#------------------------------------------------------------------------------
#$Date: 2023-05-05 05:19:07 +0300 (Fri, 05 May 2023) $
#$Revision: 283304 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/21/7712176.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_7712176
loop_
_publ_author_name
'Blagov, Maxim A.'
'Spitsyna, Nataliya G.'
'Ovanesyan, Nikolai S.'
'Lobach, Anatolii S.'
'Zorina, Leokadiya V.'
'Simonov, Sergey V.'
'Zakharov, Konstantin V.'
'Vasiliev, Alexander N.'
_publ_section_title
;
 First crystal structure of an Fe(III) anionic complex based on a pyruvic
 acid thiosemicarbazone ligand with Li⁺: synthesis, features of
 magnetic behavior and theoretical analysis.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1806
_journal_page_last               1819
_journal_paper_doi               10.1039/d2dt03630d
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C8 H10 Fe N6 O4 S2, Li, 3(H2 O)'
_chemical_formula_sum            'C8 H16 Fe Li N6 O7 S2'
_chemical_formula_weight         435.18
_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   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2022-11-02 deposited with the CCDC.	2023-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                96.8310(18)
_cell_angle_beta                 110.156(2)
_cell_angle_gamma                99.2511(18)
_cell_formula_units_Z            2
_cell_length_a                   8.07939(18)
_cell_length_b                   10.2460(2)
_cell_length_c                   11.3580(3)
_cell_measurement_reflns_used    7408
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      30.9060
_cell_measurement_theta_min      2.0480
_cell_volume                     855.61(4)
_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_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2283
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.892
_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  0.0179
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13337
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         30.877
_diffrn_reflns_theta_min         1.945
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_description       wedge
_exptl_crystal_F_000             446
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.064
_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     258
_refine_ls_number_reflns         4827
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0277
_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)+(0.0341P)²+0.4589P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4280
_reflns_number_total             4827
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt03630d2.cif
_cod_data_source_block           SNG104
_cod_depositor_comments          'Adding full bibliography for 7712176.cif.'
_cod_database_code               7712176
_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   0.624
_shelx_estimated_absorpt_t_max   0.938
_oxdiff_exptl_absorpt_empirical_full_min 0.871
_oxdiff_exptl_absorpt_empirical_full_max 1.207
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.08172(3) 0.25474(2) 0.31256(2) 0.01181(6) Uani 1 1 d . . . . .
S1 S 0.30997(5) 0.14879(4) 0.36454(3) 0.01514(8) Uani 1 1 d . . . . .
S2 S 0.25495(5) 0.46125(4) 0.37158(3) 0.01627(8) Uani 1 1 d . . . . .
O1 O -0.13641(13) 0.32147(11) 0.22398(9) 0.0163(2) Uani 1 1 d . . . . .
O2 O -0.09007(14) 0.08622(10) 0.29281(9) 0.0159(2) Uani 1 1 d . . . . .
O3 O -0.31145(15) 0.33797(12) 0.02866(10) 0.0217(2) Uani 1 1 d . . . . .
O4 O -0.24961(16) -0.01151(12) 0.39701(11) 0.0241(2) Uani 1 1 d . . . . .
N1 N 0.08186(16) 0.22072(12) 0.14349(11) 0.0150(2) Uani 1 1 d . . . . .
N2 N 0.21025(17) 0.16612(14) 0.11321(12) 0.0183(3) Uani 1 1 d . . . . .
N3 N 0.06523(16) 0.28628(12) 0.47702(11) 0.0123(2) Uani 1 1 d . . . . .
N4 N 0.15432(16) 0.40092(12) 0.56769(11) 0.0145(2) Uani 1 1 d . . . . .
N5 N 0.4543(2) 0.07461(16) 0.19751(15) 0.0254(3) Uani 1 1 d . . . . .
H5A H 0.458(3) 0.064(2) 0.128(2) 0.031 Uiso 1 1 d . U . . .
H5B H 0.518(3) 0.041(2) 0.254(2) 0.031 Uiso 1 1 d . U . . .
N6 N 0.32122(18) 0.61101(14) 0.59771(13) 0.0189(3) Uani 1 1 d . . . . .
H6A H 0.301(3) 0.631(2) 0.6635(19) 0.023 Uiso 1 1 d . U . . .
H6B H 0.396(3) 0.663(2) 0.5829(19) 0.023 Uiso 1 1 d . U . . .
C1 C 0.32247(19) 0.13000(15) 0.21305(14) 0.0167(3) Uani 1 1 d . . . . .
C2 C -0.0474(2) 0.25083(16) 0.05382(14) 0.0181(3) Uani 1 1 d . . . . .
C3 C -0.17653(19) 0.30706(15) 0.10304(14) 0.0164(3) Uani 1 1 d . . . . .
