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_4106909
_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 H13 F3 O7'
_chemical_formula_weight         314.21
_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                 103.040(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.6002(9)
_cell_length_b                   13.903(5)
_cell_length_c                   9.2080(8)
_cell_measurement_reflns_used    2225
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      2.0
_cell_volume                     698.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.847
_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  0.0560
_diffrn_reflns_av_sigmaI/netI    0.1160
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3193
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.59
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       plate
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   3.1(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.778
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3193
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.778
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                1453
_reflns_number_total             3193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204829r_si_003.cif
_cod_data_source_block           sw109
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4106909