Epalrestat tetrahydrofuran monosolvate: crystal structure and phase transition
Umeda, Daiki; Putra, Okky Dwichandra; Gunji, Mihoko; Fukuzawa, Kaori; Yonemochi, Etsuo; Acta Crystallographica Section E 73 (2017) 941–944; doi:10.1107/S2056989017007976

data_2242224
_publ_section_title
;
 Epalrestat tetrahydrofuran monosolvate: crystal structure and phase
 transition
;
_journal_coeditor_code           SU5372
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              941
_journal_page_last               944
_journal_paper_doi               10.1107/S2056989017007976
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C15 H13 N O3 S2, C4 H8 O'
_chemical_formula_moiety         'C15 H13 N O3 S2, C4 H8 O'
_chemical_formula_sum            'C19 H21 N O4 S2'
_chemical_formula_weight         391.49
_chemical_name_common
;
Epalrestat tetrahydrofuran monosolvate
;
_chemical_name_systematic
'(5<i>Z</i>)-5-[(2<i>E</i>)-2-Methyl-3-phenylprop-2-en-1-ylidene]-4-oxo-2-sulfanylidene-1,3-thiazolidine-3-acetic acid tetrahydrofuran monosolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                102.263(7)
_cell_angle_beta                 93.970(7)
_cell_angle_gamma                114.219(8)
_cell_formula_units_Z            2
_cell_length_a                   7.8956(3)
_cell_length_b                   8.9627(3)
_cell_length_c                   15.0311(4)
_cell_measurement_reflns_used    10947
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.24
_cell_measurement_theta_min      3.06
_cell_volume                     933.23(9)
_computing_cell_refinement
;
PROCESS-AUTO (Rigaku, 1998)
;
_computing_data_collection
;
PROCESS-AUTO (Rigaku, 1998)
;
_computing_data_reduction
;
PROCESS-AUTO (Rigaku, 1998)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al</i>, 2008)
;
_computing_publication_material
;
SHELXL2016 (Sheldrick, 2015), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2014 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID II'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10947
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.239
_diffrn_reflns_theta_min         3.056
_exptl_absorpt_coefficient_mu    2.797
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       plate
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.442
_exptl_crystal_size_mid          0.329
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.413
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         3342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.6912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                3184
_reflns_number_total             3342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5372sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        933.23(8)
_cod_database_code               2242224
_cod_database_fobs_code          2242224
_shelx_estimated_absorpt_t_min   0.371
_shelx_estimated_absorpt_t_max   0.736
_shelx_hkl_checksum              45038
_shelx_res_checksum              78002