The synthesis of [{n-Bu2Sn(S2N2)}2] and its use in the preparation of organometallic iridium sulfur nitrogen complexes

Abstract

The addition of [n-Bu2SnCl2] to a solution of [S4N3][Cl] in liquid ammonia gave after extraction of the dry reaction mixture the new tin disulfur dinitrido compound [{n-Bu2Sn(S2N2)}2] (1). Reaction of [{n-Bu2Sn(S2N2)}2] (1) with the pentamethylcyclopentadienyl (Cp*) iridium derivatives [{IrCl(µ-Cl)(η5-C5Me5)}2] or [(η5-C5Me5)IrCl2(PPh3)] gave different products, which were dependent on the reactant ratios. A 1:1 reaction between 1 and [{IrCl(µ-Cl)(η5-C5Me5)}2] gave only [(η5-C5Me5)Ir(S2N2)] (2) in moderate yield; the same product in higher yield was obtained from a 2:1 reaction between 1 and [(η5-C5Me5)IrCl2(PPh3)]. Reaction of 1 and [(η5-C5Me5)2IrCl2(PPh3)] (1:1 molar ratio) in the presence of NH4[PF6] gave the unusual bimetallic species [(η5-C5Me5)IrCl(PPh3)(S2N2)Ir(η5-C5Me5)][PF6] (3). The X-ray crystal structures of 1, 2, and 3 are reported.Key words: liquid ammonia, tin sulfur–nitrogen reagent, metathesis, sulfur–nitrogen metallacycle, iridium complexes.