Three polyoxometalate-based inorganic–organic hybrid compounds constructed from silver(I)-L (L = N,N′-bis-pyridin-2-ylmethylene-hydrazine) species and saturated Keggin type polyoxoanions, {[Ag3L3](PW12O40)(CH3CN)(DMF)2.5}n (1), [Ag4L3(CH3CN)4][Ag2L(CH3CN)3](PMo12O40)2·CH3CN (2) and [(SiMo12O40){Ag2L(CH3CN)3}2]·(CH3CN)2 (3), have been synthesized and structurally characterized by IR spectroscopy, UV spectroscopy, thermogravimetric (TG) analyses and complete single crystal structure analyses. The structure of 1 containing [PW12O40]3− anions as templates exhibits a one-dimensional chain structure constructed by the coordination of a silver center and bis-bidentate bridging ligands with the pyridyl rings adopting a transoid configuration. Compound 2 displays an AB-type arrangement supramolecular structure, in which A is a two-dimensional sheet formed by linking the adjacent [Ag4L3(CH3CN)4]4+ units through the cooperativity of intermolecular π–π interactions and C–H⋯π interactions, while B is composed of [PMo12O40]3− anions and binuclear [Ag2L(CH3CN)4]2+ cations. Compound 3 exhibits a new bisupporting Keggin-polyoxometalate structure in which the [SiMo12O40]4− core supports two [Ag2L(CH3CN)3]2+ fragments in two opposite positions. The luminescent properties of L and 1–3 in the solid state were investigated.
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