Pleconaril Polymorphs: Crystal Structures of Form I and Form III, Evidence of the Enantiotropy, and Assessment of the Structural Purity
Coste, Servane; Schneider, Jean-Marie; Petit, Marie-Noëlle; Coquerel, Gérard; Crystal Growth & Design 4 (2004) 1237–; doi:10.1021/cg049766r

data_4505374
_publ_section_title
;
 Pleconaril Polymorphs:&#x2009; Crystal Structures of Form I and Form III,
 Evidence of the Enantiotropy, and Assessment of the Structural Purity
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1237
_journal_paper_doi               10.1021/cg049766r
_journal_volume                  4
_journal_year                    2004
_chemical_formula_moiety         'C18 H18 F3 N3 O3'
_chemical_formula_sum            'C18 H18 F3 N3 O3'
_chemical_formula_weight         381.35
_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                89.447(3)
_cell_angle_beta                 88.427(3)
_cell_angle_gamma                81.715(3)
_cell_formula_units_Z            2
_cell_length_a                   4.8343(9)
_cell_length_b                   11.984(2)
_cell_length_c                   16.206(3)
_cell_measurement_temperature    296(2)
_cell_volume                     928.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7448
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.566728
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.094(12)
_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   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3716
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1171P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.1912
_reflns_number_gt                2373
_reflns_number_total             3716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg049766rsi20040710_120007.cif
_cod_data_source_block           pleconaril_form_I_296K
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4505374