Abstract The use of SbF 5 intercalated in graphite as fluorinating reagent of organo-silicon and-germanium derivatives is described. While Si O and Si Cl bonds are readily cleaved, Si H and Si S bonds are only reactive in bifunctional silanes. Ge X bonds (X= Br, Cl, OR, H) are unreactive. Allyl silicon and allyl germanium bonds are broken under mild conditions and in high yields, leading to the corresponding fluorosilane or fluorogermane. ...