The parent 30-electron triple-decker iron complex with cyclopentadienyl [igands, [(q-CsHs)Fe(ta-rI:q-Cst|5)Fe(q-CsHs)]PF 6 (i), was prepared for the first time by visiblelight irradiation of ferroccnc and [(ri-CsHs)Fe(q-C6H6)IPF 6 in CH2CI 2 at 0 ~ An analogous reaction performed with the use of (rI-CsHs)Co(q-C4Me 4) (2) instead of ferrocene afforded the thermally labile 30-electron cationic iron-cobalt triple-decker complex [(q-CsIts)Fe(~-q:q-CsHs)Co(q-C4Me4)}PF 6. The latter reacted with compotmd 2 at 20 ~ to form the symmetrical 30-electron cationic dicobalt triple-decker complex [(q-C4Me4)Co(~tq:q-C5Hs)Co(q-C4Me4)] PF6.
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