Diethyl 2-amino-5-[(<i>E</i>)-(1-methyl-1<i>H</i>-pyrrol-2-yl)methylideneamino]thiophene-3,4-dicarboxylate
Dufresne, Stéphane; Skene, W. G.; Acta Crystallographica Section E 66 (2010) o3221–; doi:10.1107/S1600536810046775

data_2228212
_publ_section_title
;
 Diethyl
 2-amino-5-[(<i>E</i>)-(1-methyl-1<i>H</i>-pyrrol-2-yl)methylideneamino]thiophene-3,4-dicarboxylate
;
_journal_coeditor_code           BH2321
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3221
_journal_paper_doi               10.1107/S1600536810046775
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C16 H19 N3 O4 S'
_chemical_formula_moiety         'C16 H19 N3 O4 S'
_chemical_formula_sum            'C16 H19 N3 O4 S'
_chemical_formula_weight         349.40
_chemical_melting_point          404(2)
_chemical_name_systematic
'Diethyl 2-amino-5-[(<i>E</i>)-(1-methyl-1<i>H</i>-pyrrol-2-yl)methylideneamino]thiophene-3,4-dicarboxylate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8212(18)
_cell_length_b                   9.0799(18)
_cell_length_c                   21.793(4)
_cell_measurement_reflns_used    10603
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      71.33
_cell_measurement_theta_min      4.09
_cell_volume                     1730.6(6)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'UdMX (Marris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Montel 200 optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20876
_diffrn_reflns_theta_full        71.97
_diffrn_reflns_theta_max         71.97
_diffrn_reflns_theta_min         4.09
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  1080
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_T_max  0.762
_exptl_absorpt_correction_T_min  0.7100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick,1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.540
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3367
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0845P)^2^+0.1530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                3046
_reflns_number_total             3367
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2321.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2228212
_cod_database_fobs_code          2228212