Ps. Tanner et Tp. Hanusa, ENCAPSULATED ALKALINE-EARTH METALLOCENES .4. THERMAL-INSTABILITY IN TETRAPHENYLCYCLOPENTADIENYL BARIUM COMPLEXES, Polyhedron, 13(15-16), 1994, pp. 2417-2420
Reaction of two equivalents of C(5)Ph(4)H(2) With Ba[N(SiMe(3))(2)](2)
(THF)(2) in THF or toluene-produces the solvated octaphenylbarocene (C
(5)Ph(4)H)(2)Ba(THF) in quantitative yield. The air-sensitive metalloc
ene displays a surprising lack of thermal stability, and decomposes in
the solid state at room temperature over a period of two weeks or upo
n attempted vacuum sublimation at 110-120 degrees C (10(-6) torr). Rea
ction of C(5)Ph(4)H(2) with Ba[N(SiMe(3))(2)](2)(THF)(2) in a 1 : 1 mo
lar ratio in THF or toluene produces a yellow solid that is a mixture
of the metallocene with the mono(ring) compound (C(5)Ph(4)H)BaN(SiMe(3
))(2)(THF)(n). Attempts to synthesize a barocene containing the pentap
benylcyclopentadienyl ligand were not successful.