Tetrasubstituted Pyrrolidines via a Tandem Aza-Payne/Hydroamination Reaction
Jennifer M. Schomaker; Andrea R. Geiser; Rui Huang; Babak Borhan; Journal of the American Chemical Society 129 (2007) 3794–3795; doi:10.1021/ja068077w

data_4109243
_publ_section_title
;
 Tetrasubstituted Pyrrolidines via a Tandem Aza-Payne/Hydroamination
 Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3794
_journal_page_last               3795
_journal_paper_doi               10.1021/ja068077w
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C21 H23 N O4 S'
_chemical_formula_weight         385.46
_chemical_name_systematic
; 
 ? 
;
_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                 113.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.475(2)
_cell_length_b                   22.938(5)
_cell_length_c                   9.1934(18)
_cell_measurement_temperature    173(2)
_cell_volume                     2025.9(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21223
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.185
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_F_000             816
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.812
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         9452
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.812
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          2.655
_refine_ls_shift/su_mean         0.265
_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          0.0998
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                7293
_reflns_number_total             9452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja068077wsi20061111_063039.cif
_cod_data_source_block           2d
_cod_original_cell_volume        2025.9(7)
_cod_database_code               4109243