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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.
Treatment of complex [(μ-SCH 2) 2 NCH 2 Ph] Fe 2 (CO) 6 with PPh 3 in 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 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.