4-Carbethoxy-1-[4-(<i>N</i>,<i>N</i>-dimethylamino)benzoyl]thiosemicarbazide
Bera, Hriday; Dolzhenko, Anton V.; Tan, Geok Kheng; Koh, Lip Lin; Chui, Wai Keung; Acta Crystallographica Section E 66 (2010) o1241–; doi:10.1107/S1600536810015576

data_2225825
_publ_section_title
;
 4-Carbethoxy-1-[4-(<i>N</i>,<i>N</i>-dimethylamino)benzoyl]thiosemicarbazide
;
_journal_coeditor_code           DS2029
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1241
_journal_paper_doi               10.1107/S1600536810015576
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C13 H18 N4 O3 S'
_chemical_formula_moiety         'C13 H18 N4 O3 S'
_chemical_formula_sum            'C13 H18 N4 O3 S'
_chemical_formula_weight         310.37
_chemical_melting_point          474
_chemical_name_common
;
1-[4-(Dimethylamino)benzoyl]-4-(ethoxycarbonyl)thiosemicarbazide
;
_chemical_name_systematic
;
Ethyl <i>N</i>-{2-[4-(dimethylamino)benzoyl]hydrazinethiocarbonyl}carbamate
;
_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           SHELXL-97
_cell_angle_alpha                82.290(12)
_cell_angle_beta                 74.769(11)
_cell_angle_gamma                84.469(11)
_cell_formula_units_Z            2
_cell_length_a                   7.876(4)
_cell_length_b                   8.184(4)
_cell_length_c                   12.086(6)
_cell_measurement_reflns_used    644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.52
_cell_volume                     743.3(6)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5201
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.9815
_exptl_absorpt_correction_T_min  0.9460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.453
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0806
_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^)+(0.0987P)^2^+1.3625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1988
_refine_ls_wR_factor_ref         0.2181
_reflns_number_gt                2839
_reflns_number_total             3379
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ds2029.cif
_cod_data_source_block           I
_cod_original_cell_volume        743.3(7)
_cod_database_code               2225825
_cod_database_fobs_code          2225825