4-[(1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1<i>H</i>-pyrazol-4-yl)iminomethyl]benzoic acid methanol solvate
Sun, Yu-Xi; Xie, Xue-Hui; Zhang, Ran; Zhang, Li-Feng; Xu, Lai-Xiang; Acta Crystallographica Section E 62 (2006) o4758–o4760; doi:10.1107/S1600536806039262

data_2210555
_publ_section_title
;4-[(1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1<i>H</i>-pyrazol-4-yl)iminomethyl]benzoic
 acid methanol solvate
;
_journal_coeditor_code           CI2176
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4758
_journal_page_last               o4760
_journal_paper_doi               10.1107/S1600536806039262
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C19 H17 N3 O3, C H4 O'
_chemical_formula_moiety         'C19 H17 N3 O3, C H4 O'
_chemical_formula_sum            'C20 H21 N3 O4'
_chemical_formula_weight         367.40
_chemical_name_systematic
;4-(1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)iminomethyl]benzoic
acid
 methanol solvate
;
_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                74.4500(10)
_cell_angle_beta                 85.6730(10)
_cell_angle_gamma                75.6650(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4270(7)
_cell_length_b                   10.2516(8)
_cell_length_c                   10.3014(8)
_cell_measurement_reflns_used    2860
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.95
_cell_measurement_theta_min      2.54
_cell_volume                     929.20(12)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Bruker, 2002)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX 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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0385
_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       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6972
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9726
_exptl_absorpt_correction_T_min  0.9594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.228
_refine_ls_extinction_coef       0.029(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3760
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0797
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0943P)^2^+0.0586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1764
_reflns_number_gt                2595
_reflns_number_total             3760
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2176.cif
_cod_data_source_block           I
_cod_database_code               2210555
_cod_database_fobs_code          2210555