(<i>E</i>)-1-[2,6-Dichloro-4-(trifluoromethyl)phenyl]-5-[(dimethylamino)methyleneamino]-1<i>H</i>-pyrazole-4-carboxylic acid
De-Ming Xie; Zhan Shu; Liang Shen; Zhe-Wu Ding; Zhi-Min Jin; Acta Crystallographica Section E 63 (2007) o4562–o4562; doi:10.1107/S1600536807053688

data_2216590
_publ_section_title
;(<i>E</i>)-1-[2,6-Dichloro-4-(trifluoromethyl)phenyl]-5-[(dimethylamino)methyleneamino]-1<i>H</i>-pyrazole-4-carboxylic
 acid
;
_journal_coeditor_code           IS2225
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4562
_journal_page_last               o4562
_journal_paper_doi               10.1107/S1600536807053688
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C14 H11 Cl2 F3 N4 O2'
_chemical_formula_moiety         'C14 H11 Cl2 F3 N4 O2'
_chemical_formula_sum            'C14 H11 Cl2 F3 N4 O2'
_chemical_formula_weight         395.17
_chemical_name_systematic
;
(E)-1-[2,6-Dichloro-4-(trifluoromethyl)phenyl]-5-\
[(dimethylamino)methyleneamino]-1H-pyrazole-4-carboxylic acid
;
_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                 95.626(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.4987(15)
_cell_length_b                   17.5642(16)
_cell_length_c                   11.8035(11)
_cell_measurement_reflns_used    2395
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.96
_cell_measurement_theta_min      2.34
_cell_volume                     3404.0(5)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX area-detector diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8810
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.428
_exptl_absorpt_correction_T_max  0.9308
_exptl_absorpt_correction_T_min  0.8716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2000)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.427
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3000
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+12.0677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1830
_refine_ls_wR_factor_ref         0.1916
_reflns_number_gt                2507
_reflns_number_total             3000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            is2225.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2216590
_cod_database_fobs_code          2216590