New chiral organoantimony(III) compounds containing intramolecular N -> Sb interactions - solution behaviour and solid state structures

作者：Copolovici Dana; Bojan Vilma R; Rat Ciprian I; Silvestru Anca; Breunig Hans J; Silvestru Cristian^*

来源：Dalton Transactions, 2010, 39(28): 6410-6418.

DOI：10.1039/c003318a

Hypervalent organoantimony(III) compounds of the type [2-(Me(2)NCH(2))C(6)H(4)]PhSbCl (1), [2-(Me(2)NCH(2))C(6)H(4)]MesSbBr (7) and [2-(Me(2)NCH(2))C(6)H(4)](n)Ar(3-n)Sb [n = 1, Ar = Ph (4), Mes (9); n = 2, Ar = Ph (5), Mes (10)] were prepared via salt elimination reactions between [2-(Me(2)NCH(2))C(6)H(4)]Li and MesMgBr and Ph(n)SbCl(3-n), [2-(Me(2)NCH(2))C(6)H(4)]SbBr(2) or [2-(Me(2)NCH(2))C(6)H(4)](n)SbCl(3-n) (n = 1, 2), in appropriate molar ratios. Halogen exchange reactions with aqueous KBr or KI gave [2-(Me(2)NCH(2))C(6)H(4)]ArSbX [Ar = Ph, X = Br (2), I (3); Ar = Mes, X = I (8)]. Metathesis reaction between 1 and MesMgBr affords [2-(Me(2)NCH(2))C(6)H(4)]PhMesSb (6). Compounds 1-10 were investigated by means of NMR ((1)H, (13)C) in solution and by mass spectrometry. The investigation of the molecular structures of 2-8 by single-crystal X-ray diffraction revealed that the nitrogen atoms of the pendant CH(2)NMe(2) arms are strongly coordinated to the antimony atoms. All compounds exhibit chirality and crystallize as racemic mixtures.

• 出版日期2010