Crystal structure of diethyl 2-amino-6-[(thiophen-3-yl)ethynyl]azulene-1,3-dicarboxylate
Förster, Sebastian; Seichter, Wilhelm; Weber, Edwin; Acta Crystallographica Section E 71 (2015) o212–o213; doi:10.1107/S2056989015003898

data_2240463
_publ_section_title
;
 Crystal structure of diethyl
 2-amino-6-[(thiophen-3-yl)ethynyl]azulene-1,3-dicarboxylate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o212
_journal_page_last               o213
_journal_paper_doi               10.1107/S2056989015003898
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C22 H19 N O4 S'
_chemical_formula_moiety         'C22 H19 N O4 S'
_chemical_formula_sum            'C22 H19 N O4 S'
_chemical_formula_weight         393.44
_chemical_name_systematic
;
Diethyl 2-amino-6-[(thiophen-3-yl)ethynyl]azulene-1,3-dicarboxylate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 102.9140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.2429(5)
_cell_length_b                   5.50390(10)
_cell_length_c                   32.8340(8)
_cell_measurement_reflns_used    4036
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.91
_cell_measurement_theta_min      2.49
_cell_volume                     3917.96(15)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(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       'phi and omega scans'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            18444
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.598
_diffrn_reflns_theta_min         2.546
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.9923
_exptl_absorpt_correction_T_min  0.9094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       rod
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.691
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1341P)^2^+7.3721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2419
_reflns_number_gt                2441
_reflns_number_total             3679
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5088sup1.cif
_cod_data_source_block           I
_cod_database_code               2240463
_cod_database_fobs_code          2240463
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.992
_shelx_hkl_checksum              43666
_shelx_res_checksum              36591
_shelxl_version_number           2014/6