Abstract A novel nanoscopic, partly hydroxylated aluminium fluoride was prepared in a sol- gel fluorination synthesis and characterised by IR probe molecules. It was shown that this material has, in contrast to high surface area aluminium fluoride (HS-AlF 3) which is one of the strongest Lewis acids, a low amount of strong Lewis acid sites combined with weak and medium strength Brønsted sites. Both materials were tested in the synthesis of (all-rac)-α- ...