Planarity of heteroaryldithiocarbazic acid derivatives showing tuberculostatic activity. II. Crystal structures of 3-[amino(pyrazin-2-yl)methylidene]-2-methylcarbazic acid esters
Olczak, Andrzej; Szczesio, Małgorzata; Gołka, Jolanta; Orlewska, Czesława; Gobis, Katarzyna; Foks, Henryk; Główka, Marek L.; Acta Crystallographica Section C 67 (2011) o37–o42; doi:10.1107/S0108270110049905

data_2017956
_publ_section_title
;
 Planarity of heteroaryldithiocarbazic acid derivatives showing
 tuberculostatic activity. II. Crystal structures of
 3-[amino(pyrazin-2-yl)methylidene]-2-methylcarbazic acid esters
;
_journal_coeditor_code           FG3209
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o37
_journal_page_last               o42
_journal_paper_doi               10.1107/S0108270110049905
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C14 H15 N5 S2'
_chemical_formula_moiety         'C14 H15 N5 S2'
_chemical_formula_sum            'C14 H15 N5 S2'
_chemical_formula_weight         317.43
_chemical_name_systematic
;
benzyl 3-[amino(pyrazin-2-yl)methylidene]-2-methylcarbazate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                105.7170(10)
_cell_angle_beta                 91.3680(10)
_cell_angle_gamma                93.8630(10)
_cell_formula_units_Z            2
_cell_length_a                   7.23290(10)
_cell_length_b                   7.90410(10)
_cell_length_c                   14.0969(2)
_cell_measurement_reflns_used    7068
_cell_measurement_temperature    290
_cell_measurement_theta_max      70.104
_cell_measurement_theta_min      5.8325
_cell_volume                     773.274(19)
_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>, 2006)
;
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      290
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8491
_diffrn_reflns_theta_full        66.53
_diffrn_reflns_theta_max         66.53
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    3.123
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2647
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0590P)^2^+0.1869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                2549
_reflns_number_total             2647
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3209.cif
_cod_data_source_block           C2
_cod_original_cell_volume        773.274(18)
_cod_database_code               2017956
_cod_database_fobs_code          2017956