15602-40-1Relevant articles and documents
A facile atmospheric pressure synthesis of the hexacarbonylmetalate ions, M(CO)6-, of niobium and tantalum
Dewey, Christopher G.,Ellis, John E.,Fjare, Kristi L.,Pfahl, Kathryn M.,Warnock, Garry F. P.
, p. 388 - 391 (2008/10/08)
Treatment of the pentachlorides of niobium and tantalum with 6 equiv of alkali-metal naphthalenide or 1-methylnaphthalenide in DME at -60 to -80°C provides thermally unstable red-brown intermediates that may be M(C10H8)2- or M(1-MeC10H7)2- (M = Nb, Ta). These species readily react with CO at atmospheric pressure at -60°C to provide 30-54% yields of the corresponding M(CO)6-, isolated as Et4N+, n-Bu4N+, and Na(diglyme)2+ salts. This two-step reductive carbonylation procedure is the first reported atmospheric pressure synthesis of the hexacarbonylmetalate(1-) ions of niobium and tantalum. The synthesis and properties of unsolvated NaTa(CO)6 are also described.