Exploring magnetic anisotropy and exchange coupling in FeIII2DyIII heterotrimetallic assemblies displaying slow relaxation of magnetization
Panja, Anangamohan; Jagličić, Zvonko; Jana, Narayan Ch.; Contesso, Scarlette; Brandão, Paula; Aravena, Daniel; New Journal of Chemistry 49 (2025) 19605–19615; doi:10.1039/D5NJ03857J

data_7064088
_publ_section_title
;
 Exploring magnetic anisotropy and exchange coupling in FeIII2DyIII
 heterotrimetallic assemblies displaying slow relaxation of magnetization
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19605
_journal_page_last               19615
_journal_paper_doi               10.1039/D5NJ03857J
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C60 H56 Dy Fe2 N4.5 O16.5, 2(H2 O), 0.5(N O)'
_chemical_formula_sum            'C60 H60 Dy Fe2 N5 O19'
_chemical_formula_weight         1429.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-10-22
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-10-23 deposited with the CCDC.	2025-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.547(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9305(6)
_cell_length_b                   12.5854(3)
_cell_length_c                   25.8640(7)
_cell_measurement_reflns_used    11309
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      77.8180
_cell_measurement_theta_min      3.8910
_cell_volume                     5649.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.963
_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    -80.00   3.00   0.50    0.19    --  -38.50 114.00 -45.00  166
  2  \w   -108.00 -33.00   0.50    0.19    --  -38.50 175.00  92.00  150
  3  \w     19.00  90.00   0.50    0.19    --   49.06-114.00-136.00  142
  4  \w     55.00 119.00   0.50    0.19    --   49.06-175.00  84.00  128
  5  \w     43.00 109.00   0.50    1.12    --  107.46-114.00-136.00  132
  6  \w     55.00 149.00   0.50    1.12    --  107.46-175.00  84.00  188
  7  \w     63.00 147.00   0.50    1.12    --  107.46 175.00  92.00  168
  8  \w   -101.00 -27.00   0.50    0.19    --  -38.50 -57.00 -90.00  148
  9  \w     48.00 116.00   0.50    0.19    --   49.06  37.00  90.00  136
 10  \w     54.00  94.00   0.50    0.19    --   49.06-125.00  60.00   80
 11  \w     47.00 115.00   0.50    1.12    --  107.46 -61.00   0.00  136
 12  \w     56.00  95.00   0.50    1.12    --  107.46-125.00 -30.00   78
 13  \w     44.00 129.00   0.50    1.12    --  107.46 -77.00 120.00  170
 14  \w     40.00 104.00   0.50    1.12    --  107.46 -94.00 120.00  128
 15  \w    112.00 166.00   0.50    1.12    --  107.46  45.00 -90.00  108
 16  \w     99.00 149.00   0.50    1.12    --  107.46 125.00   0.00  100
 17  \w    105.00 166.00   0.50    1.12    --  107.46  45.00 -30.00  122
 18  \w     44.00 106.00   0.50    1.12    --  107.46 -45.00 -30.00  124
 19  \w    110.00 170.00   0.50    1.12    --  107.46  45.00  30.00  120
 20  \w    103.00 171.00   0.50    1.12    --  107.46  77.00-150.00  136
 21  \w    104.00 132.00   0.50    1.12    --  107.46 114.00 -45.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23073
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.255
_diffrn_reflns_theta_min         3.531
_exptl_absorpt_coefficient_mu    11.737
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       block
_exptl_crystal_F_000             2900
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         5850
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0338
_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^)+(0.0348P)^2^+15.6847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5216
_reflns_number_total             5850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03857j2.cif
_cod_data_source_block           complex-1
_cod_depositor_comments
'Adding full bibliography for 7064086--7064089.cif.'
_cod_database_code               7064088
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.387
_shelx_estimated_absorpt_t_min   0.202
_olex2_refinement_description
;
1. Restrained distances
 O11-H11A = O11-H11B
 0.87 with sigma of 0.02
 O7-H7A = O7-H7B
 0.87 with sigma of 0.02
 H11A-H11B
 1.38 with sigma of 0.04
 H7A-H7B
 1.38 with sigma of 0.04
 N3-O8 \\sim N3-O12
 with sigma of 0.0002
 Dy1-H7A \\sim Dy1-H7B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
O9 \\sim N3 \\sim N4 \\sim O10 \\sim O12: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008 within 1.7A
3. Rigid body (RIGU) restrains
 O9, O10, O12, N4, N3, O8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: N3(0.25) O9(0.5) O10(0.25) O8(0.5) N4(0.25) O12(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C26(H26), C22(H22), C9(H9), C14(H14), C27(H27), C24(H24), C13(H13),
 C28(H28), C7(H7), C19(H19), C12(H12), C29(H29), C11(H11)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C18(H18A,H18B,H18C), C6(H6A,H6B,H6C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              77190
_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
;