Enantioselective [4 + 1]-Annulation of α,β-Unsaturated Imines with Allylic Carbonates Catalyzed by a Hybrid P-Chiral Phosphine Oxide-Phosphine.
Li, Hanyuan; Luo, Jiesi; Li, Bojuan; Yi, Xizhen; He, Zhengjie; Organic letters 19 (2017) 5637–5640; doi:10.1021/acs.orglett.7b02800

data_1547529
_publ_section_title
;
 Enantioselective [4 + 1]-Annulation of \a,\b-Unsaturated Imines with
 Allylic Carbonates Catalyzed by a Hybrid P-Chiral Phosphine
 Oxide-Phosphine.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              5637
_journal_page_last               5640
_journal_paper_doi               10.1021/acs.orglett.7b02800
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C39 H35 N O2 P2'
_chemical_formula_sum            'C39 H35 N O2 P2'
_chemical_formula_weight         611.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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
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Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
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_cell_angle_alpha                90
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scan:
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               Slice: -120.0000 - 60.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 59.8496
              2theta: -30.1038
scan:
    Number of images: 360
               Slice: -120.0000 - 60.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 59.8496
              2theta: -30.1038
scan:
    Number of images: 360
               Slice: -120.0000 - 60.0000
         Image width: 0.5000
            Exp time: 25.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 59.8496
              2theta: -30.1038
;
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AFC10: Fixed Chi 2 circle
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_diffrn_reflns_limit_l_min       -11
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_exptl_crystal_colour            Colorless
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_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_preparation       Fiber
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_refine_ls_abs_structure_details
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 Flack x determined using 2627 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
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_refine_ls_abs_structure_Flack   -0.04(4)
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'w=1/[\s^2^(Fo^2^)+(0.0525P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1547527--1547529.cif.
;
_cod_database_code               1547529
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C26(H26), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
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_shelx_res_checksum              34559
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