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_7064087
_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         'C76 H86 Dy Fe2 N5 O16, 9[H2O]'
_chemical_formula_sum            'C76 H104 Dy Fe2 N5 O25'
_chemical_formula_weight         1761.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 105.229(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6187(5)
_cell_length_b                   27.2829(8)
_cell_length_c                   18.6130(5)
_cell_measurement_reflns_used    31572
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      30.6380
_cell_measurement_theta_min      1.6390
_cell_volume                     8142.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.807
_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    -74.00   7.00   0.50    8.99    --   -4.60 -11.00 122.00  162
  2  \w    -16.00  65.00   0.50    8.99    --   -4.60  11.00 -64.00  162
  3  \w    -15.00  30.00   0.50    8.99    --   -4.60 -99.00 -90.00   90
  4  \w    -28.00  21.00   0.50    8.99    --   -4.60  77.00 150.00   98
  5  \w      0.00  70.00   0.50    8.99    --    3.35  37.00 -30.00  140
  6  \w    -71.00 -29.00   0.50    8.99    --   -4.60 -37.00 -30.00   84
;
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.807
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            94521
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.807
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.652
_diffrn_reflns_theta_min         1.875
_exptl_absorpt_coefficient_mu    1.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             3652
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.205
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         20308
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+13.7481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15240
_reflns_number_total             20308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03857j2.cif
_cod_data_source_block           complex-2
_cod_depositor_comments
'Adding full bibliography for 7064086--7064089.cif.'
_cod_database_code               7064087
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.776
_olex2_refinement_description
;
1. Restrained distances
 C71-C73 \\sim C75-C77 \\sim C74-C76
 with sigma of 0.004
 C72-C71 \\sim C72-C75 \\sim C72-C77 \\sim C72-C74 \\sim C72-C76 \\sim C72-C73
 with sigma of 0.002
 C36-C34 \\sim C36A-C34A
 with sigma of 0.004
 C32-C31 \\sim C32-C36 \\sim C32-C34 \\sim C32-C36A \\sim C32-C34A
 with sigma of 0.002
 C36-C34 \\sim C36-C33 \\sim C34-C33 \\sim C36A-C34A \\sim C36A-C35 \\sim
C34A-C35
 with sigma of 0.004
 C32-C31 \\sim C32-C36 \\sim C32-C34 \\sim C32-C36A \\sim C32-C34A \\sim
C32-C33 \\sim C32-C35
 with sigma of 0.002
2. Uiso/Uaniso restraints and constraints
C36A \\sim C36 \\sim C34A \\sim C34: within 1.7A with sigma of 0.004 and sigma
for terminal atoms of 0.008 within 1.7A
C34 \\sim C34A \\sim C36 \\sim C36A \\sim C33 \\sim C35: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008 within 1.7A
Uanis(C77) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C74)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36A) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C34A) \\sim Ueq, Uanis(C34)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C36A, C34, C34A, C36
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: C36(0.85) H36A(0.85) H36B(0.85) H36C(0.85) C75(0.5) H75A(0.5)
 H75B(0.5) H75C(0.5) C77(0.5) H77A(0.5) H77B(0.5) H77C(0.5) C74(0.5) H74A(0.5)
 H74B(0.5) H74C(0.5) C76(0.5) H76A(0.5) H76B(0.5) H76C(0.5) C34(0.85)
 H34A(0.85) H34B(0.85) H34C(0.85) C36A(0.15) H36D(0.15) H36E(0.15) H36F(0.15)
 C34A(0.15) H34D(0.15) H34E(0.15) H34F(0.15) C33(0.85) H33A(0.85) H33B(0.85)
 H33C(0.85) C35(0.15) H35A(0.15) H35B(0.15) H35C(0.15)
5.a Rotating group:
 O13(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C9(H9), C63(H63), C49(H49), C68(H68), C57(H57), C66(H66), C47(H47),
 C28(H28), C26(H26), C7(H7), C70(H70), C18(H18), C58(H58), C51(H51), C17(H17),
 C4(H4), C30(H30), C11(H11), C39(H39), C44(H44), C38(H38), C78(H78), C79(H79)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C62(H62A,H62B,H62C), C25(H25A,H25B,H25C), C65(H65A,H65B,
 H65C), C43(H43A,H43B,H43C), C56(H56A,H56B,H56C), C54(H54A,H54B,H54C), C46(H46A,
 H46B,H46C), C6(H6A,H6B,H6C), C16(H16A,H16B,H16C), C55(H55A,H55B,H55C),
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C3(H3A,H3B,H3C), C36(H36A,H36B,H36C),
  C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C74(H74A,H74B,H74C), C76(H76A,H76B,
 H76C), C73(H73A,H73B,H73C), C34(H34A,H34B,H34C), C36A(H36D,H36E,H36F),
 C34A(H34D,H34E,H34F), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              59766
_shelx_fab_checksum              93371
_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
;