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_1569012
_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 Dy2 N4, C18 H36 K N2 O6, 3(C4 H8 O)'
_chemical_formula_sum            'C84 H128 Dy2 K N6 O9'
_chemical_formula_weight         1730.02
_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             2020-04-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-04-15 deposited with the CCDC.	2023-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                81.4010(10)
_cell_angle_beta                 80.9190(10)
_cell_angle_gamma                74.9370(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0586(2)
_cell_length_b                   18.1083(3)
_cell_length_c                   18.9686(2)
_cell_measurement_reflns_used    54475
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.4650
_cell_measurement_theta_min      1.6420
_cell_volume                     4249.30(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -53.75 145.75   0.50   45.54    --  -28.00  73.76 -25.75  399
  2  \w    -53.75 145.75   0.50   45.54    --  -28.00  73.76  34.25  399
  3  \w    -53.75 145.75   0.50   45.54    --  -28.00  73.76  94.25  399
  4  \w    -53.75 145.75   0.50   45.54    --  -28.00  73.76 154.25  399
  5  \w    -53.75 145.75   0.50   45.54    --  -28.00  73.76-145.75  399
  6  \w    -53.75 145.75   0.50   45.54    --  -28.00  73.76 -85.75  399
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0358751000
_diffrn_orient_matrix_UB_12      0.0369137000
_diffrn_orient_matrix_UB_13      -0.0022198000
_diffrn_orient_matrix_UB_21      0.0397114000
_diffrn_orient_matrix_UB_22      0.0162429000
_diffrn_orient_matrix_UB_23      0.0086666000
_diffrn_orient_matrix_UB_31      0.0187056000
_diffrn_orient_matrix_UB_32      0.0063667000
_diffrn_orient_matrix_UB_33      -0.0370507000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            73354
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.628
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             1794
_exptl_crystal_recrystallization_method 'used as recieved'
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.144
_refine_diff_density_max         2.109
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.140
_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     856
_refine_ls_number_reflns         17324
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+24.6987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1308
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15886
_reflns_number_total             17324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01562a2.cif
_cod_data_source_block           average
_cod_depositor_comments
'Adding full bibliography for 1569012--1569017.cif.'
_cod_database_code               1569012
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C73H104Dy1K1N4O6
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C77-C78 \\sim C78-C79 \\sim C79-C80
 with sigma of 0.02
 C78-C80 \\sim C77-C79
 with sigma of 0.04
 O8-C77 \\sim O8-C80
 with sigma of 0.02
 O8-C78 \\sim O8-C79
 with sigma of 0.04
 O9-C1B \\sim O9-C1C
 with sigma of 0.04
 C1B-C1D \\sim C1A-C1C
 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D
 with sigma of 0.02
 O9-C1A \\sim O9-C1D
 with sigma of 0.02
 O10-C1E \\sim O10-C1H
 with sigma of 0.02
 C1E-C1F \\sim C1F-C1G \\sim C1G-C1H
 with sigma of 0.02
 O10-C1F \\sim O10-C1G
 with sigma of 0.04
 C1F-C1H \\sim C1E-C1G
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O8 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O9 \\sim C1A \\sim C1B \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O10 \\sim C1E \\sim C1F \\sim C1G \\sim C1H: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uiso(O10) = Uiso(O9)
Uiso(C1G) = Uiso(C1C)
4. Rigid body (RIGU) restrains
 O8, C77, C78, C79, C80
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, C1E, C1F, C1G, C1H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O10)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(C1G)=
 Sof(H1GA)=Sof(H1GB)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=1-FVAR(1)
 Sof(O9)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1C)=
 Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=FVAR(1)
6.a Free rotating group:
 O8(C77,C78,C79,C80), O9(C1A,C1B,C1C,C1D), O10(C1E,C1F,C1G,C1H)
6.b 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), C1A(H1AA,H1AB), C1B(H1BA,H1BB),
  C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,H1EB), C1F(H1FA,H1FB), C1G(H1GA,
 H1GB), C1H(H1HA,H1HB)
6.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C43(H43), C44(H44), C45(H45), C50(H50), C51(H51), C52(H52), C53(H53)
6.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C6AA(H6AA,H6AB,H6AC), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
  C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              45529
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id FB227THF2_101919
_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 1.208
_oxdiff_exptl_absorpt_empirical_full_min 0.885