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_1569016
_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, C18 H36 K N2 O6, 3(C4 H8 O)'
_chemical_formula_sum            'C84 H128 Gd2 K N6 O9'
_chemical_formula_weight         1719.52
_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     iterative
_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                81.5150(10)
_cell_angle_beta                 81.5720(10)
_cell_angle_gamma                74.8530(10)
_cell_formula_units_Z            2
_cell_length_a                   13.00780(10)
_cell_length_b                   18.0377(2)
_cell_length_c                   18.9498(2)
_cell_measurement_reflns_used    47878
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.9430
_cell_measurement_theta_min      2.2770
_cell_volume                     4217.51(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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.816
_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    -14.00  19.00   0.50    1.40    --    5.06 -57.00 -90.00   66
  2  \w      1.00  27.00   0.50    1.40    --    5.06 -77.00 -30.00   52
  3  \w    -15.00  13.00   0.50    1.40    --    5.06 -57.00   0.00   56
  4  \w    -51.00   3.00   0.50    1.40    --    5.06 -19.00-120.00  108
  5  \w      1.00  28.00   0.50    1.40    --    5.06 -77.00  30.00   54
  6  \w    -13.00  13.00   0.50    1.40    --    5.06 -57.00 120.00   52
  7  \w    -77.00 -37.00   0.50    1.40    --   -5.37   0.00  60.00   80
  8  \w    -42.00   3.00   0.50    1.40    --   -5.37 -37.00   0.00   90
  9  \w    -27.00   0.00   0.50    1.40    --   -5.37  77.00 120.00   54
 10  \w     -5.00  62.00   0.50    1.40    --   -5.37   0.00  60.00  134
 11  \w    -20.00  15.00   0.50    1.40    --   -5.37  57.00-180.00   70
 12  \w     -4.00  34.00   0.50    1.40    --    5.06  37.00-120.00   76
 13  \w    -10.00  16.00   0.50    1.40    --    5.06  56.00 -60.12   52
 14  \w     -8.00  19.00   0.50    1.40    --    5.06  53.00 -15.58   54
 15  \w     -9.00  20.00   0.50    1.40    --    5.06  52.00  71.45   58
 16  \w     -4.00  22.00   0.50    1.40    --    5.06  50.00  94.94   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78556
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.955
_diffrn_reflns_theta_min         2.466
_exptl_absorpt_coefficient_mu    1.665
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.496
_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    1.354
_exptl_crystal_description       block
_exptl_crystal_F_000             1786
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.313
_exptl_crystal_size_min          0.269
_refine_diff_density_max         4.827
_refine_diff_density_min         -2.514
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     978
_refine_ls_number_reflns         21844
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0455P)^2^+11.0478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18560
_reflns_number_total             21844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01562a2.cif
_cod_data_source_block           fb486_gdbbim_k2_2_042522_corr2
_cod_depositor_comments
'Adding full bibliography for 1569012--1569017.cif.'
