Ethyl (1-methyl-3-phenyl-5-thioxo-4,5-dihydro-1<i>H</i>-1,2,4-triazol-4-yl)acetate
Kruszynski, Rafal; Trzesowska, Agata; Przybycin, Magdalena; Dopieralski, Mariusz; Dobosz, Maria; Acta Crystallographica Section E 63 (2007) o4371–o4371; doi:10.1107/S1600536807050635

data_2215807
_publ_section_title
;
 Ethyl
 (1-methyl-3-phenyl-5-thioxo-4,5-dihydro-1<i>H</i>-1,2,4-triazol-4-yl)acetate
;
_journal_coeditor_code           BT2537
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4371
_journal_page_last               o4371
_journal_paper_doi               10.1107/S1600536807050635
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C13 H15 N3 O2 S'
_chemical_formula_moiety         'C13 H15 N3 O2 S'
_chemical_formula_sum            'C13 H15 N3 O2 S'
_chemical_formula_weight         277.34
_chemical_name_systematic
;
Ethyl (1-methyl-3-phenyl-5-thioxo-4,5-dihydro-1H-1,2,4-triazol-4-yl)acetate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6493(8)
_cell_length_b                   12.8459(10)
_cell_length_c                   14.2061(11)
_cell_measurement_reflns_used    99
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      60
_cell_measurement_theta_min      5
_cell_volume                     1395.9(2)
_computing_cell_refinement       'KM-4 Software (Kuma, 1993)'
_computing_data_collection       'KM-4 Software (Kuma, 1993)'
_computing_data_reduction
;
DATAPROC (Version 10.0.4; Ga\/ldecki <i>et al.</i>,  1998)
;
_computing_molecular_graphics
;
XP in SHELXTL/PC (Sheldrick, 1990b) and
ORTEP-3 for Windows (Version 1.062; Farrugia 1997)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 1997) and
PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990a)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Kuma KM-4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3095
_diffrn_reflns_theta_full        68.00
_diffrn_reflns_theta_max         80.74
_diffrn_reflns_theta_min         4.64
_diffrn_standards_decay_%        4.74
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.085
_exptl_absorpt_correction_T_max  0.6805
_exptl_absorpt_correction_T_min  0.4893
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.255
_refine_ls_abs_structure_details 'Flack (1983), 1112 Friedel pairs'
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_coef       0.0114(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0798P)^2^+0.0731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                2386
_reflns_number_total             2887
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2537.cif
_cod_data_source_block           I
_cod_database_code               2215807
_cod_database_fobs_code          2215807