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The nucleophilic acylation of pentacarbonyliron by in situ generated pivaloylliiium at low temperature affords an acylferrate complex. The structure of the [(Ph3P),N]+ salt is determined by X-ray analysis. The acylferrate reacts with electrophlles to give thermolabile products which are characterized as tetracarbonyl acylcarbene complexes by IR spectroscopy.The tandem addition of a nucleophile and an electrophile across the C-0 bond of metal carbonyls represents the most versatile access to transition-metal carbene complexes.2 In general, organolithium reagents are used as (1) Reactions of Complex Ligands, Part 28. For part 27, see: Dotz, K. H.; Sturm, W. J . Organomet. Chem., in press. ( 2 ) Recent review: Dotz, K. H.; Fischer, H.; Hofmann, P.; Kreissl, F.

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