The invention relates to a method for the prodn. of salts of weakly fluorinated alcoholato complex anions according to the following formulas, M[FX(ORF)m]z (1) M[(FRO)mXFX(ORF)m]z (2) and M[(FRO)mXFX(ORF)nFX(ORF)m]z (3) (X = B, Al, Ga, In, P, As, Sb; M = monovalent or divalent cation; n = 2 for m = 3 or n = 4 for m = 5; y = 1-2). For example, Ag[FAl(OC(CF3)3)3] in 98 % yield was prepd. by the reaction of AlMe3 with HOC(CF3)3 in presence of AgBF4 in pentane. [on SciFinder (R)]