Synthesis, crystal structure and Hirshfeld surface analysis of (2Z,2′E)-2,2′-(3-methoxy-3-phenylpropane-1,2-diylidene)bis(hydrazine-1-carbothioamide) dimethylformamide monosolvate
Guseinov, Firudin I.; Knyazev, Aleksandr V.; Shuvalova, Elena V.; Kobrakov, Konstantin I.; Samigullina, Aida I.; Atioğlu, Zeliha; Akkurt, Mehmet; Bhattarai, Ajaya; Acta Crystallographica Section E Crystallographic Communications 79 (2023) –; doi:10.1107/S2056989023007946

data_2022862
_publ_section_title
;
 Synthesis, crystal structure and Hirshfeld surface analysis of
 (2Z,2&#x2032;E)-2,2&#x2032;-(3-methoxy-3-phenylpropane-1,2-diylidene)bis(hydrazine-1-carbothioamide)
 dimethylformamide monosolvate
;
_journal_coeditor_code           YZ2041
_journal_issue                   10
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_paper_doi               10.1107/S2056989023007946
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          'C12 H16 N6 O S2, C3 H7 N O'
_chemical_formula_moiety         'C12 H16 N6 O S2, C3 H7 N O'
_chemical_formula_sum            'C15 H23 N7 O2 S2'
_chemical_formula_weight         397.52
_chemical_name_systematic
'(2<i>Z</i>,2'<i>E</i>)-2,2'-(3-Methoxy-3-phenylpropane-1,2-diylidene)bis(2-methylhydrazine-1-carbothioamide) dimethylformamide monosolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 111.749(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.45730(10)
_cell_length_b                   23.5853(3)
_cell_length_c                   11.00720(10)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.5700
_cell_measurement_theta_min      3.7250
_cell_volume                     2039.29(5)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2019/1</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2019/1</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11141
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.792
_diffrn_reflns_theta_min         3.748
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       plate
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.274
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower
;
_refine_ls_abs_structure_Flack   0.000(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         2776
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0317
_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/[\s^2^(Fo^2^)+(0.0653P)^2^+0.7217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0877
_reflns_number_gt                2751
_reflns_number_total             2776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yz2041sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2022862
_shelx_estimated_absorpt_t_min   0.493
_shelx_estimated_absorpt_t_max   0.950
_shelx_hkl_checksum              16313
_shelx_res_checksum              9141
_cod_database_fobs_code 2022862