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DOI: 10.1039/A808240E (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1999, 607-614

Synthesis and structural characterization of ruthenium carbonyl clusters containing acetylenic fluorene moieties derived from 9-ethynylfluoren-9-ol

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Cindy Sze-Wai Lau and Wing-Tak Wong

Abstract

Five new ruthenium fluorene clusters, [Ru3(CO)9(µ-H){µ3-η1∶η2∶η2-CC(C13H9)}] 1 (8%), [Ru3(CO)7(µ-CO){µ3-η1∶η2∶η4-(HOC13H8)CCHC(C13H8OH)CH}] 2 (15%), [Ru4(CO)10(µ-CO)(µ3-OH)(µ3-η1∶η2∶η2-C13H8CCH)] 3 (12%), [Ru5(CO)11(µ-H)(µ-CO)(µ3-OH)(µ5-η1∶η1∶η2∶η2∶η6-C13H7CHC)] 4 (10%) and [Ru6(CO)15(µ5-η1∶η1∶η2∶η3∶η6-C13H7CHC)] 5 (9%), have been synthesized by a reaction of 9-ethynylfluoren-9-ol with triruthenium dodecacarbonyl in tetrahydrofuran under reflux. All these compounds have been fully characterized by spectroscopic and X-ray diffraction methods. The structure of 1 consists of a fluorene ring bound to the triruthenium cluster unit via a typical µ3-(η2-⊥) co-ordination mode. Cluster 2 is based on a Ru3 triangle containing a C4 chain which arises from the coupling of two ligand molecules with the formation of a metallacyclopentadiene ring. An interesting structural feature observed in cluster 3 is the formation of a Ru4O square pyramidal framework in which the hydroxy group, originating from the ligand, is bound to the cluster in a triply bridging manner. The bonding modes of the organic fragments in 4 and 5 are very similar. They both interact with five ruthenium metal centres but with a novel Ru5 bent chain in 4 and a spiked butterfly in 5.

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