Reaction of [(μ-SCH2)2NPh]Fe2(CO)6 with Ph2PCH2PPh2 in the presence of Me3NO·2H2O gave the title complex [(μ-SCH2)2NPh]Fe2(CO)5(Ph2PCH2PPh2)(1)in 78% yield.The new complex 1 was characterized by elemental analysis,spectroscopy and X-ray crys-tallography.It crystallizes in triclinic,space group P1 with a = 10.832(2),b = 12.003(2),c = 15.579(3),V = 1785.6(6)3,Z = 2,C32H26Fe2NO5PS2,Mr = 819.40,Dc = 1.524 g/cm3,μ(MoKα)= 1.064 mm-1,F(000)= 840,T = 113(2)K,the final R = 0.0543 and wR = 0.1218 for 6203 observed reflections(I > 2σ(I)).The Ph2PCH2PPh2 ligand resides in an axial position of the square-pyramidal coordination sphere of the Fe atom and trans to the benzene ring in order to reduce the steric repulsion between Ph2PCH2PPh2 and the benzene ring.
Treatment of complex [(μ-SCH 2) 2 NCH 2 Ph]Fe 2 (CO) 6 with PPh 3 in the presence of decarbonylating agent Me 3 NO·2H 2 O afforded the title complex [(μ-SCH 2) 2 NCH 2 Ph]Fe 2 (CO) 5 (PPh 3) in 70% yield.The new complex was characterized by elemental analysis,IR,and 1 H (31 P,13 C) NMR spectroscopic techniques as well as by X-ray crystallography.It crystallizes in triclinic,space group P 1 with a=9.3016(19),b=12.698(3),c=13.904(3),V=1519.8(7)3,Z=2,C 32 H 26 Fe 2 NO 5 PS 2,M r=711.33,D c=1.554 g/cm 3,μ(MoKα)=1.187 mm-1,F(000)=728,T=113(2) K,the final R=0.0288 and wR=0.0680 for 3982 observed reflections (I > 2σ(I)).The PPh 3 ligand resides in an axial position of the square-pyramidal geometry of the neighboring Fe atom and trans to the benzene ring in order to minimize the steric repulsion between PPh 3 and the benzene ring.
