Ethyl 3-[2-(<i>p</i>-tolylcarbamothioyl)hydrazinylidene]butanoate
Zhang, Yan-Ling; Hou, Xu-Feng; Zhang, Fu-Juan; Yang, Feng-Ling; Acta Crystallographica Section E 66 (2010) o2971–; doi:10.1107/S160053681004290X

data_2228140
_publ_section_title
;
 Ethyl 3-[2-(<i>p</i>-tolylcarbamothioyl)hydrazinylidene]butanoate
;
_journal_coeditor_code           XU5056
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2971
_journal_paper_doi               10.1107/S160053681004290X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C14 H19 N3 O2 S'
_chemical_formula_moiety         'C14 H19 N3 O2 S'
_chemical_formula_sum            'C14 H19 N3 O2 S'
_chemical_formula_weight         293.38
_chemical_name_systematic
;
Ethyl 3-[2-(<i>p</i>-tolylcarbamothioyl)hydrazinylidene]butanoate
;
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   14.1747(3)
_cell_length_b                   25.1439(4)
_cell_length_c                   17.4381(2)
_cell_measurement_reflns_used    4042
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.1910
_cell_measurement_theta_min      3.0815
_cell_volume                     6215.07(18)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6852
_diffrn_reflns_theta_full        67.03
_diffrn_reflns_theta_max         67.03
_diffrn_reflns_theta_min         3.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.897
_exptl_absorpt_correction_T_max  0.7264
_exptl_absorpt_correction_T_min  0.7029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis Pro; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.365
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2775
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0565
_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^)+(0.1110P)^2^+3.4880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1747
_reflns_number_gt                2380
_reflns_number_total             2775
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5056.cif
_cod_data_source_block           I
_cod_original_cell_volume        6215.08(17)
_cod_database_code               2228140
_cod_database_fobs_code          2228140