合成了1种无机-有机杂化钼酸盐化合物(Hmorph)4[SiMo12O40]·2H2O(Hmorph=morpholine,吗啉).用元素分析、X射线单晶衍射、红外光谱和热重对晶体的结构进行了表征.该晶体属于三斜晶系,P-1空间群,晶胞参数a=1.214 71(13)nm,b=1.399 0(3)nm,c=1.735 1(2)nm,α=79.892(13)°,β=82.719(9)°,γ=71.812(14)°,V=2.749 7(7)nm3,Z=2.在该化合物晶体结构中包含质子化的吗啉分子、带负电荷的Keggin结构多阴离子簇以及水分子,在分子中通过静电引力及氢键作用交替排列.紫外光谱和电化学实验证明,标题化合物(Hmorph)4[SiMo12O40]·2H2O在水溶液中对ClO3-具有良好的电催化性质.
A new heteropolymolybdate(Hmorph)4[SiMo12O40]·2H2O(Hmorph = morpholine),has been synthesized in aqueous solution and characterized by elemental analysis,IR spectroscopy,thermogravimetric analysis(TGA)and single-crystal X-ray diffraction.The crystals are triclinic,P-1,a=1.214 71(13)nm,b=1.399 0(3)nm,c=1.735 1(2)nm,α=79.892(13)°,β=82.719(9)°,γ=71.812(14)°,V=2.749 7(7)nm3,Z=2.X-ray diffraction indicated that protonated morpholine cation and Keggin-type [SiMo12O40]4-anion were linked together through electrostatic interactions and intermolecular forces(hydrogen bonding).The UV-Vis spectrum and electrochemical properties of title compound in aqueous solution are studied at room temperature.It was found that title compound presents good electrocatalytic activities for the reduction of ClO3-.