Synthesis of a novel 1,2-dithianenucleoside via Pummerer-like reaction, followed by Vorbruggen glycosylation between a 1,2-dithiane derivative and uracil
Tadashi Miyazawa; Kouhei Umezaki; Noriko Tarashima; Kazuhiro Furukawa; Takashi Ooi; Noriaki Minakawa; Chem.Commun. 49 (2013) 7851–; doi:10.1039/c3cc44848g

data_7109680
_publ_section_title
;
 Synthesis of a novel 1,2-dithianenucleoside via Pummerer-like reaction,
 followed by Vorbruggen glycosylation between a 1,2-dithiane derivative
 and uracil
;
_journal_name_full               Chem.Commun.
_journal_page_first              7851
_journal_paper_doi               10.1039/c3cc44848g
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C11 H14 N2 O4 S2 '
_chemical_formula_sum            'C11 H14 N2 O4 S2'
_chemical_formula_weight         302.38
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 91.9959(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.8631(4)
_cell_length_b                   18.8439(6)
_cell_length_c                   12.3763(4)
_cell_measurement_reflns_used    23483
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.2
_cell_volume                     2765.01(16)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      123.1
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9977
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27240
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Higashi, T. (1999). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6301
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0009Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                5498
_reflns_number_total             6314
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3cc44848g.txt
_cod_data_source_block           '_Compound8'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C11 H14 N2 O4 S2 '
_cod_database_code               7109680