[en] Solid state CP/MAS ⁸⁹Y NMR spectroscopy, which had previously been limited to air stable materials containing solvated water, has been extended to a series of air sensitive yttrium complexes with a chemical shift range of over 1,000 ppm. The results of this study demonstrate that ⁸⁹Y CP/MAS spectra can be easily obtained on a broad range of complexes in a short period of time. A convenient method for obtaining the Hartmann-Hahn match is described, and probe ringing is shown to be minimal. The effects of variable power level, contact time, and spinning rate are described. Spectra obtained on mono-, di-, and polymetallic samples which had been characterized by X-ray crystallography show a direct correlation between the number of signals and the number of unique solid state environments. The utility of this method in identifying impurities in yttrium-containing materials difficult to characterize by other methods is demonstrated. 32 refs., 8 figs., 2 tabs