Oligophosphan-Liganden, XIV [1] Bis(distickstoff)molybdän-KomplexeMo(N2)2[PhP(CH2CH2CH2PPh2)2](PR3) / Oligophosphine Ligands, XIV [1] Bis(dinitrogen)molybdenum Complexes Mo(N2)2[PhP(CH2CH2CH2PPh2)2](PR3)

Abstract

The reaction of MoCl3(THF)3 with PhP(CH2CH2CH2PPh2)2 in THF/CH2Cl2 gave MoCl3(PhP(CH2CH2CH2PPh2)2) ·CH2CI2 (1). Sodium amalgam reduction of I in the presence of the monotertiary phosphines PMe3-nPhn (n = 0, 1, 2), in THF under nitrogen atmosphere, yielded the bis(dinitrogen) complexes Mo(N2)2[PhP(CH2CH2CH2PPh2)2](PMe3) (2), Mo(N2)2[PhP(CH2CH2CH2PPh2)2](PMe2Ph) (3), and Mo(N2)2[PhP(CH2CH2CH2PPh2)2I(PMePh2) (4). The homologous PPh3 and i-Pr3P derivatives as well as the attempted tris(dinitrogen) species Mo(N2)2[PhP(CH2CH2CH2PPh2)2] could not be isolated. Compounds 2-4 were assigned trans coordination of the N2 ligands on the basis of their IR, Raman, and 31P NMR spectra. The trans- octahedral geometry of these complexes was also confirmed by a single-crystal X-ray diffraction study performed on 3.