Diethyl 2,3-dihydrothieno[3,4-<i>b</i>]-1,4-dioxine-5,7-dicarboxylate
Ono, Katsuhiko; Tomura, Masaaki; Saito, Katsuhiro; Acta Crystallographica Section E 64 (2008) o468–o468; doi:10.1107/S1600536808000937

data_2217534
_publ_section_title
;
 Diethyl 2,3-dihydrothieno[3,4-<i>b</i>]-1,4-dioxine-5,7-dicarboxylate
;
_journal_coeditor_code           HG2368
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o468
_journal_page_last               o468
_journal_paper_doi               10.1107/S1600536808000937
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C12 H14 O6 S'
_chemical_formula_moiety         'C12 H14 O6 S'
_chemical_formula_sum            'C12 H14 O6 S'
_chemical_formula_weight         286.30
_chemical_name_systematic
;
Diethyl 2,3-dihydrothieno[3,4-<i>b</i>]-1,4-dioxine-5,7-dicarboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                94.294(7)
_cell_angle_beta                 92.024(9)
_cell_angle_gamma                105.641(9)
_cell_formula_units_Z            2
_cell_length_a                   4.6805(8)
_cell_length_b                   8.3673(17)
_cell_length_c                   17.351(3)
_cell_measurement_reflns_used    1654
_cell_measurement_temperature    295.0(10)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.31
_cell_volume                     651.4(2)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2001)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2001)'
_computing_molecular_graphics
;
<i>PLATON</i> (Spek, 2003) and <i>MERCURY</i> (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295.0(10)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5181
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.262
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0691
_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^)+(0.0793P)^2^+0.337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1625
_refine_ls_wR_factor_ref         0.1761
_reflns_number_gt                2300
_reflns_number_total             2899
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2368.cif
_cod_data_source_block           I
_cod_database_code               2217534
_cod_database_fobs_code          2217534