High nuclearity early transition metal clusters have drawn interest for their potential as biomedical X-ray contrast agents. Two isomers of a hexatungsten oxychloride cluster, (NR4)2[W6O6Cl12], were reported by J. Long In 2001, based on a previously published procedure for reduction of WCl6 with bismuth to yield W6Cl12. The preparation of W6O6X122- (X = Cl, Br) by the reduction of WOX4 with Bi in a sealed borosilicate ampoule at 360° has been extended to W6O6Br122-. The acid salts were easily extracted from the crude reaction mixture with a solution of HX in H2O, MeOH or EtOH, and from there they were converted to the tetraalkylammonium salts. The interconversion between the two isomers was explored, and efforts to monitor this by UV-vis and 17O NMR spectra will be reported. Preliminary results with the Mo analogues will also be discussed.

Synthesis, reactivity and 17O NMR studies of hexatungsten oxyhalide clusters

ACS Spring 2022

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