Synthesis, structure and computational study of 5-[(prop-2-en-1-yl)sulfanyl]-1,3,4-thiadiazol-2-amine (<i>Pesta</i>) and its heterometallic π,σ-complex [Cu~2~FeCl~2~(<i>Pesta</i>)~4~][FeCl~4~]
Slyvka, Yurii; Kinzhybalo, Vasyl; Shyyka, Olga; Mys'kiv, Marian; Acta Crystallographica Section C 77 (2021) 249–256; doi:10.1107/S2053229621004198

data_2022369
_publ_section_title
;
 Synthesis, structure and computational study of
 5-[(prop-2-en-1-yl)sulfanyl]-1,3,4-thiadiazol-2-amine (<i>Pesta</i>) and
 its heterometallic \p,\s-complex [Cu~2~FeCl~2~(<i>Pesta</i>)~4~][FeCl~4~]
;
_journal_coeditor_code           VP3015
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              249
_journal_page_last               256
_journal_paper_doi               10.1107/S2053229621004198
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Cu2 Fe Cl2 (C5 H7 N3 S2)4] [Fe Cl4]'
_chemical_formula_moiety         'C20 H28 Cl2 Cu2 Fe N12 S8 2+, Cl4 Fe 2-'
_chemical_formula_sum            'C20 H28 Cl6 Cu2 Fe2 N12 S8'
_chemical_formula_weight         1144.50
_chemical_name_systematic
;Di-\m~2~-chlorido-1:2\k^2^<i>Cl</i>;2:3\k^2^<i>Cl</i>-tetrakis[\m~2~-5-(prop-2-en-1-ylsulfanyl)-1,3,4-thiadiazol-2-amine]-1:2\k^2^<i>N</i>^4^:<i>N</i>^3^;1(\h^2^),\k<i>N</i>^4^:2\k<i>N</i>^3^;2:3\k^2^<i>N</i>^3^:<i>N</i>^4^;2\k<i>N</i>^3^:3(\h^2^),\k<i>N</i>^4^-dicopper(I)iron(II)
tetrachloridoferrate(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.15(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.650(5)
_cell_length_b                   10.686(4)
_cell_length_c                   21.107(6)
_cell_measurement_reflns_used    10912
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      29.4970
_cell_measurement_theta_min      3.6060
_cell_volume                     3981(2)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.6249
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.549
_diffrn_reflns_theta_min         2.946
_exptl_absorpt_coefficient_mu    2.627
_exptl_absorpt_correction_T_max  0.517
_exptl_absorpt_correction_T_min  0.278
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2015), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.766
_exptl_crystal_size_mid          0.538
_exptl_crystal_size_min          0.377
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.464
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0240P)^2^+6.4630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0591
_reflns_number_gt                4464
_reflns_number_total             5036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vp3015sup1.cif
_cod_data_source_block           Cu2FePesta4Cl2FeCl4
_cod_depositor_comments
'Adding full bibliography for 2022368--2022369.cif.'
_cod_database_code               2022369
_cod_database_fobs_code          2022369
_shelx_hkl_checksum              31746
_shelx_res_checksum              4463