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The synthesis and spectroscopic properties of some new acyls of Ni(II) of formula Ni(COR)(S₂ CNR′₂)(PMe₃) (R=Me₃- SiCH₂, Me₂PhCCH₂; R′=Me, Et, i-Pr) are described. Infrared and ¹Hnmr studies show a square planar structure for the complexes with a bidentate dithiocarbamate ligand. The new acyls undergo dynamical behaviour in solution and participate in carbon monoxide exchange reactions with NiRCI(PMe₃)₂ complexes to give NiR-(S₂CNR′₂)(PMe₃) and Ni(COR)CI(PMe₃)₂.