Planarity of heteroaryldithiocarbazic acid derivatives showing tuberculostatic activity. III. Mono- and diesters of 3-(pyrazin-2-ylcarbonyl)dithiocarbazic acid
Szczesio, Małgorzata; Olczak, Andrzej; Gołka, Jolanta; Gobis, Katarzyna; Foks, Henryk; Główka, Marek L.; Acta Crystallographica Section C 67 (2011) o235–o240; doi:10.1107/S0108270111021767

data_2018131
_publ_section_title
;
 Planarity of heteroaryldithiocarbazic acid derivatives showing
 tuberculostatic activity. III. Mono- and diesters of
 3-(pyrazin-2-ylcarbonyl)dithiocarbazic acid
;
_journal_coeditor_code           GD3386
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o235
_journal_page_last               o240
_journal_paper_doi               10.1107/S0108270111021767
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C8 H10 N4 O S2'
_chemical_formula_moiety         'C8 H10 N4 O S2'
_chemical_formula_sum            'C8 H10 N4 O S2'
_chemical_formula_weight         242.32
_chemical_name_systematic
;
methyl 1-methyl-2-(pyrazin-2-ylcarbonyl)hydrazinecarbodithioate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.151(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.0900(4)
_cell_length_b                   6.4482(6)
_cell_length_c                   20.7828(19)
_cell_measurement_reflns_used    8014
_cell_measurement_temperature    290
_cell_measurement_theta_max      30.41
_cell_measurement_theta_min      2.94
_cell_volume                     548.00(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2002)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2003)'
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            12608
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.465
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             252
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.210
_refine_ls_abs_structure_details
'Flack (1983), <b>with how many Friedel pairs?</b>'
_refine_ls_abs_structure_Flack   0.18(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2642
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0713P)^2^+0.2203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1232
_reflns_number_gt                2523
_reflns_number_total             2642
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3386.cif
_cod_data_source_block           G1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2018131
_cod_database_fobs_code          2018131