摘要 : A series of niobium and tantalum complexes containing 1,1-dialkylhydrazine-derived ligands was synthesized. Treatment of niobium or tantalum pentachloride with 2 equivalents of 1,1-dialkyl-2-trimethylsilylhydrazine in the presence... 展开 A series of niobium and tantalum complexes containing 1,1-dialkylhydrazine-derived ligands was synthesized. Treatment of niobium or tantalum pentachloride with 2 equivalents of 1,1-dialkyl-2-trimethylsilylhydrazine in the presence of tetramethylethylenediamine afforded [Nb(NNMe2)Cl-2(NH2NMe2)(TMEDA)]Cl (.) CH2Cl2 (30%), [Ta(NNMe2)Cl-2(NH2NMe2)(TMEDA)]Cl (.) CH2Cl2 (27%), [Nb(NN(CH2)(5))Cl-2(NH2N(CH2)(5))(TMEDA)]Cl (.) CH2Cl2 (13%), and [Ta(NN(CH2)(5))Cl-2(NH2N(CH2)(5))(TMEDA)]Cl (.) CH2Cl2 (23%) as yellow crystalline solids. Analogous treatment of niobium or tantalum pentachloride with 2 equivalents of 1-trimethylsilyl-1-aminopiperidine and one equivalent of 1-aminopiperidine afforded [Nb(NN(CH2)(5))Cl-2(NH2N(CH2)(5))(2)]Cl-.[(CH2Cl2)(C6H14)(0.5)] (61%) and [Ta(NN(CH2)(5))Cl-2(NH2N(CH2)(5))(2)]Cl-.[(CH2Cl2)(C6H14)0.5] (26%) as yellow crystalline solids. The new complexes were characterized by spectroscopic and analytical techniques, and also by X-ray crystal structure determinations. (c) 2006 Elsevier Ltd. All rights reserved. 收起