Asymmetric synthesis of 3,4-anti- and 3,4-syn-substituted aminopyrrolidines via lithium amide conjugate addition.
Davies, Stephen G.; Garner, A. Christopher; Goddard, Euan C.; Kruchinin, Dennis; Roberts, Paul M.; Smith, Andrew D.; Rodriguez-Solla, Humberto; Thomson, James E.; Toms, Steven M.; Organic & biomolecular chemistry 5 (2007) 1961–1969; doi:10.1039/b704932c

data_7151128
_publ_section_title
;
 Asymmetric synthesis of 3,4-anti- and 3,4-syn-substituted
 aminopyrrolidines via lithium amide conjugate addition.
;
_journal_issue                   12
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1961
_journal_page_last               1969
_journal_paper_doi               10.1039/b704932c
_journal_volume                  5
_journal_year                    2007
_chemical_absolute_configuration unk
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C26 H28 N2 O1 '
_chemical_formula_sum            'C26 H28 N2 O'
_chemical_formula_weight         384.52
_chemical_melting_point          ?
_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
_audit_creation_date             05-05-01
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 98.2945(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5595(2)
_cell_length_b                   17.1047(5)
_cell_length_c                   13.6097(3)
_cell_measurement_reflns_used    4221
_cell_measurement_temperature    190
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2202.08(9)
_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 0.985
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type
;
Enraf Nonius Kappa CCD
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_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8467
_diffrn_reflns_theta_full        24.393
_diffrn_reflns_theta_max         27.485
_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    0.071
_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    1.160
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_exptl_crystal_description       ' block '
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_refine_diff_density_max         0.18
_refine_diff_density_min         -0.16
_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         4299
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.000191
_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

1.43 0.829 1.03
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0748
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0580
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4299
_reflns_number_total             5060
_reflns_threshold_expression     I>1.50u(I)
_cod_data_source_file            b704932c.txt
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        ' C26 H28 N2 O1 '
_cod_database_code               7151128