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_4109244
_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            'C22 H25 N O4 S'
_chemical_formula_weight         399.49
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.540(2)
_cell_length_b                   16.113(3)
_cell_length_c                   24.914(5)
_cell_measurement_temperature    173(2)
_cell_volume                     4231.2(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0918
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48138
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.180
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.412
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.428
_refine_ls_shift/su_mean         0.023
_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          0.1317
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                3169
_reflns_number_total             5201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja068077wsi20061111_063103.cif
_cod_data_source_block           2h
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'ortho.' was replaced with
'orthorhombic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        4231.0(15)
_cod_database_code               4109244