本文采用水热技术合成了一种多钒氧酸盐[NH3(CH2)4NH,][H2pip]2[V10O28]·6H2O(1,pip=哌嗪),并且通过元素分析、红外、热重、单晶X-射线衍射对化合物1进行了表征.化合物1为单斜晶系,空间群为P21,晶胞参数为a=1.229 85(10) nm,b=1.07510(9)nm,c=1.496 71(12) nm,β=93.947 0(10)°,V=1.974 3(3) nm3,Z=2.晶体结构分析表明,化合物1是由[V10028]6-阴离子簇、质子化的1,4-丁二胺和哌嗪阳离子以及结晶水构成.有机阳离子和结晶水通过O-H…O和N-H…O氢键相互作用将阴离子连接形成三维结构.%A polyoxovanadate [NH3(CH2)4NH3][H2pip]2[V10O28]·6H2O (1,pip=piperazine) has been synthesized by hydrothermal method and characterized by elemental analysis,IR,TGA and single-crystal X-ray diffraction.Compound 1 crystallizes in the monoclinic system,space group P21,with cell parameters of a=1.229 85(10) nm,b=1.075 10(9) nm,c=1.496 71(12) nm,β=93.947 0(10).,V=1.974 3(3) nm3,Z=2.Crystallographic analysis reveals that it is constructed from anionic cluster [V10O2s]6-,protonated 1,4-butanediamine and piperazine cations,as well as waters of crystallization.Organic cations and waters of crystallization further connect the anions into a three- dimensional framework by water-anion hydrogen bonds O-H…O and cation-anion N-H…O interactions.CCDC:848090.
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