A novel high-nuclear Ni-substituted poly(polyoxometalate) [poly(POM)], [HN(CH)]NaCsH[(Cs(HO))@{(PO)-@(Ni(OH)(WO))@(-α-PWO)}]·30HO (), has been successfully developed and structurally characterized. The polyoxoanion of can be viewed as a unique huge sandwich structure made of an unprecedented Cs(HO) ({Cs}) cluster core encapsulated by two trimeric [(PO)@(Ni(OH)(WO))@(-α-PWO)] subunits, in which the {Cs} cluster presents an interesting Anderson-like arrangement and is the first example of a classical POM configuration based on the alkali metal cluster in the POM chemistry. The polyoxoanion can also be described as an unusual [(Cs(HO))@{(PO)@(Ni(OH)(WO))}] cluster packaged by six {PW} fragments. Furthermore, investigations on the Knoevenagel condensation reaction reveal that has good catalytic activity for the condensation of various aldehydes and malononitrile into corresponding products with excellent yields.
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