_cod_database_code               1569016
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.663
_shelx_estimated_absorpt_t_min   0.440
_olex2_refinement_description
;
1. Others
 Fixed Sof: O7(0.75) O8(0.25) C73(0.25) H73A(0.25) H73B(0.25) C74(0.25)
 H74A(0.25) H74B(0.25) C75(0.25) H75A(0.25) H75B(0.25) C76(0.25) H76A(0.25)
 H76B(0.25) C77(0.75) H77A(0.75) H77B(0.75) C78(0.75) H78A(0.75) H78B(0.75)
 C79(0.75) H79A(0.75) H79B(0.75) C80(0.75) H80A(0.75) H80B(0.75) O9(0.5)
 C81(0.5) H81A(0.5) H81B(0.5) C82(0.5) H82A(0.5) H82B(0.5) C83(0.5) H83A(0.5)
 H83B(0.5) C84(0.5) H84A(0.5) H84B(0.5) O10(0.5) C85(0.5) H85A(0.5) H85B(0.5)
 C86(0.5) H86A(0.5) H86B(0.5) C87(0.5) H87A(0.5) H87B(0.5) C88(0.5) H88A(0.5)
 H88B(0.5) O11(0.5) C89(0.5) H89A(0.5) H89B(0.5) C90(0.5) H90A(0.5) H90B(0.5)
 C91(0.5) H91A(0.5) H91B(0.5) C92(0.5) H92A(0.5) H92B(0.5) O12(0.5) C93(0.5)
 H93A(0.5) H93B(0.5) C94(0.5) H94A(0.5) H94B(0.5) C95(0.5) H95A(0.5) H95B(0.5)
 C96(0.5) H96A(0.5) H96B(0.5)
 Fixed Uiso: H22A(0.043) H22B(0.043) H22C(0.043) H23A(0.046) H23B(0.046)
 H23C(0.046) H73A(0.054) H73B(0.054) H74A(0.067) H74B(0.067) H75A(0.079)
 H75B(0.079) H76A(0.152) H76B(0.152) H77A(0.075) H77B(0.075) H78A(0.083)
 H78B(0.083) H79A(0.083) H79B(0.083) H80A(0.101) H80B(0.101) H81A(0.111)
 H81B(0.111) H82A(0.1) H82B(0.1) H83A(0.1) H83B(0.1) H84A(0.1) H84B(0.1)
 H85A(0.068) H85B(0.068) H86A(0.1) H86B(0.1) H87A(0.1) H87B(0.1) H88A(0.1)
 H88B(0.1) H89A(0.138) H89B(0.138) H90A(0.138) H90B(0.138) H91A(0.138)
 H91B(0.138) H92A(0.138) H92B(0.138) H93A(0.138) H93B(0.138) H94A(0.138)
 H94B(0.138) H95A(0.138) H95B(0.138) H96A(0.138) H96B(0.138)
 Fixed X: H4(-0.2184) H5(-0.2517) H6(-0.1112) H7(0.0683) H10(0.4863)
 H11(0.5221) H12(0.3836) H13(0.2028) H20A(-0.2949) H20B(-0.3538) H20C(-0.3485)
 H21A(-0.0341) H21B(-0.1579) H21C(-0.1241) H22A(0.1194) H22B(0.0564)
 H22C(0.0935) H23A(-0.0748) H23B(-0.0148) H23C(0.0401) H24A(-0.3103) H24B(-
 0.3204) H24C(-0.2363) H30A(-0.2198) H30B(-0.1654) H30C(-0.0993) H31A(0.0766)
 H31B(0.1016) H31C(0.1547) H32A(0.1604) H32B(0.1041) H32C(0.0886) H33A(-0.0989)
 H33B(-0.1297) H33C(-0.2174) H34A(-0.3228) H34B(-0.324) H34C(-0.3217)
 H40A(0.2533) H40B(0.2777) H40C(0.3659) H41A(0.16) H41B(0.2102) H41C(0.1568)
 H42A(0.3617) H42B(0.4215) H42C(0.2944) H43A(0.6062) H43B(0.6253) H43C(0.5581)
 H44A(0.5175) H44B(0.5946) H44C(0.5909) H50A(0.5778) H50B(0.58) H50C(0.5866)
 H51A(0.336) H51B(0.4104) H51C(0.4588) H52A(0.0948) H52B(0.1529) H52C(0.1599)
 H53A(0.1829) H53B(0.1762) H53C(0.1056) H54A(0.4933) H54B(0.4023) H54C(0.38)
 H55A(0.2084) H55B(0.2903) H56A(0.1812) H56B(0.2318) H57A(0.2928) H57B(0.2458)
