine_diff_density_min         -2.950
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         18116
_refine_ls_number_restraints     5886
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+111.9589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14064
_reflns_number_total             18116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01851e2.cif
_cod_data_source_block           1-Er
_cod_database_code               7708270
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
C8 \\sim C23 \\sim C50 \\sim C31 \\sim C15 \\sim C1 \\sim C43 \\sim C30 \\sim
C38 \\sim C39 \\sim C9 \\sim C49 \\sim C37 \\sim C29 \\sim C20 \\sim C10 \\sim
C6 \\sim C24 \\sim C47 \\sim C40 \\sim C3 \\sim C36 \\sim C16 \\sim C19 \\sim
C33 \\sim C48 \\sim C28 \\sim C34 \\sim C11 \\sim C44 \\sim C26 \\sim C17 \\sim
C18 \\sim C12 \\sim C35 \\sim C21 \\sim C46 \\sim C14 \\sim C27 \\sim C5 \\sim
C7 \\sim C25 \\sim C4 \\sim C42 \\sim C2 \\sim C41 \\sim C32 \\sim C45 \\sim
C13 \\sim C56 \\sim C54 \\sim C55 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim
C61 \\sim C63 \\sim C62 \\sim C64 \\sim C73 \\sim C71 \\sim C72 \\sim C76 \\sim
C74 \\sim C75 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C87 \\sim C86:
within 10A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 10A
Uanis(C57) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(O34)
\\sim Ueq, Uanis(O36) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(N6)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Rotating group:
 O12(H12A,H12B), O4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C48(H48), C28(H28), C11(H11), C17(H17), C21(H21), C14(H14), C7(H7),
 C25(H25), C2(H2), C41(H41), C32(H32), C45(H45), C13(H13), C57(H57), C61(H61),
 C73(H73), C76(H76), C83(H83), C87(H87)
3.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C63(H63A,H63B,H63C), C62(H62A,
 H62B,H62C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,H74B,H74C),
 C75(H75A,H75B,H75C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), C84(H84A,H84B,
 H84C), C86(H86A,H86B,H86C)
;
_shelx_res_checksum              78101
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.514
_oxdiff_exptl_absorpt_empirical_full_min 0.547