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_4106908
_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
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.6950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.529(2)
_cell_length_b                   16.795(5)
_cell_length_c                   9.3511(4)
_cell_measurement_reflns_used    12674
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      30.70
_cell_measurement_theta_min      3.26
_cell_volume                     1338.9(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.811
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_sigmaI/netI    0.1777
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3373
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.70
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       plate
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0090(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.808
_refine_ls_R_factor_all          0.2100
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                1149
_reflns_number_total             3373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204829r_si_002.cif
_cod_data_source_block           sw106
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4106908