Abstract

In this paper, the monosubstituted [Fe2(CO)5P(OMe)3{μ‐(edt)}] (2) and the disubstituted [Fe2(CO)4(P(OMe)3)2{μ‐(edt)}] (3) complexes we re‐synthesized by CO substitution using thermal activation method. In contrast, Darchen and co‐workers prepared complexes 2 and 3 by electron transfer catalysis method. The resulting complexes were characterized by different spectroscopic techniques. A detailed electrochemical study of complexes 2 and 3 in the absence and presence of the weak acetic acid, AcOH, was also reported. The structure of complexes 2 and 3 were confirmed by X‐ray diffraction analysis.

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