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

The Ni‐centered Anderson‐type polyoxomolybdate [Ni(OH)3Mo6O18(OCH2)3CNH3]3– was prepared in a two‐step aqueous reaction by covalent postfunctionalization of [Ni(OH)6Mo6O18]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.