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#$Revision: 298251 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/74/7717461.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_7717461
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                 102.9640(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2865(2)
_cell_length_b                   10.4627(2)
_cell_length_c                   12.9417(2)
_cell_measurement_reflns_used    14669
_cell_measurement_temperature    350(1)
_cell_measurement_theta_max      32.6670
_cell_measurement_theta_min      2.5130
_cell_volume                     1489.30(5)
_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      350(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4566
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.940
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34128
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        32.000
_diffrn_reflns_theta_max         32.980
_diffrn_reflns_theta_min         2.167
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.325
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87242
_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            black
_exptl_crystal_density_diffrn    1.754
_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         0.486
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.072
_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     220
_refine_ls_number_reflns         5271
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0395P)²+0.7363P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4229
_reflns_number_total             5271
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02901a2.cif
_cod_data_source_block           350K
_cod_depositor_comments
'Adding full bibliography for 7717460--7717461.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7717461
_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   0.540
_shelx_estimated_absorpt_t_max   0.733
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 0.07210(2) 0.47865(2) 0.24548(2) 0.02398(6) Uani 1 1 d . . . . .
S1 S 0.18649(4) 0.40289(4) 0.39614(3) 0.03311(10) Uani 1 1 d . . . . .
S2 S 0.22482(5) 0.59011(4) 0.20323(4) 0.03900(11) Uani 1 1 d . . . . .
O1 O -0.04467(12) 0.56378(12) 0.13478(9) 0.0373(3) Uani 1 1 d . . . . .
O2 O -0.05859(11) 0.35885(12) 0.25583(9) 0.0346(3) Uani 1 1 d . . . . .
O3 O -0.17731(12) 0.72269(13) 0.11132(10) 0.0408(3) Uani 1 1 d . . . . .
O4 O -0.12798(13) 0.16625(14) 0.19855(11) 0.0480(3) Uani 1 1 d . . . . .
C1 C 0.14942(14) 0.52525(15) 0.47581(12) 0.0269(3) Uani 1 1 d . . . . .
C2 C -0.05372(15) 0.69058(16) 0.28403(12) 0.0298(3) Uani 1 1 d . . . . .
C3 C -0.09661(15) 0.65910(16) 0.16899(12) 0.0302(3) Uani 1 1 d . . . . .
C4 C 0.25164(15) 0.48492(16) 0.10926(12) 0.0299(3) Uani 1 1 d . . . . .
C5 C 0.02920(14) 0.25710(15) 0.12720(12) 0.0286(3) Uani 1 1 d . . . . .
C6 C -0.06046(15) 0.25903(17) 0.19794(13) 0.0319(3) Uani 1 1 d . . . . .
C7 C -0.1023(2) 0.8020(2) 0.33230(16) 0.0475(5) Uani 1 1 d . . . . .
H7A H -0.121779 0.776526 0.397817 0.071 Uiso 1 1 calc R U . . .
H7B H -0.174346 0.832888 0.284570 0.071 Uiso 1 1 calc R U . . .
H7C H -0.042294 0.868545 0.345723 0.071 Uiso 1 1 calc R U . . .
C8 C 0.0288(2) 0.15145(19) 0.05102(17) 0.0456(5) Uani 1 1 d . . . . .
H8A H -0.027050 0.171098 -0.014675 0.068 Uiso 1 1 calc R U . . .
H8B H 0.004087 0.073757 0.079622 0.068 Uiso 1 1 calc R U . . .
H8C H 0.108972 0.140978 0.038708 0.068 Uiso 1 1 calc R U . . .
N1 N 0.02726(12) 0.61040(12) 0.33275(10) 0.0255(2) Uani 1 1 d . . . . .
N2 N 0.07576(13) 0.62244(13) 0.43945(10) 0.0293(3) Uani 1 1 d . . . . .
N3 N 0.10133(11) 0.35353(12) 0.14506(10) 0.0248(2) Uani 1 1 d . . . . .
N4 N 0.19062(12) 0.37340(13) 0.09042(10) 0.0288(3) Uani 1 1 d D . . . .
H4 H 0.2053(3) 0.3230(10) 0.0507(8) 0.035 Uiso 1 1 calc DR U . . .
N5 N 0.19856(16) 0.52008(15) 0.57908(12) 0.0371(3) Uani 1 1 d D . . . .
H5A H 0.179(2) 0.5738(18) 0.6171(16) 0.045 Uiso 1 1 d D U . . .
H5B H 0.2471(18) 0.4640(19) 0.6023(17) 0.045 Uiso 1 1 d D U . . .
N6 N 0.33270(16) 0.51031(18) 0.05376(14) 0.0436(4) Uani 1 1 d D . . . .
H6A H 0.353(2) 0.456(2) 0.0153(18) 0.052 Uiso 1 1 d D U . . .
H6B H 0.372(2) 0.5768(18) 0.0634(19) 0.052 Uiso 1 1 d D U . . .
O5W O 0.05686(14) 0.84838(14) 0.57196(11) 0.0417(3) Uani 1 1 d D . . . .
