First crystal structure of an Fe(III) anionic complex based on a pyruvic acid thiosemicarbazone ligand with Li<sup>+</sup>: synthesis, features of magnetic behavior and theoretical analysis.
Blagov, Maxim A.; Spitsyna, Nataliya G.; Ovanesyan, Nikolai S.; Lobach, Anatolii S.; Zorina, Leokadiya V.; Simonov, Sergey V.; Zakharov, Konstantin V.; Vasiliev, Alexander N.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1806–1819; doi:10.1039/d2dt03630d

data_7712176
_publ_section_title
;
 First crystal structure of an Fe(III) anionic complex based on a pyruvic
 acid thiosemicarbazone ligand with Li<sup>+</sup>: 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       '\w 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/[\s^2^(Fo^2^)+(0.0341P)^2^+0.4589P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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
;
_shelx_res_checksum              42340