Equimolar amounts of trans-[ReOX2(OEt)(PPh3)2] (XCl, Br, I) precursors and potentially bidentate N,S-donor pyrimidine-2(1H)-thione (pymSH) react in refluxing acetone to give mononuclear octahedral paramagnetic trans-[ReIIIX2(pymS)(PPh3)2](XCl, Br, I) species. Starting from a metal–ligand molar ratio of 1:3, in the presence of N(C2H5)3 as deprotonating agent inrefluxing ethanol, the same reaction proceeds stepwise, affording octahedral [ReO(pymS)3] or [ReO(pymS)3] and pentagonalbipyramidal[Re(pymS)3PPh3] complexes as a function of the reaction time. The compounds were characterized by elementalanalysis, magnetic susceptibility, UV–Vis–NIR, IR and 1H NMR spectroscopy and by cyclovoltammetric measurements.Reaction pathways and physico-chemical properties of the complexes are discussed.
Synthesis, magnetic, spectroscopic and electrochemical studies of mixed pyrimidine-2-thiolate/triphenylphosphine rhenium(V) and rhenium(III) complexes / Battistuzzi, Gianantonio; Cannio, Maria; Battistuzzi, Raffaele. - In: POLYHEDRON. - ISSN 0277-5387. - STAMPA. - 19:20-21(2000), pp. 2163-2170. [10.1016/S0277-5387(00)00517-9]
Synthesis, magnetic, spectroscopic and electrochemical studies of mixed pyrimidine-2-thiolate/triphenylphosphine rhenium(V) and rhenium(III) complexes
BATTISTUZZI, Gianantonio;CANNIO, Maria;BATTISTUZZI, Raffaele
2000
Abstract
Equimolar amounts of trans-[ReOX2(OEt)(PPh3)2] (XCl, Br, I) precursors and potentially bidentate N,S-donor pyrimidine-2(1H)-thione (pymSH) react in refluxing acetone to give mononuclear octahedral paramagnetic trans-[ReIIIX2(pymS)(PPh3)2](XCl, Br, I) species. Starting from a metal–ligand molar ratio of 1:3, in the presence of N(C2H5)3 as deprotonating agent inrefluxing ethanol, the same reaction proceeds stepwise, affording octahedral [ReO(pymS)3] or [ReO(pymS)3] and pentagonalbipyramidal[Re(pymS)3PPh3] complexes as a function of the reaction time. The compounds were characterized by elementalanalysis, magnetic susceptibility, UV–Vis–NIR, IR and 1H NMR spectroscopy and by cyclovoltammetric measurements.Reaction pathways and physico-chemical properties of the complexes are discussed.
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