Investigations of Glycosylation Reactions with 2-N-Acetyl-2N,3O-oxazolidinone-Protected Glucosamine Donors
Johan D. M. Olsson; Lars Eriksson; Martina Lahmann; Stefan Oscarson; Journal of Organic Chemistry 73 (2008) 7181–7188; doi:10.1021/jo800971s

data_4023669
_publ_section_title
;
 Investigations of Glycosylation Reactions with
 2-N-Acetyl-2N,3O-oxazolidinone-Protected Glucosamine Donors
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7181
_journal_page_last               7188
_journal_paper_doi               10.1021/jo800971s
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C15 H21 N O8 S'
_chemical_formula_sum            'C15 H21 N O8 S'
_chemical_formula_weight         375.39
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.382(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.2144(6)
_cell_length_b                   15.5943(12)
_cell_length_c                   11.3014(12)
_cell_measurement_reflns_used    549
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     914.92(16)
_computing_cell_refinement       'Cell (Stoe, 1997)'
_computing_data_collection       'Expose (Stoe, 1997)'
_computing_data_reduction        'Integrate (Stoe, 1997)'
_computing_molecular_graphics    'Diamond (Bergerhof, 1996)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'Area detector - \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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14476
_diffrn_reflns_theta_full        28.11
_diffrn_reflns_theta_max         28.11
_diffrn_reflns_theta_min         2.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
X-Red version 1.09 (Stoe, 1997).
;
_exptl_crystal_colour            colour_less
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         4393
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1603P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1697
_reflns_number_gt                3357
_reflns_number_total             4393
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo800971s_si_001.cif
_cod_data_source_block           jo1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4023669