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以1,2-乙二硫醇为螯合剂,用溶剂热方法合成了两种四元硫代锗酸盐(H3O)10K6Cu32Ge12S48·6H2O(1)和(H3O)10Rb6Cu32Ge12S48·6H2O(2),通过单晶X射线衍射、SEM、EDS、IR和UV-Vis等方法对其进行表征.结果表明,1和2是类质同晶化合物,其晶体结构中均含有二十面体[Cu8S12]16-阴离子簇,该二十面体间通过GeS4四面体连接形成3D空旷骨架,产生3D孔道,碱金属阴离子与水分子位于3D孔道内.1的结晶学数据为Mr=4 977.58,Fm3c,a=b=c=1.759 49(4)nm,α=90°,V=5.447 0(2)nm3,Z=2,Mo Kαλ=0.071 073nm,R(F)=5.77%,wR(F2)=14.95%.2的结晶学数据为:Mr=5 255.80,Fm3c,a=b=c=1.760 3(2)nm,α=90°,V=5.454 8(11)nm3,Z=2,Mo Kαλ=0.071 073nm,R(F)=5.54%,wR(F2)=18.18%.紫外-可见漫反射光谱研究表明,两种化合物的禁带宽度分别为4.7eV和5.1eV.在紫外光照射下,化合物1对偶氮胂(Ⅲ)染料溶液的脱色率可达到82%.
Two kinds of quaternary thiogermanate (H3O) 10K6Cu32Ge12S48 · 6H2O (1) and (H3O) 10Rb6Cu32Ge12S48 · 6H2O (2) were synthesized by solvothermal method using 1,2-ethanedithiol as chelating agent. X-ray diffraction, SEM, EDS, IR and UV-Vis. The results show that 1 and 2 are isomorphic compounds, all of which contain the icosahedron [Cu8S12] 16- , The icosahedron formed by 3D GeS4 tetrahedron connected to the open skeleton, resulting in 3D channels, alkali metal anions and water molecules located in the 3D pore .1 crystallographic data for Mr = 4 977.58, Fm3c, a = b = c = 1.75949 (4) nm, α = 90 °, V = 5.447 0 (2) nm3, Z = 2, Mo Kαλ = 0.071 073 nm, R (F) = 5.77%, wR (F2) = 14.95% The data of the study are: Mr = 5 255.80, Fm3c, a = b = c = 1.760 3 (2) nm, α = 90 °, V = 5.454 8 (11) nm3, Z = 2, Mo Kαλ = 0.071 073nm, R F = 5.54%, wR (F2) = 18.18% .Ultraviolet-visible diffuse reflectance spectroscopy study showed that the forbidden band width of the two compounds were 4.7eV and 5.1eV respectively.Compared with the arsenazo Ⅲ) dye solution decolorization rate can reach 82%.