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_7064089
_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         'C66 H64 Cl4 Dy Fe2 N4 O14, 0.5(H2 O), Cl O4'
_chemical_formula_sum            'C66 H65 Cl5 Dy Fe2 N4 O18.5'
_chemical_formula_weight         1661.67
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-10-23
_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                99.325(4)
_cell_angle_beta                 91.237(4)
_cell_angle_gamma                106.046(4)
_cell_formula_units_Z            4
_cell_length_a                   15.5272(16)
_cell_length_b                   18.8507(19)
_cell_length_c                   25.889(3)
_cell_measurement_reflns_used    989
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.90
_cell_volume                     7168.6(13)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            32276
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.207
_diffrn_reflns_theta_min         2.015
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6851
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.354
_refine_diff_density_min         -2.443
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1856
_refine_ls_number_reflns         32276
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+26.2136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27298
_reflns_number_total             32276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03857j2.cif
_cod_data_source_block           complex-3
_cod_depositor_comments
'Adding full bibliography for 7064086--7064089.cif.'
_cod_original_cell_volume        7168.5(13)
_cod_original_formula_sum        'C66 H65 Cl5 Dy Fe2 N4 O18.50'
_cod_database_code               7064089
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.729
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.91013
 0.08987
2. Restrained distances
 O1-O4 \\sim O5-O9
 with sigma of 0.004
 Cl16-O1 \\sim Cl16-O4 \\sim Cl16-O5 \\sim Cl16-O9
 with sigma of 0.002
 O1-O4 \\sim O7-O8
 with sigma of 0.004
 O1-O4 \\sim O5-O9 \\sim O7-O8
 with sigma of 0.004
 Cl16-O1 \\sim Cl16-O4 \\sim Cl16-O5 \\sim Cl16-O9 \\sim Cl16-O7 \\sim Cl16-O8
 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(Cl5) \\sim Ueq,
Uanis(Cl4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(Cl16) \\sim Ueq, Uanis(O7)
\\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(Cl6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C15, C24, C28, C35, C17, C22, Cl5, Cl4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O19, O16, O10, O2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O7, O9, Cl16, O4, O8, O5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: H42B(0.45) H42A(0.55) Cl2(0.8) O3(0.8) O5(0.7) O6(0.8) O9(0.7)
 O11(0.8) Cl3(0.2) O10(0.2) O16(0.2) O19(0.2) O7(0.3) Cl4(0.45) Cl5(0.55)
 C15(0.45) H15(0.45) C17(0.45) C35(0.45) H35(0.45) C22(0.55) C24(0.55)
 H24(0.55) C28(0.55) H28(0.55) O8(0.3)
6.a Free rotating group:
 O100(H10A,H10B)
6.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C5A(H5A), C9A(H9A), C11A(H11A), C12A(H12A), C14A(H14A), C15A(H15A),
 C18A(H18A), C20A(H20A), C24A(H24A), C26A(H26A), C27A(H27A), C29A(H29A),
 C30A(H30A), C33A(H33A), C35A(H35A), C39A(H39A), C41A(H41A), C42A(H42C),
 C44A(H44A), C45A(H45A), C48A(H48A), C50A(H50A), C54A(H54A), C56A(H56A),
 C57A(H57A), C59A(H59A), C60A(H60A), C3B(H3B), C5B(H5B), C9B(H9B), C11B(H11B),
 C12B(H12B), C14B(H14B), C15B(H15B), C18B(H18B), C20B(H20B), C24B(H24B),
 C26B(H26B), C27B(H27B), C29B(H29B), C30B(H30B), C33B(H33B), C35B(H35B),
 C39B(H39B), C41B(H41B), C42B(H42B), C42B(H42A), C48B(H48B), C50B(H50B),
 C54B(H54B), C56B(H56B), C57B(H57B), C59B(H59B), C60B(H60B), C15(H15), C35(H35),
  C24(H24), C28(H28)
6.c Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C22A(H22D,H22E,H22F), C23A(H23D,
 H23E,H23F), C37A(H37D,H37E,H37F), C38A(H38D,H38E,H38F), C52A(H52D,H52E,H52F),
 C53A(H53D,H53E,H53F), C62A(H62D,H62E,H62F), C64A(H64D,H64E,H64F), C65A(H65D,
 H65E,H65F), C66A(H66D,H66E,H66F), C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC),
 C22B(H22A,H22B,H22C), C23B(H23A,H23B,H23C), C37B(H37A,H37B,H37C), C38B(H38A,
 H38B,H38C), C52B(H52A,H52B,H52C), C53B(H53A,H53B,H53C), C62B(H62A,H62B,H62C),
 C64B(H64A,H64B,H64C), C65B(H65A,H65B,H65C), C66B(H66A,H66B,H66C)
;
_shelx_res_checksum              14540
_olex2_submission_special_instructions 'No special instructions were received'