Hydrothermal Synthesis of a Three-Dimensional Organic−Inorganic Hybrid Network Formed by Poly(oxomolybdophosphate) Anions and Nickel Coordination Cations

A novel organic−inorganic hybrid nickel molybdenum(V) phosphate
has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction, thermogravimetric analysis, and magnetic
susceptibility. The structure consists of poly(oxomolybdophosphate)
anions linked by both NiII cations and 4,4-bipyridine bridging ligands
to form a three-dimensional open-framework structure with large
cavities where the uncoordinated 4,4‘-bipyridinium cations and
lattice water molecules are located. This is the first example of an
extended framework solid containing poly(oxomolybdophosphate)
anions interconnected by both transition-metal complexes and
organic moieties. Crystal data:  (4,4‘-H2bpy)[Ni(4,4‘-bpy)(H2O)2Ni0.5Mo6(OH)3O12(HPO4)4]·2H2O, orthorhombic, space group Pccn (No.
56), a = 27.745(2) Å, b = 16.158(1) Å, c = 22.819(2) Å, V =
10230.3(1) Å3, and Z = 8.