(1<i>S</i>)-Benzyl 3-methyl-5-oxo-4-phenylhydrazono-4,5-dihydro-1<i>H</i>-pyrazole-1-dithiocarboxylate
Liu, Yong-Hong; Zhao, Yue; Liu, Xiao-Lan; Tong, Ben-Wan; Ye, Jun; Acta Crystallographica Section E 63 (2007) o4072–o4072; doi:10.1107/S1600536807044327

data_2215596
_publ_section_title
;(1<i>S</i>)-Benzyl
 3-methyl-5-oxo-4-phenylhydrazono-4,5-dihydro-1<i>H</i>-pyrazole-1-dithiocarboxylate
;
_journal_coeditor_code           LW2028
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4072
_journal_page_last               o4072
_journal_paper_doi               10.1107/S1600536807044327
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C18 H16 N4 O S2'
_chemical_formula_moiety         'C18 H16 N4 O S2'
_chemical_formula_sum            'C18 H16 N4 O S2'
_chemical_formula_weight         368.47
_chemical_name_systematic
;
(1<i>S</i>)-Benzyl
3-methyl-5-oxo-4-phenylhydrazono-4,5-dihydro-1H-pyrazole-1-dithiocarboxylate
;
_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           SHELXL97
_cell_angle_alpha                84.059(10)
_cell_angle_beta                 79.410(11)
_cell_angle_gamma                77.095(9)
_cell_formula_units_Z            2
_cell_length_a                   9.143(6)
_cell_length_b                   10.079(6)
_cell_length_c                   10.217(6)
_cell_measurement_reflns_used    1587
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.81
_cell_volume                     900.2(10)
_computing_cell_refinement       'SMART (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4385
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  0.9522
_exptl_absorpt_correction_T_min  0.9295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0469P)^2^+0.22P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                1974
_reflns_number_total             3062
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lw2028.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2215596
_cod_database_fobs_code          2215596