Darstellung und Charakterisierung komplexierter Triphosphane—Die Kristallstruktur von HP[PPh2Cr(CO)5]2
作者:Manfred Scheer、Steffen Gremler、Eckhard Herrmann、Peter G. Jones
DOI:10.1016/0022-328x(91)86332-k
日期:1991.8
The reaction of MIP(SiMe3)2 (MI = Li, Na, K) with R2P(Cl)M′(CO)5 (R = Ph, Et; M′ = Cr, W) or of PCl3 with MIPPh2M′(CO)n (MI = Li, K; M′ = Cr, W, n = 5; M′ = Fe, n = 4) affords triphosphanes of the type HP[PR2M′(CO)n]2. 31P NMR investigations of the reaction mixtures show a number of precursor compounds, on which basis the formation mechanism can be discussed. The products were characterized by 1H,
M I P(SiMe 3)2(M I = Li,Na,K)与R 2 P(Cl)M'(CO)5(R = Ph,Et; M'= Cr,W)或具有M I PPh 2 M'(CO)n(M I = Li,K; M'= Cr,W,n = 5; M'= Fe,n = 4)的PCl 3提供HP [PR 2 M'(CO)n ] 2。反应混合物的31 P NMR研究显示了许多前体化合物,可以在此基础上讨论其形成机理。产品的特点是1 H,13 C,31 P NMR和IR光谱以及质谱。HP [PPH 2的Cr(CO)5 ] 2(1)结晶在空间群C ^ 2 / ç,具有一1873.0(7),b 934.8(4),Ç 2202.5(9)时,β113.76°(在- 95°C且Z =4。该分子具有晶体学上的对称性,但中心PH部分在双向轴上无序。PP键的长度为219.5(2)和223.5(2)pm,PPP为121.2(1)°。