Synthesis, Magnetism, and Electrochemistry of the Ni14- and Ni5-Containing Heteropolytungstates [Ni14(OH)6(H2O)10(HPO4)4(P2W15O56)4]34–and [Ni5(OH)4(H2O)4(β-GeW9O34)(β-GeW8O30(OH))]13–
Inorganic Chemistry2013Vol. 52(15), pp. 8399–8408
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Masooma Ibrahim, Yixian Xiang, Bassem S. Bassil, Yanhua Lan, Annie K. Powell, Pedro de Oliveira, Bineta Keita, Ulrich Kortz
Abstract
The two Ni(2+)-containing heteropolytungstates [Ni14(OH)6(H2O)10(HPO4)4(P2W15O56)4](34-) (Ni14) and [Ni5(OH)4(H2O)4(β-GeW9O34)(β-GeW8O30(OH))](13-) (Ni5) have been successfully synthesized in aqueous, basic media under conventional reaction conditions, and they were characterized by single-crystal X-ray diffraction, IR spectroscopy, thermogravimetric and elemental analyses, electrochemistry, and magnetic studies. The cyclic voltammetry (CV) patterns of Ni14 and Ni5 showed chemically reversible multielectronic waves for slow scan time scales. For Ni14, an important acidity inversion effect between its reduced forms was observed. Magnetic studies revealed dominant ferromagnetic interactions among the nickel(II) ions in both polyanions.
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