Unexpected product formed by the reaction of [2,6-(MeOCH 2) 2C 6H 3]Li with SbCl 3: Structure of Sb–O intramolecularly coordinated organoantimony cation

Abstract

Reaction of [2,6-(MeOCH 2) 2C 6H 3]Li ( 1) with SbCl 3 in 1:1 molar ratio yielded except the intended product [2,6-(MeOCH 2) 2C 6H 3]SbCl 2 ( 2) unexpected complex 3 consisting of antimony anion [Sb 6Cl 22] 4− compensated by four intramolecularly coordinated organoantimony cations [2,6-(MeOCH 2) 2C 6H 3] 2Sb +. Compound 3 is labile in CH 2Cl 2(CHCl 3) solution and decomposes to compound 2 and SbCl 3. Both compounds were characterized by the help of 1H and 13C NMR spectroscopy, ESI-mass spectrometry and in the case of 3 by single crystal X-ray diffraction techniques.