A series of beta (β) zeolites has been synthesized in a fluoride medium and characterized by different techniques. XRD showed that the majority of FSiβ, FPtβ, FPdβ, and FWβ materials consisted of polymorph A. W and Al were incorporated into the framework of β, while Pt and Pd existed on the surface of β in the form of PtO x or PdO x oxides. The framework structures of FSiβ, FPtβ, and FPdβ were almost identical, as proven by 29 Si MAS NMR and FTIR spectra. The relative coverage of surface –OH groups decreased in the sequence Hβ>HZSM-5>FAlβ>FWβ>FPdβ>FPtβ>FSiβ(1)>FSiβ(2). SEM revealed an especially uniform crystalline morphology of FSiβ(2) nucleated spontaneously and a mixed morphology of FSiβ(1), FWβ, FPtβ, and FPdβ induced by seeding Hβ. The reduced FPtβ and FPdβ were catalytically active for the asymmetric hydrogenation of tiglic acid with an appreciable enantiomeric excess value of about 9–11% without adding chiral modifiers.