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Title: Conversion of nitriles to nitrenes via azavinylidenes in low-valent tungsten carbonyl complexes

Journal Article · · Journal of the American Chemical Society; (United States)
DOI:https://doi.org/10.1021/ja00098a022· OSTI ID:6840930
; ;  [1]
  1. Univ. of North Carolina, Chapel Hill, NC (United States)

Azavinylidene complexes of the type Tp[prime](CO)[sub 2]W=N=CRNu are available from the reaction of [Tp[prime](CO)[sub 3]W(N=CR)][BF[sub 4]] with nucleophiles (Tp[prime] = hydridotris(3,5-dimethylpyrazolyl)borate; R = Me, Nu = H (1a); R = Ph, Nu = Et (1d); R = Me, Nu = MeO (1e)). Related azavinylidene complexes Tp[prime](CO)[sub 2]W=N=CHR (R = Me (1a); R = Et (1b); R = CH[sub 2]Ph (1c)) form via insertion of nitrile into the W-H bond of Tp[prime](CO)[sub 3]WH when the metal reagent is photolyzed in the presence of nitriles. Donation of the lone pair of electrons from the azavinylidene nitrogen to the tungsten center, compatible with electron counting guidelines, is reflected in the low IR stretching frequencies of the carbonyl ligands and their downfield carbon resonance in [sup 15]C NMR. NMR spectra and an X-ray structure of Tp[prime](CO)[sub 2]W=N=CHCH[sub 3]Ph (1c) indicate that the azavinylidene ligand is nearly linear ([sup 3]J[sub WH] = 5.6 Hz, [sup 2]J[sub WC] = 27 Hz, and [alpha](W-N-C) = 166.6(7)[degree]). Complex 1c crystallized in the monoclinic space group P2[sub 1]/n with unit cell dimensions of a = 12.163(1), b = 17.207(2), and c = 13.312(1) [angstrom] and [beta] = 102.103(7)[degree], with Z = 4. 32 refs., 2 figs., 5 tabs.

OSTI ID:
6840930
Journal Information:
Journal of the American Chemical Society; (United States), Vol. 116:19; ISSN 0002-7863
Country of Publication:
United States
Language:
English