Short hydrogen bonds: diadducts of substituted pyridine N-oxides: synthesis, spectroscopic studies, and X-ray structure

Abstract
Hydrogen-bonded diadducts of substituted pyridine N-oxides, stabilized by [AuCl4], have been prepared and studied by spectroscopic techniques. The presence of a broad absorption around 800 cm–1 in the i.r. spectra, and the existence of bands characteristic of the ligands and [AuCl4], in the u.v. spectra, indicate a short O H O hydrogen bond. An X-ray diffraction study of one of the diadducts, [H(3Me-pyo)2][AuCl4](3Me-pyo = 3-methylpyridine N-oxide), revealed an O O distance of 2.406(9)Å. The complex crystallizes in the triclinic space group P, with a= 6.857(4), b= 8.011(1), c= 8.797(2)Å, α= 105.05(2), β= 66.89(3), γ= 89.39(2)°, and Z= 1. The structure was refined to R= 0.063 using 2 339 reflections collected on a CAD4 diffractometer. On the basis of Au O contacts, an uncommon distorted octahedral environment for AuIII may be assumed in the solid state.

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