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dc.titleArene-ruthenium complexes of an acyclic thiolate-thioether and tridentate thioether derivatives resulting from ring-closure reactions
dc.contributor.authorShin, R.Y.C.
dc.contributor.authorBennett, M.A.
dc.contributor.authorYoong Goh, L.
dc.contributor.authorChen, W.
dc.contributor.authorHockless, D.C.R.
dc.contributor.authorLeong, W.K.
dc.contributor.authorMashima, K.
dc.contributor.authorWillis, A.C.
dc.identifier.citationShin, R.Y.C., Bennett, M.A., Yoong Goh, L., Chen, W., Hockless, D.C.R., Leong, W.K., Mashima, K., Willis, A.C. (2003-01). Arene-ruthenium complexes of an acyclic thiolate-thioether and tridentate thioether derivatives resulting from ring-closure reactions. Inorganic Chemistry 42 (1) : 96-106. ScholarBank@NUS Repository.
dc.description.abstractThe reaction of [(η6-arene)RuCl2]2 (arene = C6Me6, 1,4-MeC6H4CHMe2) with a large excess of the dianion of bis(2-mercaptoethyl) sulfide, (HSCH2CH2)2S, obtained from deprotonation of the dithiol with freshly prepared NaOMe, gives the deep red, monomeric complexes [(η6-arene)Flu(η3-C4 H8S3)] (arene = C6Me6 (5), 1,4-MeC6H4CHMe2 (6)) in which the dianion is bound to the metal atom through one thioether and two thiolate sulfur atoms. Complex 5 reacts with [(η6-C6Me6)RuCl2]2 (4) in a 2:1 mole ratio to give a quantitative yield of the chloride salt of a binuclear cation [{(η6-C6Me6)Ru}2 Cl(μ2-η2:η3 -C4H8S3)]+ (7) in which the thiolate sulfur atoms of the [(η6-C6Me6)Ru(η3 -C4H8S3)] group bridge to a (η6-C6Me6)RuCl unit. This compound is also obtained directly from the reaction of 4 with the dithiolate, if the Ru dimer is used in large excess. The binuclear complex [{(η6-C6Me6)Ru}2(MeCN) (μ2-η2:η3C4 H8S3)](PF6)2·MeCN, (9)(PF6)2·MeCN, is obtained by treatment of (7)Cl with NH4PF6 in acetonitrile. Protonation of 5 with HCl gave the mono- and diprotonated derivatives viz. [(η6-C6Me6)Ru(η3 -C4H9S3)]Cl, (8)Cl, and [(η6-C6Me6)Ru(η3 -C4H10S3)]Cl2, (10)Cl2, respectively. The reaction of 5 with methyl iodide gives both the mono- and di-S-methylated derivatives. Treatment of 5 with dibromoalkanes, Br(CH2)nBr (n = 1-5), effects ring closure to give the (η6-C6Me6)Ru dications containing the trithia mesocyclic zS3 (z = 8-12) ligands, isolated as their PF6 salts. The X-ray crystal structures of 5, 6, the solvates of (7)Cl and (9)(PF6)2, and the trithia mesocyclic Ru complexes (η6-C6Me6)Ru(zS3) (PF6)2 (z = 8-11) are reported.
dc.description.sourcetitleInorganic Chemistry
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