AbstractWe describe a new solid‐state nuclear magnetic resonance (NMR) technique for correlating anisotropic and isotropic chemical shifts in powdered samples. Two‐dimensional (2D) NMR spectra are obtained by processing signals acquired inindependentexperiments for different angles between the sample spinning axis and the Zeeman magnetic field. This 2D NMR approach can therefore resolve individual static anisotropic lineshapes according to their isotropic chemical shift frequencies, without use of sudden mechanical motions or multiple‐pulse irradiation schemes. Applications of the technique are illustrated with an analysis of the chemical shift anisotropy for the eight distinct13C sites in tyr