Diethyl 2,5-bis[(2,3-dihydrothieno[3,4-<i>b</i>][1,4]dioxin-5-yl)methylideneamino]thiophene-3,4-dicarboxylate acetone monosolvate
Dufresne, Stéphane; Bolduc, Andréanne; Skene, W. G.; Acta Crystallographica Section E 67 (2011) o3138–; doi:10.1107/S160053681104339X

data_2232861
_publ_section_title
;
 Diethyl
 2,5-bis[(2,3-dihydrothieno[3,4-<i>b</i>][1,4]dioxin-5-yl)methylideneamino]thiophene-3,4-dicarboxylate
 acetone monosolvate
;
_journal_coeditor_code           MW2024
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3138
_journal_paper_doi               10.1107/S160053681104339X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C24 H22 N2 O8 S3 , C3 H6 O'
_chemical_formula_moiety         'C24 H22 N2 O8 S3, C3 H6 O'
_chemical_formula_sum            'C27 H28 N2 O9 S3'
_chemical_formula_weight         620.69
_chemical_name_systematic
;
Diethyl 2,5-bis[(2,3-dihydrothieno[3,4-<i>b</i>][1,4]dioxin-5-
yl)methylideneamino]thiophene-3,4-dicarboxylate acetone monosolvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.27(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.288(3)
_cell_length_b                   23.541(5)
_cell_length_c                   9.0627(18)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      15.00
_cell_volume                     2805.4(11)
_computing_cell_refinement       'SMART (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'UdMX (Marris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            16861
_diffrn_reflns_theta_full        72.01
_diffrn_reflns_theta_max         72.01
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    2.914
_exptl_absorpt_correction_T_max  0.8923
_exptl_absorpt_correction_T_min  0.5295
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.369
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2718
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0584P)^2^+0.6834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                2215
_reflns_number_total             2718
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            mw2024.cif
_cod_data_source_block           I
_cod_original_cell_volume        2805.5(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2232861
_cod_database_fobs_code          2232861