Five-membered sulfur-nitrogen ring compounds
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A series of 1,3,2,4,5-dithiadiazarsoles with the general formula RAs(S₂N₂) (R = Me, Et, i-Pr, t-Bu, Ph and Mes) have been prepared and characterised by multinuclear NMR, IR and Raman spectroscopies and mass spectrometry. The X-ray structures of PhAs(S₂N₂) and MesAs(S₂N₂) were determined. The low temperature X-ray structures of the half-sandwich 5,1,3,2,4-metalladithiadiazoles Cp*M(S₂N₂) (M = Co, Ir) were determined and Cp*Rh(S₂N₂) was prepared. All three metalladithiadiazoles were characterised by multinuclear NMR, IR and Raman spectroscopies and mass spectrometry. The X-ray structures of complexes [Cp*RhCp*]Cl,[Cp*Rh(μ-S₃N₂)(μ-S₂O₃)RhCp*] and Cp*Ir[S₂N₂(IrCl₂Cp*)] obtained during this work were determined. The low temperature X-ray structure of Roesky's sulfoxide (S₃N₂O) is presented together with assignments of its vibrational spectra as suggested by theoretical calculations. The experimental structures of the metalladithiadiazoles and that of Roesky's sulfoxide are compared with calculated geometries. A limited amount of simple experiments have been carried out with selected title compounds to get an insight into their reactivity.
Thesis, PhD Doctor of Philosophy
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