The magneto-structural correlations of ferric and ferrous neutral complexes with the pyruvic acid thiosemicarbazone ligand.
Blagov, Maxim A.; Lobach, Anatoly S.; Zorina, Leokadiya V.; Simonov, Sergey V.; Zakharov, Konstantin V.; Vasiliev, Alexander N.; Spitsyna, Nataliya G.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 14427–14439; doi:10.1039/d5dt01623a

data_7719284
_publ_section_title
;
 The magneto-structural correlations of ferric and ferrous neutral
 complexes with the pyruvic acid thiosemicarbazone ligand.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14427
_journal_page_last               14439
_journal_paper_doi               10.1039/d5dt01623a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C8 H12 Fe N6 O4 S2'
_chemical_formula_sum            'C8 H12 Fe N6 O4 S2'
_chemical_formula_weight         376.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-06-18 deposited with the CCDC.	2025-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.761(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5246(5)
_cell_length_b                   12.7050(8)
_cell_length_c                   12.0492(7)
_cell_measurement_reflns_used    2916
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      27.7420
_cell_measurement_theta_min      2.4950
_cell_volume                     1447.93(15)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection       'EXPO (STOE, 1999)'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6603
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         2.338
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.112a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       needle
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+3.9731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1393
_reflns_number_total             1661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01623a2.cif
_cod_data_source_block           2_120K
_cod_depositor_comments
'Adding full bibliography for 7719282--7719284.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7719284
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.664
_shelx_estimated_absorpt_t_max   0.973
_oxdiff_exptl_absorpt_empirical_full_min 0.845
_oxdiff_exptl_absorpt_empirical_full_max 1.222
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelx_res_checksum              83387