Planarity of heteroaryldithiocarbazic acid derivatives showing tuberculostatic activity: structure–activity relationships
Szczesio, Małgorzata; Gołka, Jolanta; Korona-Głowniak, Izabela; Orlewska, Czesława; Gobis, Katarzyna; Olczak, Andrzej; Acta Crystallographica Section C 74 (2018) –; doi:10.1107/S205322961800284X

data_2021048
_publ_section_title
;
 Planarity of heteroaryldithiocarbazic acid derivatives showing
 tuberculostatic activity: structure--activity relationships
;
_journal_coeditor_code           FN3253
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S205322961800284X
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C9 H12 N4 S2'
_chemical_formula_moiety         'C9 H12 N4 S2'
_chemical_formula_sum            'C9 H12 N4 S2'
_chemical_formula_weight         240.35
_chemical_name_systematic
;
(<i>Z</i>)-Methyl
2-[amino(pyridin-2-yl)methylidene]-1-methylhydrazinecarbodithioate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                79.167(2)
_cell_angle_beta                 71.019(2)
_cell_angle_gamma                84.080(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3230(2)
_cell_length_b                   8.5983(2)
_cell_length_c                   10.0343(2)
_cell_measurement_reflns_used    21672
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      78.7410
_cell_measurement_theta_min      4.7090
_cell_volume                     586.21(3)
_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
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24172
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.020
_diffrn_reflns_theta_min         4.724
_exptl_absorpt_coefficient_mu    3.906
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.176
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       needle
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.300
_refine_ls_extinction_coef       0.0147(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0656P)^2^+0.3090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                2393
_reflns_number_total             2417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3253sup1.cif
_cod_data_source_block           S3
_cod_database_code               2021048
_cod_database_fobs_code          2021048
_shelx_hkl_checksum              33366
_shelx_res_checksum              71553
_shelxl_version_number           2.014