Planarity of benzoyldithiocarbazate tuberculostatics. II. Diesters of benzoyldithiocarbazic acid
Szczesio, Małgorzata; Olczak, Andrzej; Gobis, Katarzyna; Mazerant, Ida; Kałużyńska, Sylwia; Foks, Henryk; Główka, Marek L.; Acta Crystallographica Section C 72 (2016) 75–79; doi:10.1107/S2053229615024201

data_2020326
_publ_section_title
;
 Planarity of benzoyldithiocarbazate tuberculostatics. II. Diesters of
 benzoyldithiocarbazic acid
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              75
_journal_page_last               79
_journal_paper_doi               10.1107/S2053229615024201
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C11 H13 N3 O3 S2'
_chemical_formula_moiety         'C11 H13 N3 O3 S2'
_chemical_formula_sum            'C11 H13 N3 O3 S2'
_chemical_formula_weight         299.36
_chemical_name_systematic
<i>N</i>'-[Bis(methylsulfanyl)methylidene]-<i>N</i>-methyl-4-nitrobenzohydrazide
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 91.219(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5716(2)
_cell_length_b                   16.3193(5)
_cell_length_c                   12.8982(4)
_cell_measurement_reflns_used    17780
_cell_measurement_temperature    295
_cell_measurement_theta_max      35.9090
_cell_measurement_theta_min      1.5752
_cell_volume                     1382.94(7)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2007)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2007)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0244
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28663
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.013
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.220
_refine_ls_extinction_coef       0.017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2013 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         4223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0648P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                3242
_reflns_number_total             4223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3609sup1.cif
_cod_data_source_block           G1
_cod_depositor_comments
;Adding full bibliography for 2020326--2020328.cif.

 Adding full bibliography for 2020326--2020328.cif.
;
_cod_database_code               2020326
_cod_database_fobs_code          2020326
_shelx_hkl_checksum              7497
_shelx_res_checksum              19448
_shelxl_version_number           20.13