Ethyl (<i>E</i>)-3-hydroxy-2-{<i>N</i>-[2-(thiophen-2-yl)ethenyl]carbamoyl}but-2-enoate
Liu, Bao-Shuo; Zhao, Sheng-Yin; Acta Crystallographica Section E 68 (2012) o2284–; doi:10.1107/S1600536812028176

data_2235728
_publ_section_title
;
 Ethyl
 (<i>E</i>)-3-hydroxy-2-{<i>N</i>-[2-(thiophen-2-yl)ethenyl]carbamoyl}but-2-enoate
;
_journal_coeditor_code           ZS2216
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2284
_journal_paper_doi               10.1107/S1600536812028176
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C13 H15 N O4 S'
_chemical_formula_moiety         'C13 H15 N O4 S'
_chemical_formula_sum            'C13 H15 N O4 S'
_chemical_formula_weight         281.33
_chemical_melting_point_gt       366
_chemical_melting_point_lt       368
_chemical_name_systematic
;
Ethyl (<i>E</i>)-3-hydroxy-2-{<i>N</i>-[2-
(thiophen-2-yl)ethenyl]carbamoyl}but-2-enoate
;
_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                 96.853(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.0185(15)
_cell_length_b                   13.1232(14)
_cell_length_c                   15.0141(16)
_cell_measurement_reflns_used    3746
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.471
_cell_measurement_theta_min      4.874
_cell_volume                     2742.4(5)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15596
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         5099
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0569
_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^)+(0.1017P)^2^+0.3594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1793
_reflns_number_gt                3538
_reflns_number_total             5099
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zs2216.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2235728
_cod_database_fobs_code          2235728