Synthesis and Characterization of the First Nickel(II)-Centered Single-Side Tris-Functionalized Anderson-Type Polyoxomolybdate

The Ni-centered Anderson-type polyoxomolybdate [Ni(OH)(3)Mo6O18(OCH2)(3)CNH3](3)-was prepared in a two-step aqueous reaction by covalent postfunctionalization of [Ni(OH)(6)Mo6O18](4-), isolated as its sodium Tris-NH3 salt, and characterized by single-crystal X-ray diffraction, mass spectrometry, thermogravimetric analysis, and IR spectroscopy. The incorporation of a Tris-NH2 ligand into the framework of a heteropolymolybdate bearing a divalent heteroatom, which resulted in the single-sided product, was shown for the first time.