Backbone-integrated triplet radicals in linear 2p-3d-4f heterometallic chains and magnetic hysteresis
Tsukii, Shota; Haga, Nagito; Takano, Rina; Ishida, Takayuki; Chemical Communications  (2026) –; doi:10.1039/D6CC01045H

data_7135635
_publ_section_title
;
 Backbone-integrated triplet radicals in linear 2p-3d-4f heterometallic
 chains and magnetic hysteresis.
;
_journal_issue                   28
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7343
_journal_page_last               7347
_journal_paper_doi               10.1039/d6cc01045h
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C55 H47 Co Dy F36 N4 O14'
_chemical_formula_sum            'C55 H47 Co Dy F36 N4 O14'
_chemical_formula_weight         1893.39
_chemical_name_common            '[Dy(hfac)3(5TFPBN)Co(hfac)2(5TFPBN)]n'
_chemical_name_systematic        3DyCo
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2026-01-21
_audit_creation_method
;
Olex2 1.5-ac5-018
(compiled 2021.09.08 svn.r13c46975 for Rigaku Oxford Diffraction, GUI svn.r6396)
;
_audit_update_record
;
2026-01-21 deposited with the CCDC.	2026-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.103(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.3349(10)
_cell_length_b                   11.4206(5)
_cell_length_c                   20.2951(7)
_cell_measurement_reflns_used    11796
_cell_measurement_temperature    99.9(2)
_cell_measurement_theta_max      31.6540
_cell_measurement_theta_min      2.4730
_cell_volume                     7452.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 42.72a 64-bit (release 07-10-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-018 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(2)
_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 0.805
_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    -52.00  -1.00   0.50    2.98    --   -5.30   0.00-180.00  102
  2  \w     -5.00  28.50   0.50    2.98    --    4.52 -99.00  60.00   67
  3  \w    -35.00  19.00   0.50    2.98    --   -5.30 -86.00  19.00  108
  4  \w    -44.00   9.00   0.50    2.98    --    4.52   0.00 120.00  106
  5  \w    -13.00  41.00   0.50    2.98    --   -5.30  86.00 137.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0128797352
_diffrn_orient_matrix_UB_12      0.0114653389
_diffrn_orient_matrix_UB_13      0.0254412702
_diffrn_orient_matrix_UB_21      -0.0059986631
_diffrn_orient_matrix_UB_22      0.0542020035
_diffrn_orient_matrix_UB_23      -0.0151992332
_diffrn_orient_matrix_UB_31      -0.0168766317
_diffrn_orient_matrix_UB_32      -0.0280706057
_diffrn_orient_matrix_UB_33      -0.0188983010
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.805
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34265
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.882
_diffrn_reflns_theta_min         2.113
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       block
_exptl_crystal_F_000             3736
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: heptane-dichloromethane'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.803
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         10305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0403P)^2^+4.9085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7412
_reflns_number_total             10305
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc01045h2.cif
_cod_data_source_block           20260120_dycomtfmpbn_v3
_cod_depositor_comments
'Adding full bibliography for 7135632--7135638.cif.'
_cod_database_code               7135635
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C55 H47 Co Dy F36 N4 O14'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.801
_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
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C18(H18), C23(H23), C26(H26)
3.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              33117
_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 1.834
_oxdiff_exptl_absorpt_empirical_full_min 0.448