Structural, Mechanistic, and Computational Analysis of the Effects of Anomeric Fluorines on Anomeric Fluoride Departure in 5-Fluoroxylosyl Fluorides
Seung Seo Lee; Ian R. Greig; David J. Vocadlo; John D. McCarter; Brian O. Patrick; Stephen G. Withers; Journal of the American Chemical Society 133 (2011) 15826–15829; doi:10.1021/ja204829r

data_4106911
_publ_section_title
;
 Structural, Mechanistic, and Computational Analysis of the Effects of
 Anomeric Fluorines on Anomeric Fluoride Departure in 5-Fluoroxylosyl
 Fluorides
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15826
_journal_page_last               15829
_journal_paper_doi               10.1021/ja204829r
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C11 H14 F2 O7'
_chemical_formula_weight         296.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.350(10)
_cell_angle_beta                 75.230(10)
_cell_angle_gamma                83.420(10)
_cell_formula_units_Z            6
_cell_length_a                   8.6224(8)
_cell_length_b                   13.4210(16)
_cell_length_c                   18.0267(13)
_cell_measurement_reflns_used    12727
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      2.34
_cell_volume                     2000.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.839
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_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  0.045
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8015
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       chip
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0732P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1725
_reflns_number_gt                6089
_reflns_number_total             8015
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204829r_si_005.cif
_cod_data_source_block           sw122
_cod_database_code               4106911