1,3,5-Triphosphabicyclo[3.1.0]hexene-η31-diyl Hafnium Complexes: Structure and Reactivity

Autor: Binger, Paul, Stutzmann, Stefanie, Stannek, Jörg, Günther, Klaus, Phillips, Petra, Mynott, Richard, Bruckmann, Joachim, Krüger, Carl
Zdroj: European Journal of Inorganic Chemistry; May 1999, Vol. 1999 Issue: 5 p763-769, 7p
Abstrakt: It is shown that the (P≡C–tBu)3 ligand found in the hafnium complex (COT)Hf(P≡C–tBu)35 (COT = cyclooctatetraene), which we reported recently,[3] is also present in the new hafnium complex 12, prepared by reaction of hexachloroethane with complex 5 in pentane, as well as in its trimethylphosphane adduct 14. The structures of complexes 12 and 14 have been determined by X-ray crystallography and that of 5 by comparing its 1H-, 13C-, and 31P-NMR spectra with those of the complexes 12 and 14. The organophosphorus ligand in all three complexes is a 2,4,6-tri-tert-butyl-1,3,5-triphosphabicyclo[3.1.0]hexene-η31-diyl. Hydrolysis of complexes 5 and 12 with water gives the new phosphorus heterocycle 15, whereas the new heterocycles 16 and 17 are formed in an approximately 1:1 mixture using either silica gel containing 2% H2O or Na2SO4 · 10 H2O.
Databáze: Supplemental Index