Cyclopalladation of C6H4(CH2SBut)2-1,3 and the crystal structure of [PdCl{C6H3(CH2SBut)2-2,6}]

Abstract

The new disulphide C₆H₄(CH₂SBu^t)₂-1,3 has been prepared from 1,3-di(bromomethyl)benzene and Bu^tSH using phase-transfer catalysis. It has been shown to cyclopalladate readily into the 2-position giving the title complex (2), the crystal structure of which has been determined: (2) reacts with PPh₃ to give [PdCl{C₆H₃(CH₂SBu^t)₂-2,6}(PPh₃)₂] which is extensively dissociated in solution. Crystals of (2) are orthorhombic, space group Pbcn, with a= 9.654(2), b= 14.509(3), c= 12.797(3)Å, and Z= 4. The structure has been determined from 1 024 independent F₀ values and the final R is 0.043. The molecules have crystallographic symmetry C₂.