 H58A(0.4258) H58B(0.3836) H59A(0.55) H59B(0.6103) H60A(0.7138) H60B(0.6211)
 H61A(0.2914) H61B(0.2706) H62A(0.3841) H62B(0.4704) H63A(0.5839) H63B(0.4795)
 H64A(0.4971) H64B(0.5994) H65A(0.7049) H65B(0.6134) H66A(0.7913) H66B(0.8067)
 H67A(0.3548) H67B(0.4538) H68A(0.5056) H68B(0.4483) H69A(0.6283) H69B(0.6775)
 H70A(0.7782) H70B(0.8134) H71A(0.8819) H71B(0.8335) H72A(0.8573) H72B(0.7681)
 H73A(0.5077) H73B(0.5069) H74A(0.43) H74B(0.437) H75A(0.2452) H75B(0.2348)
 H76A(0.2469) H76B(0.2212) H77A(0.2949) H77B(0.3995) H78A(0.3861) H78B(0.2609)
 H79A(0.2666) H79B(0.3906) H80A(0.4222) H80B(0.3092) H81A(0.2699) H81B(0.3149)
 H82A(0.1819) H82B(0.2797) H83A(0.1775) H83B(0.0872) H84A(0.0608) H84B(0.02)
 H85A(0.2623) H85B(0.2415) H86A(0.2803) H86B(0.2296) H87A(0.1367) H87B(0.0946)
 H88A(0.0306) H88B(-0.0094) H89A(-0.0692) H89B(-0.0283) H90A(-0.0081)
 H90B(0.079) H91A(-0.0154) H91B(-0.0378) H92A(-0.1991) H92B(-0.2049) H93A(-
 0.2231) H93B(-0.1479) H94A(-0.0793) H94B(-0.0265) H95A(0.0563) H95B(0.0661)
 H96A(-0.0362) H96B(-0.0774)
 Fixed Y: H4(0.417) H5(0.5073) H6(0.5402) H7(0.4839) H10(0.1781) H11(0.0782)
 H12(0.0393) H13(0.0982) H20A(0.4035) H20B(0.4) H20C(0.3334) H21A(0.4391)
 H21B(0.4709) H21C(0.4467) H22A(0.2534) H22B(0.3209) H22C(0.3414) H23A(0.1214)
 H23B(0.1694) H23C(0.1336) H24A(0.2028) H24B(0.2295) H24C(0.1512) H30A(0.2766)
 H30B(0.2105) H30C(0.2693) H31A(0.2021) H31B(0.1113) H31C(0.1422) H32A(0.055)
 H32B(-0.0132) H32C(0.0256) H33A(0.0483) H33B(-0.0014) H33C(0.0705)
 H34A(0.1597) H34B(0.166) H34C(0.2401) H40A(0.4716) H40B(0.4287) H40C(0.4656)
 H41A(0.2734) H41B(0.2668) H41C(0.3499) H42A(0.1533) H42B(0.1216) H42C(0.1563)
 H43A(0.2495) H43B(0.195) H43C(0.1748) H44A(0.4363) H44B(0.3583) H44C(0.376)
 H50A(0.3544) H50B(0.4326) H50C(0.4294) H51A(0.3395) H51B(0.3932) H51C(0.3224)
 H52A(0.4762) H52B(0.4904) H52C(0.4041) H53A(0.5613) H53B(0.6157) H53C(0.5533)
 H54A(0.5223) H54B(0.5957) H54C(0.544) H55A(0.3999) H55B(0.434) H56A(0.3748)
 H56B(0.2935) H57A(0.2527) H57B(0.3404) H58A(0.3465) H58B(0.286) H59A(0.2161)
 H59B(0.2669) H60A(0.1362) H60B(0.1071) H61A(0.312) H61B(0.2648) H62A(0.1839)
 H62B(0.2346) H63A(0.1042) H63B(0.0702) H64A(0.0478) H64B(-0.0013) H65A(-
 0.0092) H65B(0.0437) H66A(0.0461) H66B(0.0856) H67A(0.4302) H67B(0.3587)
 H68A(0.4679) H68B(0.452) H69A(0.4339) H69B(0.4405) H70A(0.3087) H70B(0.3658)
 H71A(0.2569) H71B(0.1974) H72A(0.1635) H72B(0.2406) H73A(-0.0214) H73B(0.0582)
 H74A(0.1197) H74B(0.0397) H75A(0.0486) H75B(0.1358) H76A(0.1021) H76B(0.0248)
 H77A(0.0905) H77B(0.1245) H78A(0.1309) H78B(0.1408) H79A(0.0313) H79B(0.0232)
