4-[(2,4-Difluorophenyl)hydrazinylidene]-3-methyl-5-oxo-4,5-dihydro-1<i>H</i>-pyrazole-1-carbothioamide
Fun, Hoong-Kun; Asik, Safra Izuani Jama; Razak, Ibrahim Abdul; Shetty, Shobhitha; Kalluraya, Balakrishna; Acta Crystallographica Section E 67 (2011) o3116–; doi:10.1107/S1600536811044576

data_2232358
_publ_section_title
;
 4-[(2,4-Difluorophenyl)hydrazinylidene]-3-methyl-5-oxo-4,5-dihydro-1<i>H</i>-pyrazole-1-carbothioamide
;
_journal_coeditor_code           IS2796
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3116
_journal_paper_doi               10.1107/S1600536811044576
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C11 H9 F2 N5 O S'
_chemical_formula_moiety         'C11 H9 F2 N5 O S'
_chemical_formula_sum            'C11 H9 F2 N5 O S'
_chemical_formula_weight         297.29
_chemical_name_systematic
;
4-[(2,4-Difluorophenyl)hydrazinylidene]-3-methyl-5-oxo-4,5-dihydro-
1<i>H</i>-pyrazole-1-carbothioamide
;
_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                103.4090(10)
_cell_angle_beta                 99.8640(10)
_cell_angle_gamma                99.3720(10)
_cell_formula_units_Z            2
_cell_length_a                   7.90030(10)
_cell_length_b                   8.24000(10)
_cell_length_c                   10.13780(10)
_cell_measurement_reflns_used    7383
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      31.86
_cell_measurement_theta_min      2.60
_cell_volume                     618.184(13)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Bruker SMART APEXII 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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15661
_diffrn_reflns_theta_full        31.86
_diffrn_reflns_theta_max         31.86
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.290
_exptl_absorpt_correction_T_max  0.9769
_exptl_absorpt_correction_T_min  0.8902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         4211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0334
_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^+0.1483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                3546
_reflns_number_total             4211
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is2796.cif
_cod_data_source_block           I
_cod_original_cell_volume        618.184(12)
_cod_database_code               2232358
_cod_database_fobs_code          2232358