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Vibrational spectra of diazoacetonitrile, [FIGURE] isolated photolysis products and their deuterated analogs are being investigated in our group. Photolysis of matrix-isolated diazoacetonitrile gives rise to several new spectral features, some attributable to the cyanomethylene free radical. The existence of the triplet in the matrix is confirmed by ESR experiments. The work completed to date will be reported and a discussion of its implications will be presented.