利用水热技术合成了一种未见报道的二维扩展结构化合物{[Cu2(2,2-′bipy)2(4,4-′bipy)]2[Cu(4,4-′bipy)][PW10(Ⅵ)W2(Ⅴ)O40]}(bipy=联吡啶),并采用红外光谱、元素分析、单晶X射线衍射对其进行了表征.结果表明:该晶体属于单斜晶系,P-1空间群;晶胞参数a=1.364 6(3)nm,b=1.402 2(3)nm,c=1.441 6(3)nm,α=63.78(3)°,β=87.06(3)°,γ=65.56(3)°,V=2.224(8)nm3,Z=1,R1=0.053 9,wR2=0.115 0. An undiscovered two-dimensional extended structure compound {[Cu2 (2,2-’bipy) 2 (4,4-’bipy)] 2 [Cu [PW10 (Ⅵ) W2 (Ⅴ) O40]} (bipy = bipyridine) was synthesized and characterized by IR, elemental analysis and single crystal X-ray diffraction.The results show that the crystal belongs to monoclinic system, P -1 space group; a = 1.364 6 (3) nm, b = 1.402 2 (3) nm, c = 1.441 6 (3) nm, α = 63.78 , γ = 65.56 (3) °, V = 2.224 (8) nm3, Z = 1, R1 = 0.053 9, wR2 = 0.115 0.