Mononuclear complexes of dysprosium(iii) with 2,6-diacetylpyridine bis(isonicotinoylhydrazone): synthesis, crystal structure, and magnetic properties
Kopotkov, Vyacheslav A.; Zorina, Leokadiya V.; Simonov, Sergey V.; Korchagin, Denis V.; Zhidkov, Mikhail V.; Dmitriev, Alexei I.; Mahmoudi, Ghodrat; Yagubskii, Eduard B.; CrystEngComm 27 (2025) 2012–2024; doi:10.1039/D5CE00066A

data_7249971
_publ_section_title
;
 Mononuclear complexes of dysprosium(iii) with 2,6-diacetylpyridine
 bis(isonicotinoylhydrazone): synthesis, crystal structure, and magnetic
 properties
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              2012
_journal_page_last               2024
_journal_paper_doi               10.1039/D5CE00066A
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C57 H84 Dy N7 O4 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C59 H84 Dy F6 N7 O10 P2 S2'
_chemical_formula_weight         1453.89
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-12-24 deposited with the CCDC.	2025-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                108.328(2)
_cell_angle_beta                 98.490(2)
_cell_angle_gamma                98.959(2)
_cell_formula_units_Z            4
_cell_length_a                   12.8264(3)
_cell_length_b                   23.1597(7)
_cell_length_c                   25.9044(6)
_cell_measurement_reflns_used    25201
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.0730
_cell_measurement_theta_min      2.0520
_cell_volume                     7055.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'EXPO (STOE, 1999)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'Image Plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       diffractometer
_diffrn_measurement_device_type  STOE
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26316
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.918
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       prism
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.200
_refine_diff_density_max         3.363
_refine_diff_density_min         -1.920
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1863
_refine_ls_number_reflns         26316
_refine_ls_number_restraints     1350
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0242P)^2^+77.9940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19820
_reflns_number_total             26316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00066a2.cif
_cod_data_source_block           Dypyr3
_cod_depositor_comments
'Adding full bibliography for 7249970--7249973.cif.'
_cod_database_code               7249971
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.577
_shelx_estimated_absorpt_t_max   0.790
_oxdiff_exptl_absorpt_empirical_full_min 0.874
_oxdiff_exptl_absorpt_empirical_full_max 1.114
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              40331