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_1569013
_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 Gd2 N4, 2(C7 H8)'
_chemical_formula_sum            'C68 H84 Gd2 N4'
_chemical_formula_weight         1271.89
_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                 116.3370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.5900(2)
_cell_length_b                   13.65900(10)
_cell_length_c                   15.5654(2)
_cell_measurement_reflns_used    9030
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.5020
_cell_measurement_theta_min      3.1690
_cell_volume                     2970.51(6)
_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      99.99(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 0.972
_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     -8.00  50.00   0.50    0.64    --   47.70 -66.00  83.00  116
  2  \w     42.00  76.00   0.50    3.00    --  107.11 -66.00  83.00   68
  3  \w     35.00  75.00   0.50    3.00    --  107.11 -99.00 150.00   80
  4  \w     79.00 104.00   0.50    3.00    --  107.11 -99.00 150.00   50
  5  \w     39.00  65.00   0.50    3.00    --  107.11 -57.00 150.00   52
  6  \w    122.00 168.00   0.50    3.00    --  107.11  37.00 150.00   92
  7  \w    137.00 177.00   0.50    3.00    --  107.11  77.00 -30.00   80
  8  \w    148.00 178.00   0.50    3.00    --  107.11  19.00 -60.00   60
  9  \w    132.00 162.00   0.50    3.00    --  107.11  57.00 -90.00   60
 10  \w    113.00 139.00   0.50    3.00    --  107.11  19.00 -60.00   52
 11  \w     94.00 178.00   0.50    3.00    --  107.11  66.00-142.00  168
 12  \w     51.00  76.00   0.50    0.64    --   47.70  66.00-142.00   50
 13  \w     38.00  64.00   0.50    3.00    --  107.11 -57.00 -60.00   52
 14  \w     35.00  75.00   0.50    3.00    --  107.11 -99.00 -30.00   80
 15  \w     36.00 108.00   0.50    3.00    --  107.11-125.00 -60.00  144
 16  \w     37.00  62.00   0.50    3.00    --  107.11 -57.00-150.00   50
 17  \w    -23.00   3.00   0.50    0.64    --   47.70 -19.00-150.00   52
 18  \w    -65.00  21.00   0.50    0.64    --  -47.70  66.00-142.00  172
 19  \w    -71.00 -46.00   0.50    3.00    --  -86.25  66.00-142.00   50
 20  \w    -82.00 -30.00   0.50    0.64    --  -47.70 125.00   0.00  104
 21  \w   -157.00-127.00   0.50    3.00    --  -86.25 -57.00 120.00   60
 22  \w   -137.00-112.00   0.50    3.00    --  -86.25 -66.00  83.00   50
 23  \w   -113.00 -38.00   0.50    0.64    --  -47.70 -66.00  83.00  150
 24  \w     35.00 104.00   0.50    3.00    --  107.11 -99.00  30.00  138
 25  \w   -154.00-120.00   0.50    3.00    --  -86.25 -99.00 150.00   68
;
_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      -0.0667410000
_diffrn_orient_matrix_UB_12      0.0747660000
_diffrn_orient_matrix_UB_13      0.0140618000
_diffrn_orient_matrix_UB_21      0.0267545000
_diffrn_orient_matrix_UB_22      -0.0423319000
_diffrn_orient_matrix_UB_23      0.1004434000
_diffrn_orient_matrix_UB_31      0.0835452000
_diffrn_orient_matrix_UB_32      0.0731218000
_diffrn_orient_matrix_UB_33      0.0436567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10923
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.013
_diffrn_reflns_theta_min         3.168
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.601
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.311
_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    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+7.9403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3111
_reflns_number_total             3184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01562a2.cif
_cod_data_source_block           fb316_gdbbim_cell_check
_cod_depositor_comments
'Adding full bibliography for 1569012--1569017.cif.'
_cod_original_cell_volume        2970.50(6)
_cod_database_code               1569013
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C68 H84 N2 Gd2'
_shelx_estimated_absorpt_t_max   0.629
_shelx_estimated_absorpt_t_min   0.269
_diffrn_oxdiff_digest_frames
;
018bc6ce0904a31ed1608fc06866fcc8c102098d1e2
;
_diffrn_oxdiff_digest_hkl
;
011a4f0015b55d5ec49e2411120a08a9575628
;
_reflns_odcompleteness_completeness 100.00
_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: C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) C16(0.5) H16A(0.5)
 H16B(0.5) H16C(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C20(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C25(H25), C26(H26), C27(H27)
3.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              23926
_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 1.194
_oxdiff_exptl_absorpt_empirical_full_min 0.826