The dimeric η6-hexamethylbenzene ruthenium(II) triazole compounds of formulation [{(η6-C6Me6)Ru(N3C2(CO2R)2)}2(μC2O4)] have been synthesized by 1,3-diploar cycloadditions of coordinated azido compound [{(η6-C6Me6)Ru(L1)N3}] (1) with substituted acetylene, RO2CC2CO2Rvia unexpected oxidation of the coordinated ligand to oxalate (where; L1 = 5-hydroxy-2-(hydroxymethyl)-4-pyrone; R = Me, 3 or Et, 4). In contrast, a similar 1,3-dipolar cycloaddition reaction of [{(η6-C6Me6)Ru(L2)N3}] (2) (where; L2 = tropolone) with acetylene yielded the monomeric triazole compound [(η6-C6Me6)Ru(L2){N3C2(CO2R)2}] (where; R = Me, 5; Et, 6). The compounds were characterized by spectroscopy and the structures of representative compounds 4 and 6 have been determined by single crystal X-ray diffraction. The two ruthenium centres in the compound 4, are linked by a tetra-dentate oxalate group. Both compounds, 4 and 6, crystallized in a triclinic space group P-1.
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