Abstract
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(NNMe 2)Cl 2(NH 2NMe 2)(TMEDA)]Cl · CH 2Cl 2 (30%), [Ta(NNMe 2)Cl 2(NH 2NMe 2)(TMEDA)]Cl · CH 2Cl 2 (27%), [Nb(NN(CH 2) 5)Cl 2(NH 2N(CH 2) 5)(TMEDA)]Cl · CH 2Cl 2 (13%), and [Ta(NN(CH 2) 5)Cl 2(NH 2N(CH 2) 5)(TMEDA)]Cl · CH 2Cl 2 (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(CH 2) 5)Cl 2(NH 2N(CH 2) 5) 2]Cl · [(CH 2Cl 2)(C 6H 14) 0.5] (61%) and [Ta(NN(CH 2) 5)Cl 2(NH 2N(CH 2) 5) 2]Cl · [(CH 2Cl 2)(C 6H 14) 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.
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