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_1569015
_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, 2(C7 H8)'
_chemical_formula_sum            'C68 H84 N4 Tb2'
_chemical_formula_weight         1275.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-14 deposited with the CCDC.	2023-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 149.942(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.9083(18)
_cell_length_b                   13.6251(2)
_cell_length_c                   15.5343(10)
_cell_measurement_reflns_used    8374
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.8150
_cell_measurement_theta_min      3.1630
_cell_volume                     2958.7(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.965
_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     49.00  74.00   0.50    0.95    --   47.70  74.00  32.00   50
  2  \w     86.00 178.00   0.50    3.81    --  107.11  74.00  32.00  184
  3  \w    140.00 177.00   0.50    3.81    --  107.11  57.00  90.00   74
  4  \w    117.00 174.00   0.50    3.81    --  107.11  37.00 -30.00  114
  5  \w    143.00 178.00   0.50    3.81    --  107.11  77.00 -90.00   70
  6  \w     47.00  80.00   0.50    3.81    --  107.11 -74.00 -95.00   66
  7  \w     37.00  65.00   0.50    3.81    --  107.11 -57.00 -30.00   56
  8  \w     39.00  65.00   0.50    3.81    --  107.11 -57.00  30.00   52
  9  \w     35.00  61.00   0.50    3.81    --  107.11 -57.00  60.00   52
 10  \w     40.00  76.00   0.50    3.81    --  107.11-125.00 120.00   72
 11  \w     77.00 102.00   0.50    3.81    --  107.11-125.00 120.00   50
 12  \w     35.00  65.00   0.50    3.81    --  107.11 -57.00 150.00   60
 13  \w     42.00 104.00   0.50    3.81    --  107.11 -99.00 -30.00  124
 14  \w     52.00 102.00   0.50    3.81    --  107.11-125.00 -90.00  100
 15  \w     37.00  65.00   0.50    3.81    --  107.11 -57.00-180.00   56
 16  \w      1.00  26.00   0.50    0.95    --   47.70 -74.00 -95.00   50
 17  \w    -25.00  25.00   0.50    0.95    --   47.70 -19.00 -90.00  100
 18  \w    -26.00  15.00   0.50    0.95    --   47.70 -19.00-150.00   82
 19  \w     38.00  63.00   0.50    3.81    --  107.11 -57.00 -60.00   50
 20  \w    -69.00  19.00   0.50    0.95    --  -47.70  74.00  32.00  176
 21  \w    -39.00 -14.00   0.50    3.81    --  -86.25  37.00-120.00   50
 22  \w    -78.00 -24.00   0.50    3.81    --  -86.25  74.00  32.00  108
 23  \w   -113.00 -27.00   0.50    0.95    --  -47.70 -74.00 -95.00  172
 24  \w   -136.00-111.00   0.50    3.81    --  -86.25 -74.00 -95.00   50
 25  \w   -159.00-133.00   0.50    3.81    --  -86.25 -57.00   0.00   52
 26  \w   -158.00-132.00   0.50    3.81    --  -86.25 -77.00 -30.00   52
;
_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      -0.0313275000
_diffrn_orient_matrix_UB_12      0.0792548000
_diffrn_orient_matrix_UB_13      0.0162052000
_diffrn_orient_matrix_UB_21      -0.0995509000
_diffrn_orient_matrix_UB_22      -0.0480146000
_diffrn_orient_matrix_UB_23      -0.1485413000
_diffrn_orient_matrix_UB_31      0.0355013000
_diffrn_orient_matrix_UB_32      -0.0647440000
_diffrn_orient_matrix_UB_33      0.1299069000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11155
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.208
_diffrn_reflns_theta_min         3.174
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.915
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.411
_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            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       block
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0251
_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^)+(0.0196P)^2^+10.2906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3052
_reflns_number_total             3155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01562a2.cif
_cod_data_source_block           fb315_tbbbim_5_cell_check
_cod_depositor_comments
'Adding full bibliography for 1569012--1569017.cif.'
_cod_original_cell_volume        2958.7(8)
_cod_database_code               1569015
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C68H84N4Tb2
_shelx_estimated_absorpt_t_max   0.560
_shelx_estimated_absorpt_t_min   0.346
_diffrn_oxdiff_digest_frames
;
01b582c51b2d0432e1f422e9b0bbe32c4d02122c543
;
_diffrn_oxdiff_digest_hkl
;
01743b24eef3a4245fb088edba31b018278de1
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2. Others
 Fixed Sof: C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) H23A(0.5) H23B(0.5)
 H23C(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 H16C(0.5) C14(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C20(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C18(0.5) H18A(0.5) H18B(0.5)
 H18C(0.5) C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C13(0.5) H13A(0.5) H13B(0.5)
 H13C(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C4(H4), C27(H27), C5(H5), C25(H25), C26(H26)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C17(H17A,H17B,H17C), C16(H16A,H16B,
 H16C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C18(H18A,
 H18B,H18C), C22(H22A,H22B,H22C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              49113
_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 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.810