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A pyridine-derived tetraphosphane ligand (donor set: NP 4 ) has been found to undergo remarkably specific C-P bond cleavage reactions, thereby producing a ligand with an NP 3  donor set. The reaction may be reversed under suitable conditions, with regeneration of the original NP 4  ligand. In order to investigate the mechanism of this reaction, the NP 3  donor ligand C 5 H 3 N[CMe(CH 2 PMe 2 ) 2 ][CMe 2 (CH 2 PMe 2 )] (11) was prepared, and its iron(II) complex 4 generated from Fe(BF 4 ) 2  ・6H 2 O, with methyl diethylphosphinite (7) as an additional monodentate ligand. Ligand 11 has, in addition to the NP 3  donor set, one methyl group in close contact with the iron center, reminiscent of an agostic M・ ・ ・H-C interaction. Depending on the stoichiometric amount of iron(II) salt, a side product 15 is formed, which has a diethylphosphane ligand instead of the phosphinite 7 coordinated to iron(II). While attempts to deprotonate the metal-coordinated methyl group in 4 were unsuccessful, the reaction was shown to occur in an alternative complex (18), which is similar to 4 but has a trimethylphosphane ligand instead of the phosphinite 7. The reaction of complex 15 with CO gave two different products, which were both characterized by single-crystal X-ray diffraction. One (19) is the dicarbonyl iron(II) complex of the triphosphane ligand 11, the other (3) is the carbonyl iron(II) complex of the tetraphosphane C 5 H 3 N[CMe(CH 2 PMe 2 ) 2 ] 2  (1). This suggests an intermolecular mechanism for the C-P bond formation in question.

Bond Activation in Iron(II) and Nickel(II) Complexes of Polypodal Phosphanes