New hypercoordinated organoantimony(V) bromides. Synthesis and structural characterization

Abstract

The oxidative addition of bromine to [2-(Me 2 NCH 2)C 6 H 4 ]SbBr 2 and [2-(Me 2 NCH 2)C 6 H 4 ]Ph 2 Sb resulted in the new hypercoordinated organoantimony(V) compounds [2-(Me 2 NCH 2) C 6 H 4 ]SbBr 4 (1) and [2-(Me 2 NCH 2)C 6 H 4 ]Ph 2 SbBr 2 (2), respectively. The new species were isolated as colourless solids and their solution behaviour was investigated by 1 H and 13 C{ 1 H} NMR spectroscopy. Single-crystal X-ray diffraction studies evidenced strong N→Sb intramolecular interactions in 1 and 2. While 2 has a monomeric structure, in the crystal of 1 the molecules are associated in polymeric chains by weak Br•••H contacts. The ionic derivative [{2-(Me 2 NH + CH 2)C 6 H 4 }Ph 2 SbBr 2 ]Br-•CHCl 3 (3•CHCl 3) was isolated as a hydrolysis product during our attempts to grow single-crystals of 2 from a n-hexane/CHCl 3 mixture of solvents.