We have studied the 19F chemical‐shift anisotropy in NF3 and CHF3 trapped in β‐quinol clathrates. It is known that molecules trapped in these compounds become aligned at low temperatures so that studies of relatively isolated oriented molecules become possible. The nuclear magnetic resonance was observed at several frequencies with the magnetic field applied at various angles relative to the crystal axis. The orientation of the molecules in the cavity and the dipolar broadening due to the lattice protons could be estimated rather closely by a qualitative analysis of the line shapes. The principal components of the chemical‐shift tensor of NF3 could be determined from the observed variation of the first and second moments of the line with the strength and orientation of the magnetic field. This determination was further substantiated by the good agreement between the calculated and observed line shapes for various values of the magnetic field. For CHF3, where the chemical‐shift anisotropy is smaller, only a cruder analysis was practicable. The values of the anisotropy of the chemical‐shift tensor obtained were σ∥−σ⊥ = (390±60) ppm for NF3 and σ∥−σ⊥ = (105±20) ppm for CHF3, where σ⊥ is the average of the two components of the chemical‐shift tensor perpendicular to the fluorine bond direction. For NF3 a difference of (140±40) ppm between the two perpendicular components was found, indicating a deviation from uniaxial symmetry of the NF bond. The sign and order of magnitude of the chemical‐shift anisotropy are discussed and can be understood on the basis of current ideas about the relationship between the bond characters and the chemical‐shift anisotropy.