The tris(trifluoromethyl)methyl phosphonium ion, P(CF(3))(3)CH(3)(+), preparation and structure.
The P(CF(3))(3)CH(3)(+) ion is synthesized as P(CF(3))(3)CH(3)(+)AsF(6)(-) by methylation in a MeF/SO(2)/AsF(5) system or as P(CF(3))(3)CH(3)(+)Sb(2)F(11)(-) in a MeF/HF/SbF(5) system at low temperatures. In contrast to (CF(3))(3)(CH(3))P(+)AsF(6)(-), P(CF(3))(3)CH(3)(+)Sb(2)F(11)(-) is a stable, colorless crystalline solid. A crystal structure determination shows the presence of a slightly distorted tetrahedral phosphonium cation with P-C(F) distances of 188.1-188.7(4) and a P-C(H) bond length of 176.7(4) pm. The phosphonium salt (CF(3))(3)(CH(3))P(+)AsF(6)(-) was also obtained by abstraction of a fluoride ion from the anion [(CF(3))(3)(CH(3))PF(2)](-) salt using AsF(5).
Shyshkov
Oleg
O
Institute of Inorganic & Physical Chemistry, University of Bremen, D-28334 Bremen, Germany.
Dieckbreder
Uwe
U
Drews
Thomas
T
Kolomeitsev
Alexander
A
Röschenthaler
Gerd-Volker
GV
Seppelt
Konrad
K