Synthesis of (phosphine)silver(I) trifluoromethanesulfonate complexes and the molecular structure of di-μ-trifluoromethylsulfonate-(tetrakis-triphenylphosphine)disilver(I)
摘要:
Reactions of silver trifluoromethanesulfonate (triflate) and equimolar amounts of triphenylphosphine, 1,2- bis(diphenylphosphino)ethane. bis(diphenylphosphino)methane, or 1,1 -bis(diphenylphosphino)ethane in either DME or CH2Cl2 solution produced the corresponding 1:1 complexes [(L)Ag(I)(SO3CF3)] (2-5) in > 80% yields. A related 2:1 complex [(Ph3P)(2)Ag(I)(SO3CF3)] (1) was also obtained using 2 equiv. of Ph3Ph. Both P-31 NMR variable temperature solution spectra as well as solid state spectra were recorded for the new complexes, and were generally helpful in structural assignments. An X-ray crystallographic study of 1 shows this to be a dimeric complex with bridging triflate ions; the silver atoms having distorted tetrahedral coordination. (C) 2000 Elsevier Science S.A. All rights reserved.