Treatment of [Cp*Mo(SBu
t)
3] (
1; Cp* =
5-C
5Me
5) with [Fc][PF
6] (Fc = ferrocene) afforded thecationic sulfido-bridged dinuclear complex [(Cp*MoS)(
2-S)
2(Cp*Mo)(S
2Bu
t)][PF
6] (
2) and the cationic incomplete cubane-type complex [(Cp*Mo)
3(
2-S)
3(
3-S)][PF
6](
3) in a ratio of ca. 1:4. The dinuclear complex
2 reactedwith [NiCl
2(PPh
3)
2] and [Ni(cod)
2] (cod = 1,5-cyclooctadiene) to give the heterobimetallic cluster [(Cp*Mo)
2{Ni(PPh
3)}
2(
2-S)
2(
3-S)
3][PF
6] (
4) with an unprecedentedMo
2Ni
2S
5 core and the edge-linked quadruple cubane-type cluster [(Cp*Mo)
2Ni
2(
3-S)
2(
4-S)
2]
4[PF
6]
4 (
5) withfour Mo
2Ni
2S
4 cores, respectively. On the other hand, theincomplete cubane-type cluster
3 serves as a good precursor to the heterobimetallic cubane-type clusters [(Cp*Mo)
3(
3-S)
4M'L][PF
6] (M' = Ru, Ni, and Pd).