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_7249973
_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 H63 Dy N7 O5 P3, 2(Cl O4), C2 H6 O, 1.9(H2 O)'
_chemical_formula_sum            'C77 H72.8 Cl2 Dy N7 O15.9 P3'
_chemical_formula_weight         1676.93
_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                99.0853(8)
_cell_angle_beta                 94.0652(8)
_cell_angle_gamma                91.2834(8)
_cell_formula_units_Z            4
_cell_length_a                   13.80326(14)
_cell_length_b                   17.08518(16)
_cell_length_c                   31.8500(3)
_cell_measurement_reflns_used    44032
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      31.1890
_cell_measurement_theta_min      2.1170
_cell_volume                     7394.03(13)
_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 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0251
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            82579
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.100
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.626
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       prism
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.016
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1999
_refine_ls_number_reflns         32555
_refine_ls_number_restraints     127
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0364P)^2^+24.7527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27209
_reflns_number_total             32555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00066a2.cif
_cod_data_source_block           Dypyr2
_cod_depositor_comments
'Adding full bibliography for 7249970--7249973.cif.'
_cod_original_cell_volume        7394.02(12)
_cod_original_formula_sum        'C77 H72.80 Cl2 Dy N7 O15.90 P3'
_cod_database_code               7249973
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.616
_shelx_estimated_absorpt_t_max   0.909
_oxdiff_exptl_absorpt_empirical_full_min 0.823
_oxdiff_exptl_absorpt_empirical_full_max 1.243
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              70729