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#$Date: 2025-10-06 11:47:14 +0200 (Mon 06 de Oct de 2025) $
#$Revision: 302684 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/92/7719284.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7719284
loop_
_publ_author_name
'Blagov, Maxim A.'
'Lobach, Anatoly S.'
'Zorina, Leokadiya V.'
'Simonov, Sergey V.'
'Zakharov, Konstantin V.'
'Vasiliev, Alexander N.'
'Spitsyna, Nataliya G.'
_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       'φ 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/[σ²(Fo²)+(0.0340P)²+3.9731P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.250000 0.84476(4) 0.000000 0.01622(14) Uani 1 2 d S T P . .
S1 S 0.33126(7) 0.98021(6) 0.14367(5) 0.02592(18) Uani 1 1 d . . . . .
O1 O 0.10520(18) 0.72513(15) -0.06781(14) 0.0215(4) Uani 1 1 d . . . . .
O2 O -0.0774(2) 0.62504(16) -0.03389(16) 0.0308(5) Uani 1 1 d . . . . .
N1 N 0.11498(19) 0.81275(15) 0.12553(15) 0.0120(4) Uani 1 1 d . . . . .
N2 N 0.1375(2) 0.85926(15) 0.22780(15) 0.0127(4) Uani 1 1 d . . . . .
H2 H 0.0930(17) 0.8426(6) 0.2758(18) 0.015 Uiso 1 1 calc R U . . .
N3 N 0.2570(2) 0.97276(17) 0.34862(17) 0.0229(5) Uani 1 1 d . . . . .
H3A H 0.2101(12) 0.9506(6) 0.3952(12) 0.027 Uiso 1 1 calc R U . . .
H3B H 0.3154(15) 1.0180(12) 0.3650(5) 0.027 Uiso 1 1 calc R U . . .
C1 C 0.2383(2) 0.93493(18) 0.24549(19) 0.0156(5) Uani 1 1 d . . . . .
C2 C 0.0135(2) 0.74564(18) 0.10552(18) 0.0139(5) Uani 1 1 d . . . . .
C3 C 0.0109(2) 0.69360(19) -0.0078(2) 0.0167(5) Uani 1 1 d . . . . .
C4 C -0.0920(3) 0.7173(2) 0.1826(2) 0.0216(5) Uani 1 1 d . . . . .
H4A H -0.052452 0.662670 0.234647 0.032 Uiso 1 1 calc R U . . .
H4B H -0.178173 0.690804 0.139157 0.032 Uiso 1 1 calc R U . . .
H4C H -0.114653 0.779747 0.224808 0.032 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 158.05(10) . 2 ?
N1 Fe1 O1 73.83(7) . . ?
N1 Fe1 O1 90.52(7) 2 . ?
N1 Fe1 O1 90.52(7) . 2 ?
N1 Fe1 O1 73.83(7) 2 2 ?
O1 Fe1 O1 89.93(10) . 2 ?
N1 Fe1 S1 117.29(5) . 2 ?
N1 Fe1 S1 78.69(5) 2 2 ?
O1 Fe1 S1 95.23(5) . 2 ?
O1 Fe1 S1 152.08(5) 2 2 ?
N1 Fe1 S1 78.68(5) . . ?
N1 Fe1 S1 117.29(5) 2 . ?
O1 Fe1 S1 152.08(5) . . ?
O1 Fe1 S1 95.23(5) 2 . ?
S1 Fe1 S1 92.93(4) 2 . ?
C1 S1 Fe1 97.01(8) . . ?
C3 O1 Fe1 117.88(14) . . ?
C2 N1 N2 119.41(18) . . ?
C2 N1 Fe1 119.58(15) . . ?
N2 N1 Fe1 120.96(14) . . ?
C1 N2 N1 118.89(19) . . ?
C1 N2 H2 120.6 . . ?
N1 N2 H2 120.6 . . ?
C1 N3 H3A 120.0 . . ?
C1 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
N3 C1 N2 114.8(2) . . ?
N3 C1 S1 122.09(18) . . ?
N2 C1 S1 123.12(17) . . ?
N1 C2 C4 126.0(2) . . ?
N1 C2 C3 112.91(19) . . ?
C4 C2 C3 121.05(19) . . ?
O2 C3 O1 125.6(2) . . ?
O2 C3 C2 118.7(2) . . ?
O1 C3 C2 115.7(2) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 2.1366(18) . ?
Fe1 N1 2.1366(18) 2 ?
Fe1 O1 2.1481(18) . ?
Fe1 O1 2.1481(18) 2 ?
Fe1 S1 2.4983(7) 2 ?
Fe1 S1 2.4984(7) . ?
S1 C1 1.696(2) . ?
O1 C3 1.282(3) . ?
O2 C3 1.225(3) . ?
N1 C2 1.290(3) . ?
N1 N2 1.361(2) . ?
N2 C1 1.357(3) . ?
N2 H2 0.79(3) . ?
N3 C1 1.325(3) . ?
N3 H3A 0.81(2) . ?
N3 H3B 0.81(2) . ?
C2 C4 1.491(3) . ?
C2 C3 1.515(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N2 H2 O1 0.79 2.06 2.736(2) 143.9 8_565 yes
N3 H3A O1 0.81 2.51 3.126(3) 134.3 8_565 yes
N3 H3B O2 0.81 2.02 2.777(3) 155.6 3 yes
C4 H4A S1 0.98 3.03 3.952(3) 158.1 7_565 yes
C4 H4B O2 0.98 2.65 3.630(3) 175.5 2_455 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N1 N2 C1 -175.6(2) . . . . ?
Fe1 N1 N2 C1 6.8(3) . . . . ?
N1 N2 C1 N3 -177.3(2) . . . . ?
N1 N2 C1 S1 3.9(3) . . . . ?
Fe1 S1 C1 N3 171.5(2) . . . . ?
Fe1 S1 C1 N2 -9.9(2) . . . . ?
N2 N1 C2 C4 4.4(3) . . . . ?
Fe1 N1 C2 C4 -177.99(18) . . . . ?
N2 N1 C2 C3 -174.64(18) . . . . ?
Fe1 N1 C2 C3 3.0(3) . . . . ?
Fe1 O1 C3 O2 -178.7(2) . . . . ?
Fe1 O1 C3 C2 0.0(3) . . . . ?
N1 C2 C3 O2 176.9(2) . . . . ?
C4 C2 C3 O2 -2.2(3) . . . . ?
N1 C2 C3 O1 -1.9(3) . . . . ?
C4 C2 C3 O1 179.0(2) . . . . ?
