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.

The synthesis of 2-BrC 6 H 4 SbPh 2 (1) and the serendipitous formation 2-(2'-BrC 6 H 4)C 6 H 4 SbPh 2 (2) are reported. Compounds 1 and 2 were characterized in solution by NMR spectroscopy and their identity was confirmed by high-resolution mass spectrometry. The molecular structures of both compounds were determined by single-crystal X-ray diffraction.

The heteroleptic mercury(II) complex [HgCl{SeC 6 H 4 (CH 2 NMe 2)-2}] (1) was prepared by reacting the corresponding lithium organoselenolate in an equimolar ratio with HgCl 2. The complex [Hg(SCN){SeC 6 H 4 (CH 2 NMe 2)-2}] (2) was prepared by the salt metathesis reaction between 1 and KSCN in a 1:1 molar ratio. The metal complexes were characterized in solution by multinuclear NMR spectroscopy and mass spectrometry and the solid state structure of 1 was determined by single crystal X-ray diffraction. In the crystal of 1 a 1D zigzag polymeric chain was formed by Se•••Hg secondary interactions.