π-2-methylallylpalladium (II) complexes containing a nine-membered chelate ring with an azine diphosphine ligand: crystal structure of [
作者:Jan Cermak、Sarath D. Perera、Bernard L. Shaw、Mark Thornton-Pett
DOI:10.1016/0020-1693(95)04761-1
日期:1996.3
r/3-2-MeCaH4)PdCI }2] gave the cationic palladium (II) complex [ (~-2-MeC3H4) Pd PPh2CH2C (But ) =N-N=C (Bu t) CH2PPh2 } ] CI (2a), containing a nine-membered chelate ring with the azine in the E,Z-configuration. The crystal structure of 2a shows that the E,Z-azine backbone C--C=N-N=C--C is essentially planar and the methylallyl ligand is non-planar. The corresponding PF6 salt 2b was prepared using
用0.5当量的[(r / 3-2-MeCaH4)PdCI} 2]处理嗪二膦Z〜Z--PPh2CH2C(But)--NN = C(But)CH2PPh2(1)得到阳离子钯(II)络合物[(〜-2-MeC3H4)Pd PPh2CH2C(But)= NN = C(Bu t)CH2PPh2}] CI(2a),在E,Z-中含有九元螯合环配置。2a的晶体结构表明,E,Z-嗪骨架C–C = NN = C–C基本为平面,而甲基烯丙基配体为非平面。使用在EtOH中的NH4PF 6制备相应的PF6盐2b。2b的质子NMR光谱与温度有关,并且在243 K处获得慢交换极限光谱,其中所有四个CH2P质子都是不等价的,四个具有4J(H〜,H,r,)22.2 Hz的烯丙基质子也是如此。给出了质子,31p IH}和13C IH} NMR数据。2a晶体是单斜晶,