Synthesis of the hydroxide cluster [Al13(μ3-OH)6(μ-OH)18(H2O)24]15+ from an aqueous solution.

A scalable synthesis of the "flat" tridecameric inorganic cluster [Al(13)(μ(3)-OH)(6)(μ-OH)(18)(H(2)O)(24)](15+) has been realized by treating an aqueous aluminum nitrate solution with a zinc-metal powder at room temperature. Single crystals and polycrystalline samples are readily obtained in yields exceeding 55% relative to the starting reagent Al(NO(3))(3). Products have been characterized by X-ray diffraction and solid-state (27)Al MAS and MQMAS NMR.