Layered materials composed of metal-alkanethiolate units have been synthesi
zed and characterized. The self-assembly occurs at the interface between a
metal-ion-containing aqueous phase and an alkanethiol-containing organic ph
ase. Key features of the structure have been determined from X-ray diffract
ion and infrared spectroscopy measurements. The highly ordered bilayers are
characterized by tilted, all-trans alkyl chains. A new model for the inpla
ne structure has been presented, which is based on a hexagonal arrangement
of metal atoms in the central plane.