The complexes NEt4[Fe(NS3)(CNR)] (1), [FeFe(NS3)(CNR)}2-S,S' ] (2), [CoFe(NS3)(CNMe)}2-S,S' ] (3), and [NiFe(NS3)(CNMe)}2-S,S' ] (4) (R = Me, t-Bu, or C6H11(Cy)) have been prepared and the X-ray crystal structures of NEt4[Fe(NS3)(CNMe)] (1a) and [FeFe(NS3)(CNCy)}2-S,S' ] (2c) have been determined. Mössbauer and IR spectroscopic data and room temperature magnetic moments for these complexes are reported.Key words: iron, cobalt, nickel, thiolate, isocyanide.