Nonamorphism in Flufenamic Acid and a New Record for a Polymorphic Compound with Solved Structures
Vilmalí López-Mejías; Jeff W. Kampf; Adam J. Matzger; Journal of the American Chemical Society 134 (2012) 9872–9875; doi:10.1021/ja302601f

data_4118081
_publ_section_title
;
 Nonamorphism in Flufenamic Acid and a New Record for a Polymorphic
 Compound with Solved Structures
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9872
_journal_page_last               9875
_journal_paper_doi               10.1021/ja302601f
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C14 H10 F3 N O2'
_chemical_formula_sum            'C14 H10 F3 N O2'
_chemical_formula_weight         281.23
_chemical_melting_point          397.09
_chemical_name_common            'flufenamic acid'
_chemical_name_systematic
;
 2-[[3-(trifluoromethyl)phenyl]amino]benzoic acid
;
_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                80.632(6)
_cell_angle_beta                 81.041(6)
_cell_angle_gamma                73.532(5)
_cell_formula_units_Z            6
_cell_length_a                   8.7589(2)
_cell_length_b                   11.6629(3)
_cell_length_c                   20.0229(14)
_cell_measurement_reflns_used    16515
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      68.10
_cell_measurement_theta_min      2.30
_cell_volume                     1922.33(16)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r5'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r5'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Rigaku Saturn70 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0962
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31175
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_diffrn_reflns_theta_min         3.98
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         6770
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0610P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                3562
_reflns_number_total             6770
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja302601f_si_001_4.cif
_cod_data_source_block           faf273_FORM_4
_cod_original_cell_volume        1922.33(15)
_cod_database_code               4118081