The complexes NEt4[Fe(NS3)(CNR)] (1), [Fe{Fe(NS3)(CNR)}(2)-S,S'] (2), [Co{F
e(NS3)(CNMe)}(2)-S,S' ] (3), and [Ni{Fe(NS3)(CNMe)}(2)-S,S'] (4) (R = Me, t
-Bu, or C6H11(Cy)) have been prepared and the X-ray crystal structures of N
Et4[Fe(NS3)(CNMe)] (1a) and [Fe{Fe(NS3)(CNCy)}(2)-S,S'] (2c) have been dete
rmined. Mossbauer and IR spectroscopic data and room temperature magnetic m
oments for these complexes are reported.