Planarity of heteroaryldithiocarbazic acid derivatives showing tuberculostatic activity. IV. Diesters of benzoylcarbonohydrazonodithioic acid
Szczesio, Małgorzata; Olczak, Andrzej; Gobis, Katarzyna; Foks, Henryk; Główka, Marek L.; Acta Crystallographica Section C 68 (2012) o99–o103; doi:10.1107/S0108270112001734

data_2018439
_publ_section_title
;
 Planarity of heteroaryldithiocarbazic acid derivatives showing
 tuberculostatic activity. IV. Diesters of benzoylcarbonohydrazonodithioic
 acid
;
_journal_coeditor_code           WQ3009
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o99
_journal_page_last               o103
_journal_paper_doi               10.1107/S0108270112001734
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C10 H10 Cl2 N2 O S2'
_chemical_formula_moiety         'C10 H10 Cl2 N2 O S2'
_chemical_formula_sum            'C10 H10 Cl2 N2 O S2'
_chemical_formula_weight         309.22
_chemical_name_systematic
;
Dimethyl (3,4-dichlorobenzoyl)carbonohydrazonodithioate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.3670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2225(4)
_cell_length_b                   11.2741(5)
_cell_length_c                   13.0892(5)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    296
_cell_measurement_theta_max      29.744
_cell_measurement_theta_min      2.3885
_cell_volume                     1354.99(10)
_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  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33334
_diffrn_reflns_theta_full        29.83
_diffrn_reflns_theta_max         29.83
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.9143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.314
_refine_ls_abs_structure_details 'Flack (1983), <b>???? Friedel pairs</b>'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         7766
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+0.1856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                7138
_reflns_number_total             7766
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wq3009.cif
_cod_data_source_block           D1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2018439
_cod_database_fobs_code          2018439