C4 C 0.24161(18) 0.49081(14) 0.52278(13) 0.0144(3) Uani 1 1 d . . . . .
C5 C -0.04178(19) 0.19476(14) 0.50131(13) 0.0141(3) Uani 1 1 d . . . . .
C6 C -0.13389(19) 0.08001(15) 0.39164(13) 0.0153(3) Uani 1 1 d . . . . .
C7 C -0.0681(2) 0.2324(2) -0.08269(15) 0.0295(4) Uani 1 1 d . . . . .
H7A H 0.033615 0.291308 -0.091392 0.044 Uiso 1 1 calc R U . . .
H7B H -0.181317 0.255263 -0.133233 0.044 Uiso 1 1 calc R U . . .
H7C H -0.070225 0.138375 -0.113447 0.044 Uiso 1 1 calc R U . . .
C8 C -0.0797(2) 0.20194(16) 0.62034(15) 0.0211(3) Uani 1 1 d . . . . .
H8A H 0.018106 0.176845 0.686794 0.032 Uiso 1 1 calc R U . . .
H8B H -0.194105 0.139774 0.604241 0.032 Uiso 1 1 calc R U . . .
H8C H -0.088068 0.293940 0.648703 0.032 Uiso 1 1 calc R U . . .
Li1 Li -0.5309(4) 0.2818(3) -0.1207(3) 0.0226(6) Uani 1 1 d . . . . .
O5W O -0.49658(18) 0.24266(13) -0.28257(12) 0.0282(3) Uani 1 1 d D . . . .
H5WA H -0.476(3) 0.300(2) -0.318(2) 0.042 Uiso 1 1 d D U . . .
H5WB H -0.572(3) 0.1787(19) -0.324(2) 0.042 Uiso 1 1 d D U . . .
O6W O -0.6717(2) 0.41561(14) -0.15615(12) 0.0346(3) Uani 1 1 d D . . . .
H6WA H -0.663(4) 0.4862(18) -0.116(2) 0.052 Uiso 1 1 d D U . . .
H6WB H -0.724(3) 0.413(3) -0.2282(15) 0.052 Uiso 1 1 d D U . . .
O7W O -0.66728(16) 0.11818(12) -0.09097(11) 0.0215(2) Uani 1 1 d D . . . .
H7WA H -0.716(3) 0.136(2) -0.0464(18) 0.032 Uiso 1 1 d D U . . .
H7WB H -0.745(2) 0.0666(19) -0.1460(18) 0.032 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'
Li Li -0.0003 0.0001 '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
N3 Fe1 N1 176.37(5) . . ?
N3 Fe1 O2 82.09(5) . . ?
N1 Fe1 O2 95.62(5) . . ?
N3 Fe1 O1 95.20(5) . . ?
N1 Fe1 O1 81.77(5) . . ?
O2 Fe1 O1 84.87(4) . . ?
N3 Fe1 S2 85.20(4) . . ?
N1 Fe1 S2 96.87(4) . . ?
O2 Fe1 S2 166.58(3) . . ?
O1 Fe1 S2 92.05(3) . . ?
N3 Fe1 S1 97.47(4) . . ?
N1 Fe1 S1 85.33(4) . . ?
O2 Fe1 S1 90.40(3) . . ?
O1 Fe1 S1 165.74(3) . . ?
S2 Fe1 S1 95.505(15) . . ?
C1 S1 Fe1 94.69(5) . . ?
C4 S2 Fe1 95.15(5) . . ?
C3 O1 Fe1 113.07(9) . . ?
C6 O2 Fe1 112.50(9) . . ?
C3 O3 Li1 147.77(14) . . ?
C2 N1 N2 119.16(12) . . ?
C2 N1 Fe1 117.13(10) . . ?
N2 N1 Fe1 123.71(9) . . ?
C1 N2 N1 111.40(12) . . ?
C5 N3 N4 118.73(12) . . ?
C5 N3 Fe1 116.96(10) . . ?
N4 N3 Fe1 124.26(9) . . ?
C4 N4 N3 111.22(12) . . ?
C1 N5 H5A 117.6(15) . . ?
C1 N5 H5B 120.7(15) . . ?
H5A N5 H5B 121(2) . . ?
C4 N6 H6A 119.8(14) . . ?
C4 N6 H6B 121.0(14) . . ?
H6A N6 H6B 119.0(19) . . ?
N2 C1 N5 118.02(14) . . ?
N2 C1 S1 124.45(11) . . ?
N5 C1 S1 117.53(12) . . ?
N1 C2 C7 124.55(14) . . ?
N1 C2 C3 112.16(13) . . ?
C7 C2 C3 123.29(13) . . ?
O3 C3 O1 123.75(14) . . ?
O3 C3 C2 120.46(13) . . ?
O1 C3 C2 115.79(12) . . ?
