The complexes M(SC3H4NH2)2 (M = Ni, Pd) are not deprotonated by anhydrous liquid ammonia at -33.5° but undergo successive deprotonation upon treatment with 1 and 2 molar equiv of amide ion in ammonia. The reprotonation and methylation of the resulting species are described and interpreted in relation to infrared spectral data. © 1969, American Chemical Society. All rights reserved.