Cationic complexes [Mo(η 3 –C 3 H 4 –Me–2)(N–N)(CO) 3 ] + PF 6 − , {N–N=bipy (2); DAD (Ar–NC(Me)–C(Me)N–Ar: Ar=o-Me–C 6 H 4 (3), 2,6-Me 2 –C 6 H 3 (4); Ar–BIAN (Ar=o-Me–C 6 H 4 (5), Ar=iPr 2 –C 6 H 3 (6)}; were synthesized by treating the compound Mo(CO) 3 (p-xylene) with the allyloxyphosphonium salt in situ in presence of diimine ligand. Complex 4 was characterized by single crystal X-ray diffraction. The solid state structure of the complexes revealed a preference for the more unsymmetrical axial isomer.