One-pot synthesis of sulphur-bridged rhenium containing molecular cubanes: Spectroscopic and structural characterisation

• Neutral rhenium(I) molecular cubanes were obtained in one-pot reaction.
• Molecular cubanes were synthesised by oxidative addition of diaryl disulphide to rhenium carbonyl.
• Dimethyl formamide was used as a catalyst to synthesis rhenium(I) molecular cubanes.
• Structural studies revealed distorted cubic structure of Re4S4 core.

Sulphur-bridged rhenium(I) based molecular cubanes [Re4(CO)12(μ3-SR)4] (1, R = C4H9; 2, R = C6H5; 3, R = C6H4CH3; 4, R = CH2C6H5) have been synthesised in one-pot reaction via oxidative addition of dialkyl/diaryl disulphide, RSSR to low valent transition metal carbonyl, Re2(CO)10 with catalytic amount of dimethyl formamide. The molecular cubanes 1–4 have been characterised by elemental analysis, NMR, IR and UV–Vis absorption spectroscopic techniques. The molecular structures of 2 and 4 were determined by single crystal X-ray diffraction analysis and the structural studies ascertain the presence of Re4S4 distorted cube. The synthetic strategy offers a simple route for preparation of the class of sulphur-bridged Re(I) based molecular cubanes.

Rhenium(I) based sulphur-bridged molecular cubanes were obtained in one-pot reaction via oxidative addition of diaryl disulphide to rhenium carbonyl with dimethyl formamide as catalyst.Figure optionsDownload as PowerPoint slide