When [(OC) 3 Fe(µ-CO)(µ-dppm)PtCl 2 ] (1) is allowed to react with stoichiometric amounts of various isocyanides, cleavage of the metal−metal bond occurs, yielding the heterodinuclear isocyanide complexes [(OC) 4 Fe{µ-dppm}Pt(Cl) 2 (CNR)] (2a: R = 2,6-xylyl; 2b: R = o-anisyl; 2c: R = benzyl; 2d: R = cyclohexyl; 2e: R = tosylmethyl). Reduction of 2a−2e by NaBH 4 in the presence of PPh 3 affords the isocyanide-bridged complexes [(OC) 3 Fe(µ-C=N−R)(µ-dppm)Pt(PPh 3 )] (3a: R = 2,6-xylyl; 3b: R = o-anisyl; 3c: R = benzyl; 3d: R = cyclohexyl; 3e: R = tosylmethyl). Metathesis of 2a−2d with NaI rapidly results in the formation of [(OC) 4 Fe{µ-dppm}PtI 2 (CNR)] (4a−4d), which is slowly transformed under extrusion of CO giving [(OC) 2 IFe{µ-dppm}(µ-CO)PtI(CNR)] (6a: R = 2,6-xylyl; 6b: R =
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