The reaction of pentacarbonyl(cyc1ooctatetraene)diiron (1) with aryllithium reagents, ArLi (Ar = C6H6, 0-, m-, andp-CH~C6H4, p-C1C,&, p-CF3C6H4), in ether at low temperature afforded acylmetalate intermediates. Subsequent alkylation with Et30BF4 in aqueous solution a t 0 "C gave the six new dimetal bridging carbene complexes CsHs(CO)zFe(cl-C(oczHs)Ar)Fe(CO)z (2, Ar = C&; 3, Ar = o -C H~C~H~; 4, Ar = m-CH3C6H4; 5, Ar = p-CH3CeH4; 6, Ar = p-ClC,&; 7, Ar = p-CF,C&4); the structure of 7 has been established by X-ray diffraction analysis. Complex 7 crystallized in the monoclinic system, space group P21/n, with a = 8.766(2) A, b = 23.404(5) A, c = 10.270(2) A, j 3 = 94.25(2)', V = 2101.27(7) A3, Z = 4, Ddcd = 1.68 g/cm3, R = 0.0347, and R, = 0.0330 for 2496 reflections with Fo2 > 3a(FO2).