Incorporation of Fe into the void corner of the incomplete cubane-type Ir3S(SH)3 sulfido-hydrosulfido cluster to give new cubane-type Ir3FeS4 clusters

Treatment of incomplete cubane-type cluster [(Cp*Ir)3(μ3-S)(μ2-SH)3]Cl (1; Cp* = η5-C5Me5) with FeCl2 in the presence of excess NEt3 afforded a cationic cubane-type cluster [(Cp*Ir)3(FeCl)(μ3-S)4][FeCl2(μ-Cl)2FeCl2]0.5 (4), although isolation of 4 as pure crystals was somehow unable to be reproduced. On the other hand, reaction of 1 with FeCl3 or Fe(BF4)2·6H2O in the presence of excess NEt3 has proved to result in the formation of a neutral cluster [(Cp*Ir)3(FeCl)(μ3-S)4] (5) in moderate yield. Cluster 5 was allowed to react with small amount of O2 gas to give μ3-SO2 cluster [(Cp*Ir)3(FeCl)(μ3-SO2)(μ3-S)3] (6). New clusters 4, 5, and 6 were characterized by the single crystal X-ray diffraction.