1,5-Dimethyl-4-{[1-(3-methyl-5-oxo-1-phenyl-4,5-dihydro-1<i>H</i>-pyrazol-4-ylidene)ethyl]amino}-2-phenyl-1<i>H</i>-pyrazol-3(2<i>H</i>)-one
Zhu, Hualing; Shi, Jun; Wei, Zhen; Bai, Yanan; Bu, Luxia; Acta Crystallographica Section E 66 (2010) o1583–; doi:10.1107/S1600536810020532

data_2226463
_publ_section_title
;
 1,5-Dimethyl-4-{[1-(3-methyl-5-oxo-1-phenyl-4,5-dihydro-1<i>H</i>-pyrazol-4-ylidene)ethyl]amino}-2-phenyl-1<i>H</i>-pyrazol-3(2<i>H</i>)-one
;
_journal_coeditor_code           HB5465
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1583
_journal_paper_doi               10.1107/S1600536810020532
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C23 H23 N5 O2'
_chemical_formula_moiety         'C23 H23 N5 O2'
_chemical_formula_sum            'C23 H23 N5 O2'
_chemical_formula_weight         401.46
_chemical_name_systematic
;
1,5-Dimethyl-4-{[1-(3-methyl-5-oxo-1-phenyl-4,5-dihydro-1<i>H</i>-pyrazol-4-
ylidene)ethyl]amino}-2-phenyl-1<i>H</i>-pyrazol-3(2<i>H</i>)-one
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 102.76(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.486(4)
_cell_length_b                   10.209(2)
_cell_length_c                   19.753(4)
_cell_measurement_reflns_used    5835
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.930
_cell_measurement_theta_min      2.039
_cell_volume                     4029.1(15)
_computing_cell_refinement       'Crystalclear (Rigaku, 2005)'
_computing_data_collection       'Crystalclear (Rigaku, 2005)'
_computing_data_reduction        'Crystalclear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13299
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Crystalclear; Rigaku, 2005)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.197
_refine_ls_extinction_coef       0.0113(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3553
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0698P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1049
_reflns_number_gt                2858
_reflns_number_total             3553
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5465.cif
_cod_data_source_block           I
_cod_original_cell_volume        4029.3(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2226463
_cod_database_fobs_code          2226463