New organometallic clusters with the MFe2(µ3-S)2 core (M = Mo or Fe) have been synthesized from inorganic [MoFe3S4] or [Fe4S4] clusters under high pressure CO. The reaction of (Cl4-cat)2Mo2Fe6S8(PR3)6
[R = Et, nPr] with high pressure CO produced the crystalline [MoFe2S2]4+ clusters, (Cl4-cat)Mo(O)Fe2S2(CO)n(PR3)6−n
[n
= 4, Et =
I, nPr =
II; n = 5, Et =
III] after flash column chromatography. The similar [MoFe2S2]4+ cluster, (Cl4-cat)2MoFe2S2(CO)2(depe)2
(IV), also has been achieved by the reactions of (Cl4-cat)MoFe3S3(CO)6(PEt3)2 with depe by reductive decoupling of the cluster. For the [Fe3(µ3-S)2]4+ cluster, [Fe4S4(PcHex3)4](BPh4) was reacted with high pressure CO to produce a new Fe3S2(CO)7(PcHex)2
(V) compound. These reactions generalized the preparation of organometallic compounds from inorganic clusters. All the compounds have been characterized by single crystal X-ray crystallography. A possible reaction pathway for the synthesis of the MFe2(µ3-S)2 clusters (M = Mo or Fe) has also been suggested.
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