A substituted EDOT precursor: diethyl 3,4-dihydroxythiophene-2,5-dicarboxylate
Faulmann, Christophe; Pullen, Anthony E.; Acta Crystallographica Section C 60 (2004) o338–o340; doi:10.1107/S0108270104006754

data_2014054
_publ_section_title
;
 A substituted EDOT precursor: diethyl
 3,4-dihydroxythiophene-2,5-dicarboxylate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o338
_journal_page_last               o340
_journal_paper_doi               10.1107/S0108270104006754
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C10 H12 O6 S'
_chemical_formula_moiety         'C10 H12 O6 S'
_chemical_formula_sum            'C10 H12 O6 S'
_chemical_formula_weight         260.27
_chemical_name_common            2,5-Dicarbethoxy-3,4-dihydroxythiophene
_chemical_name_systematic
;
diethyl 3,4-dihydroxythiophene-2,5-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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 99.059(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.7337(9)
_cell_length_b                   19.8208(14)
_cell_length_c                   13.6271(15)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      2.35
_cell_volume                     2329.5(4)
_computing_cell_refinement       'IPDS Software'
_computing_data_collection
;
IPDS Software (Stoe & Cie, 1996)
;
_computing_data_reduction        'IPDS Software'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and CAMERON (Watkin et al., 1996)
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE imaging-plate'
_diffrn_measurement_method       '\f scan'
_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  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20063
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 (Blessing, 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         4535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0720
_reflns_number_gt                3225
_reflns_number_total             4535
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1705.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2014054
_cod_database_fobs_code          2014054