 H80A(-0.0725) H80B(-0.0381) H81A(-0.0156) H81B(0.0081) H82A(0.1096)
 H82B(0.1265) H83A(0.1487) H83B(0.1851) H84A(0.0723) H84B(0.0776) H85A(-0.0001)
 H85B(-0.0066) H86A(0.1122) H86B(0.1123) H87A(0.1699) H87B(0.1854) H88A(0.112)
 H88B(0.1255) H89A(0.1694) H89B(0.1621) H90A(0.2781) H90B(0.237) H91A(0.3102)
 H91B(0.3732) H92A(0.3362) H92B(0.3554) H93A(0.2835) H93B(0.215) H94A(0.3173)
 H94B(0.2262) H95A(0.2472) H95B(0.3223) H96A(0.3412) H96B(0.4011)
 Fixed Z: H4(0.7583) H5(0.6562) H6(0.5778) H7(0.5984) H10(0.8234) H11(0.9186)
 H12(0.9934) H13(0.9771) H20A(0.8928) H20B(0.9731) H20C(0.9245) H21A(0.9379)
 H21B(0.9659) H21C(0.8863) H22A(1.0185) H22B(1.0662) H22C(0.9829) H23A(1.0736)
 H23B(1.1112) H23C(1.0384) H24A(0.9873) H24B(1.0654) H24C(1.0457) H30A(0.718)
 H30B(0.6668) H30C(0.681) H31A(0.6892) H31B(0.6836) H31C(0.7408) H32A(0.8439)
 H32B(0.8402) H32C(0.913) H33A(0.973) H33B(0.9196) H33C(0.9495) H34A(0.8839)
 H34B(0.7989) H34C(0.8353) H40A(0.5477) H40B(0.4768) H40C(0.4989) H41A(0.6042)
 H41B(0.5224) H41C(0.5489) H42A(0.6988) H42B(0.6252) H42C(0.6338) H43A(0.6716)
 H43B(0.6091) H43C(0.684) H44A(0.5458) H44B(0.5192) H44C(0.6) H50A(0.7591)
 H50B(0.7885) H50C(0.704) H51A(0.9031) H51B(0.9158) H51C(0.8691) H52A(0.8269)
 H52B(0.8907) H52C(0.8757) H53A(0.6508) H53B(0.7117) H53C(0.724) H54A(0.6348)
 H54B(0.6586) H54C(0.6035) H55A(0.1473) H55B(0.1806) H56A(0.2719) H56B(0.2402)
 H57A(0.3628) H57B(0.3802) H58A(0.3904) H58B(0.4512) H59A(0.4686) H59B(0.4078)
 H60A(0.4294) H60B(0.4033) H61A(0.053) H61B(0.1298) H62A(0.0477) H62B(0.0408)
 H63A(0.0856) H63B(0.099) H64A(0.2248) H64B(0.1792) H65A(0.268) H65B(0.3183)
 H66A(0.3364) H66B(0.2555) H67A(0.0535) H67B(0.0366) H68A(0.0675) H68B(0.1473)
 H69A(0.1811) H69B(0.0983) H70A(0.1183) H70B(0.1622) H71A(0.2396) H71B(0.2075)
 H72A(0.3328) H72B(0.3493) H73A(0.45) H73B(0.3999) H74A(0.4831) H74B(0.5345)
 H75A(0.5314) H75B(0.4919) H76A(0.3934) H76B(0.4337) H77A(0.3576) H77B(0.3502)
 H78A(0.4715) H78B(0.4657) H79A(0.5265) H79B(0.5353) H80A(0.4633) H80B(0.4309)
 H81A(0.1833) H81B(0.2492) H82A(0.149) H82B(0.1823) H83A(0.2924) H83B(0.2385)
 H84A(0.3362) H84B(0.259) H85A(0.2657) H85B(0.185) H86A(0.2263) H86B(0.1538)
 H87A(0.2745) H87B(0.1972) H88A(0.3101) H88B(0.2322) H89A(0.4336) H89B(0.5111)
 H90A(0.3924) H90B(0.4475) H91A(0.5385) H91B(0.4691) H92A(0.5513) H92B(0.4661)
 H93A(0.4268) H93B(0.4742) H94A(0.3565) H94B(0.3751) H95A(0.4688) H95B(0.4128)
 H96A(0.5398) H96B(0.4722)
;
_shelx_res_checksum              59699
_shelx_fab_checksum              51829
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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
;