Asymmetric [3 + 2] Cycloaddition of Methyleneindolinones with N,N'-Cyclic Azomethine Imines Catalyzed by a N,N'-Dioxide-Mg(OTf)2 Complex.
Yin, Chengkai; Lin, Lili; Zhang, Dong; Feng, Juhua; Liu, Xiaohua; Feng, Xiaoming; The Journal of organic chemistry 80 (2015) 9691–9699; doi:10.1021/acs.joc.5b01760

data_4036368
_publ_section_title
;
 Asymmetric [3 + 2] Cycloaddition of Methyleneindolinones with N,N'-Cyclic
 Azomethine Imines Catalyzed by a N,N'-Dioxide-Mg(OTf)2 Complex.
;
_journal_issue                   19
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              9691
_journal_page_last               9699
_journal_paper_doi               10.1021/acs.joc.5b01760
_journal_volume                  80
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C27 H30 N3 O7'
_chemical_formula_sum            'C27 H30 N3 O7'
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_space_group_name_Hall           'P 2ac 2ab'
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Olex2 1.2
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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  1 omega    9.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega   17.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671   38.0000 -120.0000 88

  4 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671  -77.0000  -90.0000 94

  5 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671 -125.0000   30.0000 67

  6 omega   38.00   91.00   1.0000    2.2400
omega____ theta____ kappa____ phi______ frames
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  7 omega   39.00  177.00   1.0000    2.2400
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  8 omega   38.00   91.00   1.0000    2.2400
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  9 omega   90.00  175.00   1.0000    2.2400
omega____ theta____ kappa____ phi______ frames
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 10 omega   40.00   98.00   1.0000    2.2400
omega____ theta____ kappa____ phi______ frames
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 11 omega   40.00   98.00   1.0000    2.2400
omega____ theta____ kappa____ phi______ frames
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 12 omega   38.00   91.00   1.0000    2.2400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

 13 omega   38.00   91.00   1.0000    2.2400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 53

 14 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671  -77.0000 -150.0000 94

 15 omega    9.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671   77.0000 -120.0000 95

 16 omega  -35.00   -1.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671  -19.0000  -60.0000 34

 17 omega    9.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1671   77.0000  -30.0000 95
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_diffrn_orient_matrix_UB_33      0.0491600000
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'clear light colourless'
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;
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 Flack x determined using 1881 quotients [(I+)-(I-)]/[(I+)+(I-)]
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_refine_ls_abs_structure_Flack   -0.04(9)
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_refine_ls_number_parameters     339
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N8(H8), C14(H14), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C18(H18), C24(H24), C25(H25), C26(H26), C27(H27), C31(H31)
2.d Idealised Me refined as rotating group:
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 H36C), C37(H37A,H37B,H37C)
;
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_olex2_submission_special_instructions 'No special instructions were received'