In course of a detailed analysis of various intermetallic compounds derived from the AlB 2 type structure, highresolution X-ray diffraction on single crystals proved very powerful in deriving precise composition of individual phases. E.g., the homogeneity ranges of EuGa 2 and SrGa 2 were determined and associated structure distortions induced by changes in composition were analyzed. The structural models derived are also discussed on the basis of solid state NMR data and in comparison to quantum chemical calculations.