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以Sb2O3、Na2WO4、CoCl2及2,2′-联吡啶为原料,采用水热合成方法,制得了新颖的有机-无机杂化的类Dawson型多金属氧酸盐:[Co(2,2′-bpy)3]2[Co(2,2′-bpy)2Cl][Co(2,2′-bpy)2]H2-[SbW18O60]·4H2O(2,2′-bpy=2,2′-bipyridine),并通过元素分析,IR,XPS,EPR,TG,变温磁化率和X-射线单晶衍射等分析手段对化合物进行表征.X-射线单晶衍射测定表明,该化合物属于正交晶系,Pba2空间群,晶胞参数:a=2.1208(2)nm,b=2.4506(2)nm,c=1.2931(1)nm,Z=2,R1=0.0416,wR2=0.0771.晶体解析表明,Sb2O3与Na2WO4在水热条件下组装成少见的类Dawson型多金属氧酸盐阴离子[SbW18O60]9-,该阴离子的{W18}簇结构骨架中包含一个三角锥形{SbO3}基团.EPR谱分析表明,高自旋态和低自旋态Co2+共存于标题化合物中.磁性质研究表明标题化合物显示抗磁性.
The novel organic-inorganic hybrid Dawson-type polyoxometallates were prepared by the hydrothermal method using Sb2O3, Na2WO4, CoCl2 and 2,2’-bipyridyl as raw materials: [Co (2,2’- (2,2’-bpy) 2Cl] [Co (2,2’-bpy) 2] H2- [SbW18O60] · 4H2O (2,2’-bpy = 2,2’-bipyridine ) Were synthesized and characterized by elemental analysis, IR, XPS, EPR, TG, temperature-dependent magnetic susceptibility and X-ray single crystal diffraction.The X-ray single crystal diffraction analysis showed that the compound belongs to orthorhombic system, P = 0.2931 (1) nm, Z = 2, R1 = 0.0416, wR2 = 0.0771. The crystal analysis shows that Sb2O3 and Na2WO4 was assembled into a rare class of Dawson-type polyoxometalate anions [SbW18O60] 9- under hydrothermal conditions, and the anion had a triangular pyramid {SbO3} group in its {W18} cluster structure. , High-spin states and low-spin states Co2 + coexist in the title compound.Studies on magnetic properties show that the title compound shows diamagnetism.