一种具有Keggin结构的有机-无机复合的单铈取代夹心型磷钨酸盐的合成及其结构表征(英文)

Synthesis and structure characterization of an organic-inorganic complex mono-cerium(Ⅳ) substituted sandwich-type phosphotungstate with Keggin structure

在水热条件下合成了一种具有Keggin结构的有机-无机复合的单铈取代夹心型磷钨酸盐[H2dap]2.5H5-[Ce(α-PW11O39)2].11.5H2O(1);利用元素分析、红外光谱和单晶X射线衍射表征了其结构.结果表明,化合物1属于三斜晶系,P-1空间群,晶胞参数为:a=1.254 9(7)nm,b=1.915 9(11)nm,c=2.129 0(12)nm,α=68.426(10)°,β=88.320(10)°,γ=89.853(10)°,V=4.758(5)nm3,Z=2,Dc=4.116g/cm3,GOOF=1.022,R1=0.111 2,wR2=0.218 9.化合物1分子由1个晶体学独立单铈取代夹心型[Ce(α-PW11-O39)2]10-磷钨酸多阴离子,2.5个双质子化的[H2dap]2+阳离子,5个质子及11.5个结晶水分子组成.

An organic-inorganic complex mono-CeIVsubstituted sandwich-type phosphotungstate[（H2dap）2]2.5H5[Ce（α-PW11O39）2].11.5H2O（1;dap=1,2-diaminopropane）was prepared under hydrothermal conditions.The structure of as-synthesized product was characterized by means of elemental analysis,infrared spectrometry and single-crystal X-ray diffraction.Resultsindicate that 1 crystallizes in the triclinic P-1space group with a =1.254 9（7）nm,b =1.915 9（11）nm,c=2.129 0（12）nm,α=68.426（10）°,β=88.320（10）°,γ=89.853（10）°,V =4.758（5）nm3,Z=2,Dc=4.116g/cm3,GOOF =1.022,R1=0.111 2,and wR2=0.218 9.Besides,the molecule of 1 is composed of 1crystallographically independentmono-CeIV substituted sandwich-type[Ce（α-PW11O39）2]10-polyoxoanion,2.5discrete diproto-nated [H2dap]2＋ cations,5protons and 11.5lattice water molecules.