A novel hexanuclear Ni-substituted polyoxometalate [Ni-4(H2O)(2)(alpha-NiW9O34)(2)](16-) (1) has been synthesized through a hydrothermal method. Polyoxoanion 1 exhibits a usual tetranuclear sandwich-type structure based on unprecedented [alpha-NiW9O34](12-) building units and represents the first polyoxotungstate with four-coordinate nickel centers as heteroatoms.
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