H5W1 H 0.059(2) 0.779(2) 0.546(2) 0.063 Uiso 1 1 d D U . . .
H5W2 H 0.099(2) 0.842(3) 0.6297(17) 0.063 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 173.24(5) . . ?
N1 Fe1 O1 83.07(5) . . ?
N3 Fe1 O1 90.26(5) . . ?
N1 Fe1 O2 96.72(5) . . ?
N3 Fe1 O2 81.78(5) . . ?
O1 Fe1 O2 86.96(6) . . ?
N1 Fe1 S1 85.31(4) . . ?
N3 Fe1 S1 101.27(4) . . ?
O1 Fe1 S1 167.74(4) . . ?
O2 Fe1 S1 90.57(4) . . ?
N1 Fe1 S2 95.07(4) . . ?
N3 Fe1 S2 86.08(4) . . ?
O1 Fe1 S2 90.75(4) . . ?
O2 Fe1 S2 167.63(4) . . ?
S1 Fe1 S2 94.129(19) . . ?
C1 S1 Fe1 94.99(5) . . ?
C4 S2 Fe1 96.11(6) . . ?
C3 O1 Fe1 112.97(10) . . ?
C6 O2 Fe1 113.22(10) . . ?
N2 C1 N5 118.27(14) . . ?
N2 C1 S1 124.25(12) . . ?
N5 C1 S1 117.48(12) . . ?
N1 C2 C7 126.20(14) . . ?
N1 C2 C3 112.18(13) . . ?
C7 C2 C3 121.62(14) . . ?
O3 C3 O1 122.81(15) . . ?
O3 C3 C2 120.89(15) . . ?
O1 C3 C2 116.31(14) . . ?
N6 C4 N4 117.84(15) . . ?
N6 C4 S2 120.93(14) . . ?
N4 C4 S2 121.24(12) . . ?
N3 C5 C8 127.85(15) . . ?
N3 C5 C6 111.37(13) . . ?
C8 C5 C6 120.76(14) . . ?
O4 C6 O2 124.44(16) . . ?
O4 C6 C5 119.46(15) . . ?
O2 C6 C5 116.09(14) . . ?
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 120.60(13) . . ?
C2 N1 Fe1 115.39(10) . . ?
N2 N1 Fe1 124.01(10) . . ?
C1 N2 N1 111.24(12) . . ?
C5 N3 N4 122.41(13) . . ?
C5 N3 Fe1 117.26(10) . . ?
N4 N3 Fe1 120.17(10) . . ?
C4 N4 N3 116.27(13) . . ?
C4 N4 H4 121.9 . . ?
N3 N4 H4 121.9 . . ?
C1 N5 H5A 118.3(17) . . ?
C1 N5 H5B 119.7(16) . . ?
H5A N5 H5B 122(2) . . ?
C4 N6 H6A 121.1(18) . . ?
C4 N6 H6B 120.7(17) . . ?
H6A N6 H6B 118(2) . . ?
H5W1 O5W H5W2 105(3) . . ?
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 1.9205(12) . ?
Fe1 N3 1.9246(12) . ?
Fe1 O1 1.9328(12) . ?
Fe1 O2 1.9629(12) . ?
Fe1 S1 2.2288(5) . ?
Fe1 S2 2.2480(5) . ?
S1 C1 1.7524(16) . ?
S2 C4 1.7166(17) . ?
O1 C3 1.285(2) . ?
O2 C6 1.283(2) . ?
O3 C3 1.235(2) . ?
O4 C6 1.235(2) . ?
C1 N2 1.331(2) . ?
C1 N5 1.328(2) . ?
C2 N1 1.295(2) . ?
C2 C7 1.484(2) . ?
C2 C3 1.495(2) . ?
C4 N6 1.311(2) . ?
C4 N4 1.349(2) . ?
C5 N3 1.284(2) . ?
C5 C8 1.480(2) . ?
C5 C6 1.509(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N1 N2 1.3722(17) . ?
N3 N4 1.3706(18) . ?
N4 H4 0.780(15) . ?
N5 H5A 0.810(15) . ?
N5 H5B 0.813(15) . ?
N6 H6A 0.820(15) . ?
N6 H6B 0.821(15) . ?
O5W H5W1 0.804(19) . ?
O5W H5W2 0.79(2) . ?
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 0.96 2.66 3.246(3) 119.9 3_565
N4 H4 O3 0.78 2.10 2.7702(18) 143.6 3_565
N5 H5A O2 0.810(15) 2.460(17) 3.191(2) 151(2) 3_566
N5 H5B O4 0.813(15) 2.147(16) 2.944(2) 167(2) 4_666
N6 H6A O5W 0.820(15) 2.024(17) 2.825(2) 165(2) 2_545
N6 H6B O5W 0.821(15) 2.21(2) 2.894(2) 142(2) 4_675
O5W H5W1 N2 0.804(19) 2.18(2) 2.9562(19) 164(3) .
O5W H5W2 O4 0.79(2) 2.17(2) 2.902(2) 153(3) 3_566
