One-Step Preparation and Crystallization of Almost Insoluble Palladium(II) and Platinum(II/IV) Complexes from a Biphasic Solvent System

Scarcely soluble palladium­(II) and platinum­(II/IV) halido complexes with diamino ligands were prepared via a biphasic solvent system. Metal precursors like tetrachloridopalladate salts were dissolved in oxygen-free water, whereas the organic diamino ligands were dissolved in dry and oxygen-free dichloromethane. The dichloromethane layer was carefully covered with the aqueous layer under nitrogen atmosphere at room temperature. The desired products crystallized within a few weeks at the phase boundary. In the case of dihalidopalladium complexes with diamino-binaphthalene and diamino-carbohydrate ligands, crystals were obtained without further manipulation that were suitable for X-ray structure analysis.