The first variable-temperature isotropic high-resolution NMR spectra of solids (frozen liquids) are reported. Magic angle spinning, combined with cross-polarization and dipolar decoupling, were employed to obtain low-temperature 13C NMR spectra of benzene and tert-butyl acetate. The preliminary results clearly demonstrate the value of variable-temperature magic angle spinning high-resolution NMR methods for the study of organic solids. © 1978, American Chemical Society. All rights reserved.