Cyclic Metal(IV)Amides Synthesis and structure of cyclic amide complexes of quadrivalent titanium, vanadium, and chromium are described, and their electrochemical behavior is investigated by cyclic voltammetry. The novel amides of formula ML 2 {MTi, ( 3b ); MV, ( 3c ); MCr, ( 3d ); L=[(CH 3 ) 3 SiNCH 2 CH 2 NSi(CH 3 ) 3 ]} are formed by reaction of the halide adducts MCl 3 (THF) 3 with the dilithium salt Li 2 L with concomitant disproportionation. Formation of 3d proceeds via the complex [3 d] ⊖ and requires additional oxidation with oxygen or iodine. An X‐ray crystalstructure determination of 3b reveals the titanium atom in strongly distorted tetrahedral environment with approximate symmetry D 2d . The amide complexes 3b – d are monomeric, thermally stable, and sublime readily without decomposition; they are very sensitive to water and soluble in all common organic solvents.
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Herrmann et al. (1991) studied this question.