Lithium amide conjugate addition for the asymmetric synthesis of 3-aminopyrrolidines
Davies, Stephen G.; Garner, A. Christopher; Goddard, Euan C.; Kruchinin, Dennis; Roberts, Paul M.; Rodriguez-Solla, Humberto; Smith, Andrew D.; Chemical Communications (Cambridge, United Kingdom)  (2006) 2664–2666; doi:10.1039/b604835h

data_7101241
_publ_section_title
;
 Lithium amide conjugate addition for the asymmetric synthesis of
 3-aminopyrrolidines
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   25
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2664
_journal_page_last               2666
_journal_paper_doi               10.1039/b604835h
_journal_year                    2006
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C33 H34 N2 O1'
_chemical_formula_sum            'C33 H34 N2 O'
_chemical_formula_weight         474.65
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             03-28-04
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 100.0736(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1297(3)
_cell_length_b                   8.2098(2)
_cell_length_c                   19.4751(4)
_cell_measurement_reflns_used    2964
_cell_measurement_temperature    190
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2696.6(1)
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      190
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
;
Enraf Nonius Kappa CCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.01
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5704
_diffrn_reflns_theta_full        27.218
_diffrn_reflns_theta_max         27.424
_diffrn_reflns_theta_min         5.129
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1016.000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.14
_refine_diff_density_min         -0.12
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1889
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         2894
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.000475
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2

1.12 -0.692E-01 0.612
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0350
_refine_ls_wR_factor_gt          0.0325
_refine_ls_wR_factor_ref         0.0325
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                2894
_reflns_number_total             3244
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b604835h.txt
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C33 H34 N2 O1'
_cod_database_code               7101241