Abstract
A new, more convenient route to the benzene cluster [Ru3(CO)9(µ3-η2:η2:η2-C6H6)] directly from [Ru3(CO)12] has been established. Triruthenium dodecacarbonyl, [Ru3(CO)12], undergoes reaction with Me3NO–CH2Cl2 in the presence of cyclohexa-1,3-diene to give the clusters [Ru3H(CO)9(C6H7)] and [Ru3(CO)9(µ3-η2:η2:η2-C6H6)] in moderate yield. Triosmium dodecacarbonyl does not react similarly, but from the reaction of [Os3(CO)10(MeCN)2] with cyclohexa-1,3-diene a key intermediate compound [Os3(CO)10(η4-C6H8)] has been isolated and the solid-state structure of its acetonitrile solvate established by single crystal X-ray diffraction analysis at 150 K. The structure is monoclinic, space group P21/n, with a= 8.932(8), b= 17.387(13), c= 14.833(15)A, β= 105.69(6)° and Z= 4. The three osmium atoms form a regular triangle with a mean Os–Os distance of 2.877(12)A. Two osmium atoms, Os(1) and Os(2), are co-ordinated to four carbonyl ligands and one, Os(3), co-ordinates to two carbonyl ligands. All carbonyl ligands are terminal and approximately linear. The cyclohexadiene ligand is η4 co-ordinated to Os(3)via the 1,3-diene moiety, donating four electrons in total. On thermolysis, this compound is converted to [Os3H(CO)9(C6H7)] and then eventually to [Os3(CO)9(µ3-η2:η2:η2-C6H6)] by established means.
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