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Two inorganic–organic hybrid complexes based on bi-capped Keggin-type cluster, {([Cu^II(2,2′-bpy)₂]₂[PMo^VI₈V^V₂V^IV₂O₄₀(V^IVO)₂])[Cu^I(2,2′-bpy)]}∙2H₂O (<b>1</b>) and {[Cu^II(2,2′-bpy)₂]₂[SiMo^VI_8.5Mo^V_2.5V^IVO₄₀(V^IVO)₂]}[Cu^I_0.5(2,2′-bpy)(H₂O)_0.5] (<b>2</b>) (bpy = bipyridine), had been hydrothermally synthesized and structurally characterized by elemental analysis, FT-IR, TGA, PXRD and X-ray single-crystal diffraction analysis. Compound <b>1</b> consists of a novel 1-D chain structure constructed from [Cu^I(2,2′-bpy)]⁺ unit linking bi-supported POMs anion {[Cu^II(2,2′-bpy)₂]₂[PMo^VI₈V^V₂V^IV₂O₄₀(V^IVO)₂]}⁻. Compound <b>2</b> is a bi-capped Keggin cluster bi-supported Cu-bpy complex. The main highlights of the two compounds are that Cu-bpy cations contain both Cu^I and Cu^II complexes. Furthermore, the fluorescence properties, the catalytic properties, and the photocatalytic performance of compounds <b>1</b> and <b>2</b> have been assessed, and the results show that both compounds are active for styrene epoxidation and degradation and adsorption of Methylene blue (MB), Rhodamine B (RhB) and mixed aqueous solutions.