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_7249970
_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         'C75 H64 Dy N7 O5 P3, 3(C F3 O3 S)'
_chemical_formula_sum            'C78 H64 Dy F9 N7 O14 P3 S3'
_chemical_formula_weight         1845.95
_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                100.909(2)
_cell_angle_beta                 95.649(2)
_cell_angle_gamma                114.947(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9596(4)
_cell_length_b                   13.7413(3)
_cell_length_c                   25.0477(7)
_cell_measurement_reflns_used    14544
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      30.8300
_cell_measurement_theta_min      2.0810
_cell_volume                     3890.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_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  0.0585
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            46522
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         1.686
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.193
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       prism
_exptl_crystal_F_000             1866
_exptl_crystal_size_max          0.416
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.075
_refine_diff_density_max         2.243
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         19321
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0398P)^2^+2.3112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16064
_reflns_number_total             19321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00066a2.cif
_cod_data_source_block           Dypyr1
_cod_depositor_comments
'Adding full bibliography for 7249970--7249973.cif.'
_cod_database_code               7249970
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.637
_shelx_estimated_absorpt_t_max   0.916
_oxdiff_exptl_absorpt_empirical_full_min 0.499
_oxdiff_exptl_absorpt_empirical_full_max 1.344
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              97266