N4 C4 N6 117.20(13) . . ?
N4 C4 S2 123.99(11) . . ?
N6 C4 S2 118.81(12) . . ?
N3 C5 C8 125.56(13) . . ?
N3 C5 C6 112.17(12) . . ?
C8 C5 C6 122.21(13) . . ?
O4 C6 O2 123.86(13) . . ?
O4 C6 C5 119.88(13) . . ?
O2 C6 C5 116.21(13) . . ?
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 . . ?
O6W Li1 O3 114.63(15) . . ?
O6W Li1 O5W 100.18(14) . . ?
O3 Li1 O5W 115.09(15) . . ?
O6W Li1 O7W 111.69(15) . . ?
O3 Li1 O7W 105.36(14) . . ?
O5W Li1 O7W 110.02(14) . . ?
O6W Li1 H5WB 101.5(6) . . ?
O3 Li1 H5WB 129.1(6) . . ?
O5W Li1 H5WB 19.1(5) . . ?
O7W Li1 H5WB 92.2(5) . . ?
O6W Li1 H7WA 99.1(5) . . ?
O3 Li1 H7WA 101.5(5) . . ?
O5W Li1 H7WA 125.7(5) . . ?
O7W Li1 H7WA 17.4(4) . . ?
H5WB Li1 H7WA 107.0(6) . . ?
Li1 O5W H5WA 121.0(18) . . ?
Li1 O5W H5WB 106.9(18) . . ?
H5WA O5W H5WB 117(2) . . ?
Li1 O6W H6WA 131.5(19) . . ?
Li1 O6W H6WB 114(2) . . ?
H6WA O6W H6WB 111(3) . . ?
Li1 O7W H7WA 111.3(17) . . ?
Li1 O7W H7WB 122.7(16) . . ?
H7WA O7W H7WB 101(2) . . ?
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 N3 1.9112(12) . ?
Fe1 N1 1.9109(12) . ?
Fe1 O2 1.9700(10) . ?
Fe1 O1 1.9785(10) . ?
Fe1 S2 2.2247(4) . ?
Fe1 S1 2.2302(4) . ?
S1 C1 1.7479(15) . ?
S2 C4 1.7512(15) . ?
O1 C3 1.2819(17) . ?
O2 C6 1.2934(17) . ?
O3 C3 1.2419(18) . ?
O3 Li1 1.928(3) . ?
O4 C6 1.2362(18) . ?
N1 C2 1.2918(19) . ?
N1 N2 1.3762(17) . ?
N2 C1 1.321(2) . ?
N3 C5 1.2916(18) . ?
N3 N4 1.3740(16) . ?
N4 C4 1.3254(19) . ?
N5 C1 1.337(2) . ?
N5 H5A 0.79(2) . ?
N5 H5B 0.82(2) . ?
N6 C4 1.3317(19) . ?
N6 H6A 0.83(2) . ?
N6 H6B 0.82(2) . ?
C2 C7 1.486(2) . ?
C2 C3 1.500(2) . ?
C5 C8 1.482(2) . ?
C5 C6 1.490(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Li1 O6W 1.911(3) . ?
Li1 O5W 1.957(3) . ?
Li1 O7W 1.984(3) . ?
Li1 H5WB 2.31(2) . ?
Li1 H7WA 2.37(2) . ?
O5W H5WA 0.774(15) . ?
O5W H5WB 0.792(15) . ?
O6W H6WA 0.786(15) . ?
O6W H6WB 0.775(15) . ?
O7W H7WA 0.763(14) . ?
O7W H7WB 0.781(14) . ?
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
N5 H5A O7W 0.79(2) 2.51(2) 3.189(2) 144(2) 1_655
N5 H5B O4 0.82(2) 2.21(2) 3.009(2) 164(2) 1_655
N6 H6A O1 0.83(2) 2.21(2) 2.9821(17) 155.7(18) 2_566
N6 H6B S1 0.82(2) 2.64(2) 3.4103(14) 157.0(18) 2_666
C7 H7B O5W 0.98 2.50 3.451(2) 163.7 .
C8 H8C S2 0.98 3.03 3.9381(17) 154.9 2_566
O5W H5WA S2 0.774(15) 3.042(17) 3.7713(14) 158(2) 2_565
O5W H5WB O4 0.792(15) 1.933(15) 2.7153(17) 169(2) 2_455
O6W H6WA O3 0.786(15) 2.027(16) 2.8048(17) 170(3) 2_465
O6W H6WB N4 0.775(15) 2.163(15) 2.9357(17) 174(3) 1_454
O7W H7WA N2 0.763(14) 2.100(15) 2.8399(16) 164(2) 1_455
O7W H7WB O2 0.781(14) 2.045(15) 2.8152(15) 169(2) 2_455
