5-Amino-1-phenyl-3-trifluoromethyl-1<i>H</i>-pyrazole-4-carboxylic acid
Caruso, Francesco; Raimondi, Maria Valeria; Daidone, Giuseppe; Pettinari, Claudio; Rossi, Miriam; Acta Crystallographica Section E 65 (2009) o2173–; doi:10.1107/S1600536809032188

data_2223004
_publ_section_title
;
 5-Amino-1-phenyl-3-trifluoromethyl-1<i>H</i>-pyrazole-4-carboxylic
 acid
;
_journal_coeditor_code           BX2218
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2173
_journal_paper_doi               10.1107/S1600536809032188
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C11 H8 F3 N3 O2'
_chemical_formula_moiety         'C11 H8 F3 N3 O2'
_chemical_formula_sum            'C11 H8 F3 N3 O2'
_chemical_formula_weight         271.20
_chemical_name_systematic
;
5-Amino-1-phenyl-3-trifluoromethyl-1<i>H</i>-pyrazole-4-carboxylic acid
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.716(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.757(3)
_cell_length_b                   10.740(3)
_cell_length_c                   21.277(6)
_cell_measurement_reflns_used    3829
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      2.24
_cell_volume                     2224.9(11)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0723
_diffrn_reflns_av_sigmaI/netI    0.0897
_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       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20692
_diffrn_reflns_theta_full        24.69
_diffrn_reflns_theta_max         24.69
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.9927
_exptl_absorpt_correction_T_min  0.9571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat needle'
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.321
_refine_ls_extinction_coef       0.0099(12)
_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   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         3772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0233P)^2^+1.9621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1398
_reflns_number_gt                2737
_reflns_number_total             3772
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bx2218.cif
_cod_data_source_block           I
_cod_original_cell_volume        2225.0(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2223004
_cod_database_fobs_code          2223004