1-(4-Carboxybutan-2-ylidene)-4-phenylthiosemicarbazide
Mendoza-Meroño, Rafael; Menéndez-Taboada, Laura; García-Granda, Santiago; Acta Crystallographica Section E 68 (2012) o1945–o1946; doi:10.1107/S1600536812023793

data_2234972
_publ_section_title
;
 1-(4-Carboxybutan-2-ylidene)-4-phenylthiosemicarbazide
;
_journal_coeditor_code           DS2195
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1945
_journal_page_last               o1946
_journal_paper_doi               10.1107/S1600536812023793
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C12 H15 N3 O2 S'
_chemical_formula_moiety         'C12 H15 N3 O2 S'
_chemical_formula_sum            'C12 H15 N3 O2 S'
_chemical_formula_weight         265.33
_chemical_melting_point          437
_chemical_name_common
'4-phenyl-1-(4-oxopentanoic acid)thiosemicarbazone'
_chemical_name_systematic
;
1-(4-Carboxybutan-2-ylidene)-4-phenylthiosemicarbazide
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.000
_cell_angle_beta                 104.176(3)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   11.2812(4)
_cell_length_b                   9.3450(4)
_cell_length_c                   13.4120(5)
_cell_measurement_reflns_used    6997
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.3842
_cell_measurement_theta_min      3.3959
_cell_volume                     1370.87(9)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2010)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and Mercury  (Macrae
<i>et al.</i>, 2008)
;
_computing_publication_material
;
WinGX publication routines (Farrugia, 1999),
PLATON (Spek, 2003), PARST-95 (Nardelli, 1995) and
publCIF (Westrip, 2010).
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.2673
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Ruby Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12283
_diffrn_reflns_theta_full        70.52
_diffrn_reflns_theta_max         70.52
_diffrn_reflns_theta_min         4.04
_diffrn_standards_number         12646
_exptl_absorpt_coefficient_mu    2.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2010)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.2599
_exptl_crystal_size_mid          0.1755
_exptl_crystal_size_min          0.1152
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0645P)^2^+0.3083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                2294
_reflns_number_total             2601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ds2195.cif
_cod_data_source_block           I
_cod_database_code               2234972
_cod_database_fobs_code          2234972