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DOI: 10.1039/A805368E (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1998, 3391-3396

Synthesis and structural characterisation of ruthenium carbonyl clusters containing hydrocarbyl ligands derived from (hydroxy)alkynes HC[triple bond, length half m-dash]CC(H)(OH)CH3

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Cindy Sze-Wai Lau and Wing-Tak Wong

Abstract

Five new ruthenium ketonic clusters [Ru4(CO)12{µ4-η1∶η1∶η2∶η2-CH3C(H)CCC(H)CH2C(O)CH3}] 1 (10%), [Ru5(CO)14(µ-H)2{µ4-η1∶η1∶η2∶η2-CC(H)C(O)CH3}] 2 (15%), [Ru6(CO)16{µ4-η1∶η1∶η2∶η2-CC(H)C(O)CH3}2] 3 (15%), [Ru7(CO)19{µ4-η1∶η1∶η2∶η2-CC(H)C(O)CH3}{µ5-η1∶η1∶η1∶η1∶η2-CCC(H)CH3}] 4 (8%), and [Ru5(CO)12(µ-CO){µ4-η1∶η1∶η2∶η2-CC(H)C(O)CH3}(µ4-η2-HCCCH2CH3)] 5 (10%) have been synthesised by reaction of but-3-yn-2-ol with triruthenium dodecacarbonyl, in cyclohexane, under reflux. All the compounds have been fully characterised by spectroscopic and X-ray diffraction methods. The structure of 1 is based on a Ru4 butterfly skeleton containing a fragment of C8 ketonic chain which arises from the coupling of two ligand molecules with the elimination of a water molecule. An interesting feature in clusters 2, 3, 4 and 5 is the formation of a metallocycloketonic ring with a µ4-η1∶η1∶η2∶η2 coordination mode which is derived from the activation of the C[triple bond, length half m-dash]C triple bond. Both 2 and 5 consist of a wingtip bridged butterfly core, which is also bonded with two bridged hydrides in 2 and a µ4-η2 acetylide fragment in 5 respectively. Cluster 2 is also closely related to cluster 3, in that it seems to be a monomeric unit of 3 forming a six atom raft geometry with two metallocycloketonic rings. The metal core of 4 is similar to 3, except that one Ru–Ru bond in 4 is broken to form two more metal–metal bonds with an additional Ru atom to give a novel Ru7 core, which is best described as a distorted Ru4 square plane sharing an edge with an edge-bridged butterfly. Moreover, one of the metallocycloketonic rings in 3 is replaced by an allenyl CCC(H)CH3 ligand, which is coordinated to an edge-bridged butterfly in 4.

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