Dynamic Kinetic Resolution of Allylic Azides via Asymmetric Dihydroxylation.
Ott, Amy A.; Goshey, Charles S.; Topczewski, Joseph J.; Journal of the American Chemical Society 139 (2017) 7737–7740; doi:10.1021/jacs.7b04203

data_4126191
_publ_section_title
;
 Dynamic Kinetic Resolution of Allylic Azides via Asymmetric
 Dihydroxylation.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7737
_journal_page_last               7740
_journal_paper_doi               10.1021/jacs.7b04203
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C17 H19 N3 O2'
_chemical_formula_weight         297.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.9690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.0290(2)
_cell_length_b                   10.7498(4)
_cell_length_c                   11.6520(4)
_cell_measurement_temperature    293(2)
_cell_volume                     754.16(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15848
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.936
_diffrn_reflns_theta_min         3.799
_exptl_absorpt_coefficient_mu    0.707
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_F_000             316
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.137
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details
;
 Flack x determined using 1348 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2968
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.1214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0711
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                2923
_reflns_number_total             2968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04203_si_003.cif
_cod_data_source_block           15259_0m-auto
_cod_depositor_comments
'Adding full bibliography for 4126190--4126191.cif.'
_cod_database_code               4126191
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              5408
_shelx_hkl_checksum              34997