Synthesis and reactivity of new mono- and dinuclear niobium and tantalum imido complexes: X-ray crystal structure of [Ta(η5-C5H4SiMe3)Cl2{NC6Me4-4-(N(SiMe3)2)}]
作者:Antonio Antiñolo、Iván Dorado、Mariano Fajardo、Andrés Garcés、Marek M. Kubicki、Carmen López-Mardomingo、Antonio Otero、Sanjiv Prashar
DOI:10.1016/j.jorganchem.2005.12.016
日期:2006.3
dienyl or lithium dimethylamide, has been studied and the following compounds prepared:[Nb(η5-C5H4SiMe3)RClNC6Me4-4-(N(SiMe3)2)}] (R = η5-C5H4SiMe3 (8), PhC(NSiMe3)2 (9), NMe2 (10)). In an attempt to form the hetero bimetallic complex, [Nb(η5-C5H4SiMe3)Cl2}(μ-1,4-NC6Me4N)Ta(η5-C5H4SiMe3)Cl2}] (11), the reaction of 7 with [Ta(η5-C5H4SiMe3)Cl4] has been studied. Analysis of the reaction products showed
[1,4- SiMe 3(H)N} 2 C 6 Me 4 ](1)与2当量的LiBu n反应,然后添加SiMe 3 Cl,得到二胺化合物[1,4-( SiMe 3)2 N} 2 C 6 Me 4 ](2)。[TA(η 5 -C 5 H ^ 4森达3)氯4 ]与发生反应2,在2:1的化学计量比,以最初得到的双核的混合物,[TA(η 5 -C 5 H ^4森达3)氯2 } 2(μ-1,4-NC 6我4 N)](3),和单核,[TA(η 5 -C 5 H ^ 4森达3)氯2 NC 6我4 - 4-(N(SiMe 3)2)}](4),亚氨基配合物。通过使反应混合物经历重复的抽真空循环以除去挥发物,然后添加溶剂并随后加热,可以仅获得图3所示的混合物。该单核酰亚胺络合物4,由[TA(η的反应中分离5 -C 5 H 4 SiMe 3)Cl 4 ]与2的化学计量比为1:1。通过X射线衍射研究确定了4的分子结构。[TaCl