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259ChemInform Abstract The title complexes (III) can be prepared using slightly different methods. On the basis of 1H NMR, IR, and electronic spectroscopy data, the presence of a single metal-metal covalent bond is suggested. This assumption is confirmed by an X-ray diffraction study of (IIIa) (space group P1, Z=2). The electrochemical behavior of (III) is investigated by cyclic voltammetry using the examples of (IIIa)-(IIIc), and (IIIe). In all cases the addition or abstraction of one electron to or from the bimetallic compound leads to a porphyrin anion or cation whose lifetime is short and varies with the axial ligand. Electroreduction seems to involve the porphyrin π ring system but participation of a σ metal-based orbital cannot be ruled out. In contrast to the octaethylporphyrinato complexes the tetraphenylporphyrinato derivatives are reduced in two one-electron transfer steps.