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Issue title: In Honor of Alan H. Cowley
Article type: Research Article
Authors: Agapiou, Kyriacos | Jones, Richard A. | Yang, Xiaoping
Affiliations: e-MAT Technology, Moses Lake, WA, USA | Department of Chemistry and Biochemistry, The University of Texas at Austin, Austin, TX, USA
Note: [] Corresponding author. E-mail: [email protected]
Abstract: Reaction of diethylacetylene dicarboxylate (EtO_{2}CC≡CCO_{2}Et) with trans-(N_{3})_{2}Ru(PMe_{3})_{4} in THF at 25°C gave the bis-triazolato complex (PMe_{3})_{3}Ru[N_{3}C_{2}-(CO_{2}Et)_{2}]_{2} (1) in 41% yield. Reaction of trans-(N_{3})_{2}Ru(PMe_{3})_{4} with phenylacetylene in toluene at 110^{\circ}C gave the mixed azide acetylide complex cis-(PMe_{3})_{4}Ru(N_{3})(C≡CC_{6}H_{5}) (2) (51%. The analogous alkynyl acetylide cis-(PMe_{3})_{4}Ru(N_{3})(C≡CC_{6}H_{4}C≡ CH) (3) is formed from 1,4-diethynylbenzene in 72% yield. Reaction of trans-(N_{3})_{2}Ru(PMe_{3})_{4} with HC≡CSiMe_{3} in CH_{2}Cl_{2} at 41°C gave trans-(PMe_{3})_{4}Ru[C≡ C(SiMe_{3})]_{2} (4) (37%. A similar reaction in toluene at 110°C gave the dinuclear azide [(PMe_{3})_{3}(N_{3})Ru]_{2}(μ_{1,3}- N_{3})_{2} (5) (30% 3,5-bis(trifluoromethyl)pyrazole (PzH) with trans-(N_{3})_{2}Ru(PMe_{3})_{4} in refluxing toluene gave [(PMe_{3})_{3}Ru]_{2}(μ_{1}-N_{3})_{3}][Pz· 2PzH (6). Complexes 1–6 have been characterized spectroscopically as well as by single crystal X-ray diffraction studies.
Keywords: Ruthenium complexes, azide, acetylide, triazolato, X-ray crystal structures
DOI: 10.3233/MGC-2010-0003
Journal: Main Group Chemistry, vol. 9, no. 1-2, pp. 41-56, 2010
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