Dimethyl 3<i>t</i>,4<i>t</i>-dicarboxytetrahydrofuran-2<i>r</i>,5<i>c</i>-dicarboxylate
Villiers, Claude; Thuéry, Pierre; Ephritikhine, Michel; Acta Crystallographica Section E 62 (2006) o1724–o1726; doi:10.1107/S1600536806011755

data_2208868
_publ_section_title
;Dimethyl
 3<i>t</i>,4<i>t</i>-dicarboxytetrahydrofuran-2<i>r</i>,5<i>c</i>-dicarboxylate
;
_journal_coeditor_code           DN2022
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1724
_journal_page_last               o1726
_journal_paper_doi               10.1107/S1600536806011755
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C10 H12 O9'
_chemical_formula_moiety         'C10 H12 O9'
_chemical_formula_sum            'C10 H12 O9'
_chemical_formula_weight         276.20
_chemical_name_systematic
;
Dimethyl 3t,4t-dicarboxytetrahydrofuran-2r,5c-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                 96.634(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.5117(4)
_cell_length_b                   25.419(3)
_cell_length_c                   8.1970(7)
_cell_measurement_reflns_used    7691
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.97
_cell_volume                     1140.73(19)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \f
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7691
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_description       platelet
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.267
_refine_ls_extinction_coef       0.015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0165P)^2^+0.7399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                1700
_reflns_number_total             2112
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2022.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2208868
_cod_database_fobs_code          2208868