One-Pot Synthesis of Glycosyl-β-azido Ester via Diazotransfer Reaction Toward Access of Glycosyl-β-triazolyl Ester.
Mishra, Amrita; Tiwari, Vinod K.; The Journal of organic chemistry 80 (2015) 4869–4881; doi:10.1021/acs.joc.5b00179

data_4031062
_publ_section_title
;
 One-Pot Synthesis of Glycosyl-\b-azido Ester via Diazotransfer Reaction
 Toward Access of Glycosyl-\b-triazolyl Ester.
;
_journal_issue                   10
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              4869
_journal_page_last               4881
_journal_paper_doi               10.1021/acs.joc.5b00179
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C21 H26 N3 O6, C6 H5, C H2 O'
_chemical_formula_sum            'C28 H33 N3 O7'
_chemical_formula_weight         523.57
_chemical_name_systematic
;
 ?
;
_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                 90.485(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7814(10)
_cell_length_b                   10.1234(8)
_cell_length_c                   26.655(3)
_cell_measurement_reflns_used    952
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8347
_cell_measurement_theta_min      2.9773
_cell_volume                     2909.1(5)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies ltd.'
_computing_data_collection       'CrysAlisPro, Agilent Technologies ltd.'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies ltd.'
_computing_publication_material  'CrysAlisPro, Agilent Technologies ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0938
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.692
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_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  0.0527
_diffrn_reflns_av_sigmaI/netI    0.1753
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11517
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42054
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         8333
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.2651
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0967P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2027
_refine_ls_wR_factor_ref         0.2498
_reflns_number_gt                2648
_reflns_number_total             8333
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo5b00179_si_001.cif
_cod_data_source_block           compound-6a
_cod_database_code               4031062