4-[(5-Chloro-3-methyl-1-phenyl-1<i>H</i>-pyrazol-4-yl)methylideneamino]-1,5-dimethyl-2-phenyl-1<i>H</i>-pyrazol-3(2<i>H</i>)-one
Zhu, Hualing; Zhu, Jinhua; Ban, Litong; Zhang, Pingping; Zhang, Miao; Acta Crystallographica Section E 66 (2010) o2724–; doi:10.1107/S1600536810039048

data_2227792
_publ_section_title
;
 4-[(5-Chloro-3-methyl-1-phenyl-1<i>H</i>-pyrazol-4-yl)methylideneamino]-1,5-dimethyl-2-phenyl-1<i>H</i>-pyrazol-3(2<i>H</i>)-one
;
_journal_coeditor_code           LH5137
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2724
_journal_paper_doi               10.1107/S1600536810039048
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C22 H20 Cl N5 O'
_chemical_formula_moiety         'C22 H20 Cl N5 O'
_chemical_formula_sum            'C22 H20 Cl N5 O'
_chemical_formula_weight         405.88
_chemical_name_systematic
;
4-[(5-Chloro-3-methyl-1-phenyl-1<i>H</i>-pyrazol-4-yl)methylideneamino]-
1,5-dimethyl-2-phenyl-1<i>H</i>-pyrazol-3(2<i>H</i>)-one
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3982(17)
_cell_length_b                   9.5204(19)
_cell_length_c                   24.401(5)
_cell_measurement_reflns_used    4998
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.866
_cell_measurement_theta_min      1.683
_cell_volume                     1935.4(7)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>,
2006)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            15458
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.9781
_exptl_absorpt_correction_T_min  0.9570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2008)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.247
_refine_ls_extinction_coef       0.0242(16)
_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   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0533P)^2^+0.6515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                2871
_reflns_number_total             3397
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5137.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2227792
_cod_database_fobs_code          2227792