Polymer-Induced Heteronucleation of Tolfenamic Acid: Structural Investigation of a Pentamorph
Vilmalí López-Mejías; Jeff W. Kampf; Adam J. Matzger; Journal of the American Chemical Society 131 (2009) 4554–4555; doi:10.1021/ja806289a

data_4104113
_publ_section_title
;
 Polymer-Induced Heteronucleation of Tolfenamic Acid: Structural
 Investigation of a Pentamorph
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4554
_journal_page_last               4555
_journal_paper_doi               10.1021/ja806289a
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C14 H12 Cl N O2'
_chemical_formula_sum            'C14 H12 Cl N O2'
_chemical_formula_weight         261.70
_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                103.680(2)
_cell_angle_beta                 98.253(2)
_cell_angle_gamma                93.038(2)
_cell_formula_units_Z            6
_cell_length_a                   7.5237(8)
_cell_length_b                   14.3308(16)
_cell_length_c                   17.592(2)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      2.50
_cell_volume                     1816.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0815
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61047
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  0.9728
_exptl_absorpt_correction_T_min  0.9288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  TWINABS  (Version 2007/5), Bruker AXS scaling and
  corrections for twinned crystals University of Gottingen, Germany 2007.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0723
_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^)+(0.0709P)^2^+3.4080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1752
_reflns_number_gt                6236
_reflns_number_total             7521
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806289a_si_002.cif
_cod_data_source_block           tolfo2
_cod_original_cell_volume        1816.5(3)
_cod_database_code               4104113