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The rearrangement of alkyne by its 1,2-substituent shift mediated by transition-metal complexes is known to afford its tautomeric vinylidene complexes.1 1,2-H, SiMe3and acylmigration of alkyne converting to bridging vinylidene complexes have been well established in dinuclear Ru complexes, such as [(h–Cp)2Ru2(CO)2(m–CO)(m–C=CH2)]2 and [(h–Cp)(h–Cp*)Ru2(CO)2(m–CO){m–C=C(COOCH3)2)}], which have been prepared by methodical syntheses: the initial alkyne exchange reaction of diruthenacyclopetenone structure by ethyne or dimethylacetylenedicarboxylate, followed by 1,2–H and acyl-shift via their intra-molecular C–H or C–C bond cleavages. Recently, by using a sequence of the 13C-labelling alkyne, its transformation to vinylidene-mononuclear ruthenium complexes is reported, suggesting that the acyl group exhibits the migratory aptitude.4 There are still only a few reports concerning the bridging vinylidene complexes of dinuclear iron. In our recent studies for introducing alkyne into trans-[(h–Cp)2Fe2(CO)4], a vinylidenediiron complex of dimethylacetylenedicarboxylate (dmad), cis-[(h–Cp)2Fe2(m–CO)(CO)2{m–C=C(COOCH3)2}], was newly prepared, although only in 8% yield. This title complex is given by a 1,2-acyl shift of dimethylacetylenedicarboxylate through an intramolecular C–C bond cleavage reaction, while the reaction is also accompanied by the cyclotrimerization of X-ray Structure Analysis Online

x-ray structure analysis online

Crystal Structure of a Vinylidene Iron Complex, &lt;i&gt;Cis&lt;/i&gt;-[(&lt;i&gt;η&lt;/i&gt;-Cp)&lt;sub&gt;2&lt;/sub&gt;Fe&lt;sub&gt;2&lt;/sub&gt;(&lt;i&gt;μ&lt;/i&gt;-CO)(CO)&lt;sub&gt;2&lt;/sub&gt;-{&lt;i&gt;μ&lt;/i&gt;-C=C(COOCH&lt;sub&gt;3&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;}], Formed by 1,2-Acyl Shift of Dimethylacetylenedicarboxylate