Parallel kinetic resolution of acyclic γ-amino-α,β-unsaturated esters: application to the asymmetric synthesis of 4-aminopyrrolidin-2-ones.
Davies, Stephen G.; Lee, James A.; Roberts, Paul M.; Thomson, James E.; Yin, Jingda; Organic letters 14 (2012) 218–221; doi:10.1021/ol203011u

data_1503520
_publ_section_title
;
 Parallel kinetic resolution of acyclic \g-amino-\a,\b-unsaturated esters:
 application to the asymmetric synthesis of 4-aminopyrrolidin-2-ones.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              218
_journal_page_last               221
_journal_paper_doi               10.1021/ol203011u
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C8 H16 N2 O2'
_chemical_formula_sum            'C8 H16 N2 O2'
_chemical_formula_weight         172.23
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
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_cell_length_a                   13.5392(6)
_cell_length_b                   6.7124(4)
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_cell_measurement_temperature    150
_cell_measurement_theta_max      76
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_cell_volume                     1860.27(17)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
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_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
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_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
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_diffrn_radiation_monochromator  graphite
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
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_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
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_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 5.80P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1994
_refine_ls_wR_factor_gt          0.1944
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_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                1574
_reflns_number_total             1911
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.15
_oxford_diffrn_Wilson_scale      0.01
_oxford_refine_ls_r_factor_ref   0.0708
_oxford_refine_ls_scale          8.3(6)
_oxford_reflns_number_all        1911
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            ol203011u_si_002.cif
_cod_data_source_block           70
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P b c a '
_cod_database_code               1503520
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE O   (   1,X'S) H   (  11,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) H   (  22,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE N   (   4,X'S) H   (  41,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE N   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) H   ( 113,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) H   ( 123,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;