Catalytic Asymmetric Cycloaddition with Unsymmetrical EWG-activated Alkenes to Fully Substituted Pyrrolidines Bearing Three Different Carbonyl Groups
Wu, Shi-Lu; Li, Ning; Yin, Guan-Wu; Xu, Zheng; Ye, Fei; Li, Li; Cui, Yu-Ming; Xu, Li-Wen; Chemical Communications  (2019) –; doi:10.1039/C9CC07738C

data_7124433
_publ_section_title
;
 Catalytic Asymmetric Cycloaddition with Unsymmetrical EWG-activated
 Alkenes to Fully Substituted Pyrrolidines Bearing Three Different
 Carbonyl Groups
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07738C
_journal_year                    2019
_chemical_formula_sum            'C21 H20 Br I N O5'
_chemical_formula_weight         573.18
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-05-08 deposited with the CCDC.	2019-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9203(13)
_cell_length_b                   18.197(4)
_cell_length_c                   19.707(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2123.1(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15740
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    3.423
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1124
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.023(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         4836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                4190
_reflns_number_total             4836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc07738c2.cif
_cod_data_source_block           123
_cod_database_code               7124433