Magnetic hysteresis and large coercivity in bisbenzimidazole radical-bridged dilanthanide complexes.
Benner, Florian; La Droitte, Léo; Cador, Olivier; Le Guennic, Boris; Demir, Selvan; Chemical science 14 (2023) 5577–5592; doi:10.1039/d3sc01562a

data_1569017
_publ_section_title
;
 Magnetic hysteresis and large coercivity in bisbenzimidazole
 radical-bridged dilanthanide complexes.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              5577
_journal_page_last               5592
_journal_paper_doi               10.1039/d3sc01562a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C54 H68 N4 Tb2, C18 H36 K N2 O6, C4 H7 O, 2(C4 H8 O)'
_chemical_formula_sum            'C84 H127 K N6 O9 Tb2'
_chemical_formula_weight         1721.85
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-01 deposited with the CCDC.	2023-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                81.6460(10)
_cell_angle_beta                 81.5260(10)
_cell_angle_gamma                74.9200(10)
_cell_formula_units_Z            2
_cell_length_a                   12.99810(10)
_cell_length_b                   18.0236(2)
_cell_length_c                   18.9237(2)
_cell_measurement_reflns_used    51604
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.9720
_cell_measurement_theta_min      2.5650
_cell_volume                     4207.27(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.809
_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    -56.00  24.00   0.50    4.00    --    4.98 -67.00   0.00  160
  2  \w    -14.00  75.00   0.50    4.00    --    4.98  67.00 134.00  178
  3  \w      0.00  25.00   0.50    4.00    --    4.98 -77.00 -90.00   50
  4  \w      0.00  25.00   0.50    4.00    --    4.98 -77.00 -60.00   50
  5  \w     -8.00  19.00   0.50    4.00    --    4.98  51.00 -44.55   54
  6  \w      0.00  28.00   0.50    4.00    --    4.98 -77.00 150.00   56
  7  \w      0.00  26.00   0.50    4.00    --    4.98 -77.00-120.00   52
  8  \w      2.00  28.00   0.50    4.00    --    4.98 -77.00 -30.00   52
  9  \w     -8.00  20.00   0.50    4.00    --    4.98 -57.00  90.00   56
 10  \w     -2.00  40.00   0.50    4.00    --    4.98  37.00 120.00   84
 11  \w      0.00  25.00   0.50    4.00    --    4.98 -77.00  90.00   50
 12  \w    -29.00   2.00   0.50    4.00    --   -5.29 -37.00-180.00   62
 13  \w    -28.00  -2.00   0.50    4.00    --   -5.29  77.00-120.00   52
 14  \w    -40.00   0.00   0.50    4.00    --   -5.29 -37.00-120.00   80
 15  \w    -27.00  -2.00   0.50    4.00    --   -5.29  77.00 -60.00   50
 16  \w    -13.00  12.00   0.50    4.00    --   -5.29  57.00   0.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0534954000
_diffrn_orient_matrix_UB_12      0.0194654000
_diffrn_orient_matrix_UB_13      0.0112606000
_diffrn_orient_matrix_UB_21      0.0184176000
_diffrn_orient_matrix_UB_22      0.0149811000
_diffrn_orient_matrix_UB_23      0.0270925000
_diffrn_orient_matrix_UB_31      0.0059691000
_diffrn_orient_matrix_UB_32      0.0328472000
_diffrn_orient_matrix_UB_33      -0.0243623000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.809
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            79545
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.809
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.002
_diffrn_reflns_theta_min         2.068
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.773
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             1788
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.131
_refine_diff_density_max         9.647
_refine_diff_density_min         -6.477
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     921
_refine_ls_number_reflns         21689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+33.8377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18462
_reflns_number_total             21689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01562a2.cif
_cod_data_source_block           fb445_tbbbimrad_k2_042522_2_corr
_cod_depositor_comments
'Adding full bibliography for 1569012--1569017.cif.'
_cod_database_code               1569017
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C84H104N6O6Tb2K
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.566
_diffrn_oxdiff_digest_frames
;
01f06d4cb6a6138baa62c863007a7cfc5b011365d79
;
_diffrn_oxdiff_digest_hkl
;
0114988ac1f9e3e76c790502ac264c79df626e
;
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H74A(0.5) H74B(0.5) C77(0.4) H77A(0.4) H77B(0.4) C78(0.4)
 H78A(0.4) H78B(0.4) C79(0.4) H79A(0.4) H79B(0.4) C80(0.4) H80A(0.4) H80B(0.4)
 C81(0.6) H81A(0.6) H81B(0.6) C82(0.6) H82A(0.6) H82B(0.6) C83(0.6) H83A(0.6)
 H83B(0.6) C84(0.6) H84A(0.6) H84B(0.6) O9(0.75) O10(0.25) C85(0.25) H85A(0.25)
 H85B(0.25) C86(0.25) H86A(0.25) H86B(0.25) C87(0.25) H87A(0.25) H87B(0.25)
 H88A(0.75) H88B(0.75) H88C(0.25) H88D(0.25) C89(0.75) H89A(0.75) H89B(0.75)
 C90(0.75) H90A(0.75) H90B(0.75) C91(0.75) H91A(0.75) H91B(0.75)
3.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,
 H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B),
  C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,
 H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
 C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B),
  C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,
 H87B), C88(H88A,H88B), C88(H88C,H88D), C89(H89A,H89B), C90(H90A,H90B),
 C91(H91A,H91B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              8498
_shelx_fab_checksum              83590
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.286
_oxdiff_exptl_absorpt_empirical_full_min 0.857