Cation Clock Reactions for the Determination of Relative Reaction Kinetics in Glycosylation Reactions: Applications to Gluco- and Mannopyranosyl Sulfoxide and Trichloroacetimidate Type Donors.
Adero, Philip O.; Furukawa, Takayuki; Huang, Min; Mukherjee, Debaraj; Retailleau, Pascal; Bohé, Luis; Crich, David; Journal of the American Chemical Society 137 (2015) 10336–10345; doi:10.1021/jacs.5b06126

data_4124256
_publ_section_title
;
 Cation Clock Reactions for the Determination of Relative Reaction
 Kinetics in Glycosylation Reactions: Applications to Gluco- and
 Mannopyranosyl Sulfoxide and Trichloroacetimidate Type Donors.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10336
_journal_page_last               10345
_journal_paper_doi               10.1021/jacs.5b06126
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C31 H34 O5'
_chemical_formula_weight         486.58
_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                 97.560(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1588(6)
_cell_length_b                   9.3746(6)
_cell_length_c                   12.4312(7)
_cell_measurement_temperature    100(2)
_cell_volume                     1289.12(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker D8'
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29560
_diffrn_reflns_theta_full        31.73
_diffrn_reflns_theta_max         31.73
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.9423
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       columnar
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6573
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0416
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                5880
_reflns_number_total             6573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b06126_si_002.cif
_cod_data_source_block           sac1_p21_s
_cod_depositor_comments
'Adding full bibliography for 4124255--4124256.cif.'
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4124256