The tris(pyrazolyl)hydroaluminate derivatives, [HAlTp Bu t ,Me ]Li and {[HAlTp Me 2 ]Li} 2 , have been synthesized via the reactions of LiAlH 4 with 3-tert-butyl-5methylpyrazole and 3,5-dimethylpyrazole, respectively, while the tris(pyrazolyl)hydrogallate counterparts, [HGaTp Bu t ,Me ]Li and {[HGaTp Me 2 ]Li} 2 , are obtained from the corresponding reactions with LiGaH 4. X-ray diffraction studies demonstrate that the 3-tert-butyl-5-methylpyrazolyl derivatives, [HAlTp Bu t ,Me ]Li and [HGaTp Bu t ,Me ]Li, are monomeric with lithium in a trigonal coordination environment, whereas the less sterically demanding 3,5-dimethylpyrazolyl derivatives, {[HAlTp Me 2 ]Li} 2 and {[HGaTp Me 2 ]Li} 2 , are dimeric. In addition to the tris(pyrazolyl)hydroaluminate derivative, [HAlTp Bu t ,Me ]Li, the tetrakis derivative, [(pz Bu t ,Me)AlTp Bu t ,Me ]Li, has also been isolated. X-ray diffraction studies demonstrate that [(pz Bu t ,Me)AlTp Bu t ,Me ]Li, as obtained from solutions in benzene, exists as a monomer in the solid state with tridentate coordination, whereas crystals obtained from THF exhibit a bidentate coordination mode, which is supplemented by coordination of THF, i.e. [(pz Bu t ,Me) 2 AlBp Bu t ,Me ]Li(THF). NMR spectroscopic studies, however, indicate that [(pz Bu t ,Me)AlTp Bu t ,Me ]Li is fluxional in both benzene and THF solutions.