Abstract

Interaction of Re(NBu t) 3(NHBu t) and CF 3SO 3H in Et 2O leads to the known [Re(NBu t) 3(NH 2Bu t)]O 3SCF 3 but also to a low yield, presumably via a competitive reaction, of a red compound, Re 4(NBu t) 8(μ-O) 2(μ 3-O) 2(OSO 2CF 3) 4, whose X-ray crystal structure has been determined. The structure has a Re 4O 4 core comprising oxo-bridged, five- and six-coordinate rhenium centres. The six-coordinate rhenium centres have cis oriented oxo, NBu t and η 1-O 3SCF 3 ligands; the five-coordinate centres have pairs of NBu t and μ 3-O ligands and a μ-O ligand.

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