PPh<sub>3</sub> Mediated Reductive Annulation Reaction between Isatins and Electron Deficient Dienes to Construct Spirooxindole Compounds.
Zhang, Lei; Lu, Hong; Xu, Guo-Qiang; Wang, Zhu-Yin; Xu, Peng-Fei; The Journal of organic chemistry 82 (2017) 5782–5789; doi:10.1021/acs.joc.7b00595

data_4037491
_publ_section_title
;
 PPh<sub>3</sub> Mediated Reductive Annulation Reaction between Isatins
 and Electron Deficient Dienes to Construct Spirooxindole Compounds.
;
_journal_issue                   11
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5782
_journal_page_last               5789
_journal_paper_doi               10.1021/acs.joc.7b00595
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C30 H22 Br N3 O5 S'
_chemical_formula_sum            'C30 H22 Br N3 O5 S'
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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)
(compiled Mar 27 2014,17:12:48)
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_computing_data_collection
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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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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
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;
  1 omega  -14.00   79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega   40.00  145.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
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  3 omega   53.00   79.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -150.0000 26

  4 omega   47.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
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  5 omega   65.00  123.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   44.00   69.00   1.0000    1.0000
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  7 omega   51.00   81.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
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  8 omega   44.00   92.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
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  9 omega   40.00   91.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
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 10 omega   73.00  123.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  120.0000 50

 11 omega   98.00  170.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  120.0000 72

 12 omega   58.00  126.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
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 13 omega  -18.00   40.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 14 omega  -47.00   -5.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 15 omega   36.00   88.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
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 16 omega  -14.00   61.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000   60.0000 75
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_diffrn_orient_matrix_UB_31      -0.1844070000
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_diffrn_orient_matrix_UB_33      -0.0083203000
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.996
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_diffrn_reflns_limit_h_max       5
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_diffrn_source                   'sealed X-ray tube'
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
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Empirical absorption correction using spherical harmonics,
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_exptl_crystal_colour            'clear light yellow'
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+16.2334P] where P=(Fo^2^+2Fc^2^)/3'
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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:
 C9(H9A,H9B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C16(H16), C17(H17), C19(H19), C20(H20),
 C25(H25), C26(H26), C28(H28), C29(H29)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C30(H30A,H30B,H30C)
;
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_olex2_submission_special_instructions 'No special instructions were received'