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#$Date: 2025-03-04 22:09:45 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298251 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/74/7717460.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.
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data_7717460
loop_
_publ_author_name
'Blagov, Maxim A.'
'Akimov, Alexander V.'
'Lobach, Anatoly S.'
'Zorina, Leokadiya V.'
'Simonov, Sergey V.'
'Zakharov, Konstantin V.'
'Vasiliev, Alexander N.'
'Spitsyna, Nataliya G.'
_publ_section_title
;
 The hydrate of a neutral iron(III) complex based on the pyruvic acid
 thiosemicarbazone ligand with abrupt spin-crossover with
 T<sub>1/2</sub> = 340 K and a wide hysteresis loop of 45 K.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              346
_journal_page_last               356
_journal_paper_doi               10.1039/d4dt02901a
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         'C8 H11 Fe N6 O4 S2, H2 O'
_chemical_formula_sum            'C8 H13 Fe N6 O5 S2'
_chemical_formula_weight         393.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2024-10-07 deposited with the CCDC.	2024-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.816(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1829(3)
_cell_length_b                   10.4546(3)
_cell_length_c                   12.7936(3)
_cell_measurement_reflns_used    7665
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      32.8330
_cell_measurement_theta_min      2.1680
_cell_volume                     1458.47(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω 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  0.0233
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33763
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        32.000
_diffrn_reflns_theta_max         33.080
_diffrn_reflns_theta_min         2.191
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.102a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       prism
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         5244
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0256
_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/[σ²(Fo²)+(0.0288P)²+1.0818P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4680
_reflns_number_total             5244
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02901a2.cif
_cod_data_source_block           150K
_cod_depositor_comments
'Adding full bibliography for 7717460--7717461.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7717460
_shelx_shelxl_version_number     2016/6
_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   0.534
_shelx_estimated_absorpt_t_max   0.728
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.07316(2) 0.48030(2) 0.24589(2) 0.01017(4) Uani 1 1 d . . . . .
S1 S 0.18833(3) 0.40292(3) 0.39723(2) 0.01400(6) Uani 1 1 d . . . . .
S2 S 0.22657(3) 0.59181(3) 0.20401(2) 0.01656(6) Uani 1 1 d . . . . .
O1 O -0.04378(8) 0.56553(9) 0.13368(7) 0.01658(16) Uani 1 1 d . . . . .
O2 O -0.05973(8) 0.36209(8) 0.25661(7) 0.01465(15) Uani 1 1 d . . . . .
O3 O -0.17905(8) 0.72449(9) 0.11055(7) 0.01743(17) Uani 1 1 d . . . . .
O4 O -0.12921(9) 0.16799(9) 0.20084(7) 0.01940(18) Uani 1 1 d . . . . .
C1 C 0.14989(10) 0.52416(10) 0.47851(9) 0.01199(18) Uani 1 1 d . . . . .
C2 C -0.05507(10) 0.69081(11) 0.28543(9) 0.01310(19) Uani 1 1 d . . . . .
C3 C -0.09700(10) 0.66042(11) 0.16872(9) 0.01338(19) Uani 1 1 d . . . . .
C4 C 0.25494(10) 0.48563(11) 0.10963(9) 0.01325(19) Uani 1 1 d . . . . .
C5 C 0.02969(10) 0.25780(11) 0.12792(9) 0.01287(19) Uani 1 1 d . . . . .
C6 C -0.06117(10) 0.26071(11) 0.19890(9) 0.01371(19) Uani 1 1 d . . . . .
C7 C -0.10541(12) 0.80021(12) 0.33620(10) 0.0194(2) Uani 1 1 d . . . . .
H7A H -0.125073 0.772044 0.403497 0.029 Uiso 1 1 calc R U . . .
H7B H -0.179959 0.831774 0.287611 0.029 Uiso 1 1 calc R U . . .
H7C H -0.044388 0.868932 0.350954 0.029 Uiso 1 1 calc R U . . .
C8 C 0.02984(12) 0.15109(12) 0.05170(10) 0.0194(2) Uani 1 1 d . . . . .
H8A H -0.029276 0.169171 -0.015532 0.029 Uiso 1 1 calc R U . . .
H8B H 0.006902 0.071551 0.082766 0.029 Uiso 1 1 calc R U . . .
H8C H 0.111990 0.141976 0.037472 0.029 Uiso 1 1 calc R U . . .
N1 N 0.02738(9) 0.61036(9) 0.33427(7) 0.01119(16) Uani 1 1 d . . . . .
N2 N 0.07513(9) 0.62150(9) 0.44210(7) 0.01292(17) Uani 1 1 d . . . . .
N3 N 0.10263(9) 0.35469(9) 0.14557(7) 0.01113(16) Uani 1 1 d . . . . .
N4 N 0.19352(9) 0.37326(9) 0.09093(8) 0.01288(17) Uani 1 1 d D . . . .
H4 H 0.2094(3) 0.3208(8) 0.0503(7) 0.015 Uiso 1 1 calc DR U . . .
N5 N 0.19869(10) 0.51779(10) 0.58320(8) 0.01561(18) Uani 1 1 d D . . . .
H5A H 0.1803(16) 0.5732(15) 0.6235(13) 0.019 Uiso 1 1 d D U . . .
H5B H 0.2493(14) 0.4607(15) 0.6087(13) 0.019 Uiso 1 1 d D U . . .
N6 N 0.33729(10) 0.51040(11) 0.05381(9) 0.01802(19) Uani 1 1 d D . . . .
H6A H 0.3563(17) 0.4577(15) 0.0113(13) 0.022 Uiso 1 1 d D U . . .
