title: The tris(trifluoromethyl)methyl phosphonium ion, P(CF(3))(3)CH(3)(+), preparation and structure.
abstract: 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).
authors.affiliation: Institute of Inorganic & Physical Chemistry, University of Bremen, D-28334 Bremen, Germany.
authors.forename: Oleg
authors.initials: O
authors.lastname: Shyshkov
authors.forename: Uwe
authors.initials: U
authors.lastname: Dieckbreder
authors.forename: Thomas
authors.initials: T
authors.lastname: Drews
authors.forename: Alexander
authors.initials: A
authors.lastname: Kolomeitsev
authors.forename: Gerd-Volker
authors.initials: GV
authors.lastname: Röschenthaler
authors.forename: Konrad
authors.initials: K
authors.lastname: Seppelt