H6B H 0.3816(15) 0.5753(14) 0.0678(14) 0.022 Uiso 1 1 d D U . . .
O5W O 0.05691(9) 0.84554(9) 0.57132(7) 0.01669(16) Uani 1 1 d D . . . .
H5W1 H 0.0601(18) 0.7808(16) 0.5438(14) 0.025 Uiso 1 1 d D U . . .
H5W2 H 0.0926(17) 0.8347(18) 0.6285(13) 0.025 Uiso 1 1 d D 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'
Fe Fe 0.3463 0.8444 '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'
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 N3 173.55(4) . . ?
N1 Fe1 O1 83.42(4) . . ?
N3 Fe1 O1 90.40(4) . . ?
N1 Fe1 O2 95.77(4) . . ?
N3 Fe1 O2 81.98(4) . . ?
O1 Fe1 O2 86.80(4) . . ?
N1 Fe1 S1 85.59(3) . . ?
N3 Fe1 S1 100.45(3) . . ?
O1 Fe1 S1 168.40(3) . . ?
O2 Fe1 S1 90.65(3) . . ?
N1 Fe1 S2 95.24(3) . . ?
N3 Fe1 S2 86.66(3) . . ?
O1 Fe1 S2 90.59(3) . . ?
O2 Fe1 S2 168.32(3) . . ?
S1 Fe1 S2 94.083(13) . . ?
C1 S1 Fe1 94.74(4) . . ?
C4 S2 Fe1 95.89(4) . . ?
C3 O1 Fe1 112.69(7) . . ?
C6 O2 Fe1 113.03(7) . . ?
N5 C1 N2 118.35(10) . . ?
N5 C1 S1 117.46(9) . . ?
N2 C1 S1 124.19(8) . . ?
N1 C2 C7 125.76(10) . . ?
N1 C2 C3 111.95(10) . . ?
C7 C2 C3 122.29(10) . . ?
O3 C3 O1 122.97(10) . . ?
O3 C3 C2 120.65(10) . . ?
O1 C3 C2 116.38(10) . . ?
N6 C4 N4 117.72(10) . . ?
N6 C4 S2 121.08(9) . . ?
N4 C4 S2 121.19(9) . . ?
N3 C5 C8 127.88(11) . . ?
N3 C5 C6 111.35(10) . . ?
C8 C5 C6 120.76(10) . . ?
O4 C6 O2 124.24(11) . . ?
O4 C6 C5 119.80(10) . . ?
O2 C6 C5 115.94(10) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 N1 N2 120.36(9) . . ?
C2 N1 Fe1 115.50(7) . . ?
N2 N1 Fe1 124.15(7) . . ?
C1 N2 N1 111.17(9) . . ?
C5 N3 N4 122.33(9) . . ?
C5 N3 Fe1 117.39(8) . . ?
N4 N3 Fe1 120.17(7) . . ?
C4 N4 N3 115.94(9) . . ?
C4 N4 H4 122.0 . . ?
N3 N4 H4 122.0 . . ?
C1 N5 H5A 119.1(12) . . ?
C1 N5 H5B 121.2(12) . . ?
H5A N5 H5B 119.6(17) . . ?
C4 N6 H6A 122.5(13) . . ?
C4 N6 H6B 119.9(12) . . ?
H6A N6 H6B 116.8(17) . . ?
H5W1 O5W H5W2 104.1(19) . . ?
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 1.9096(9) . ?
Fe1 N3 1.9152(9) . ?
Fe1 O1 1.9318(8) . ?
Fe1 O2 1.9608(9) . ?
Fe1 S1 2.2262(3) . ?
Fe1 S2 2.2354(3) . ?
S1 C1 1.7523(11) . ?
S2 C4 1.7207(12) . ?
O1 C3 1.2874(14) . ?
O2 C6 1.2897(14) . ?
O3 C3 1.2416(14) . ?
O4 C6 1.2359(14) . ?
C1 N5 1.3312(14) . ?
C1 N2 1.3338(14) . ?
C2 N1 1.3010(14) . ?
C2 C7 1.4862(16) . ?
C2 C3 1.4965(15) . ?
C4 N6 1.3102(15) . ?
C4 N4 1.3551(15) . ?
C5 N3 1.2887(14) . ?
C5 C8 1.4819(16) . ?
C5 C6 1.5058(16) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N1 N2 1.3693(12) . ?
N3 N4 1.3691(13) . ?
N4 H4 0.802(13) . ?
N5 H5A 0.831(13) . ?
N5 H5B 0.837(13) . ?
N6 H6A 0.834(13) . ?
N6 H6B 0.835(13) . ?
O5W H5W1 0.767(15) . ?
O5W H5W2 0.760(15) . ?
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
C8 H8C O3 0.98 2.59 3.2128(16) 121.2 3_565
N4 H4 O3 0.80 2.07 2.7441(13) 142.3 3_565
N5 H5A O2 0.831(13) 2.355(14) 3.0991(14) 149.4(16) 3_566
N5 H5B O4 0.837(13) 2.082(13) 2.9080(13) 168.8(16) 4_666
N6 H6A O5W 0.834(13) 1.972(14) 2.7882(14) 165.7(18) 2_545
N6 H6B O5W 0.835(13) 2.120(15) 2.8472(14) 145.4(17) 4_675
O5W H5W1 N2 0.767(15) 2.143(15) 2.9000(13) 169.2(19) .
O5W H5W2 O4 0.760(15) 2.131(16) 2.8504(13) 158.3(19) 3_566
