| 层状多硫代锑(Ⅲ)酸镉(Ⅱ)化合物(1,4-DABH2)Cd2Sb2S6的溶剂热合成与表征 | |
| Solvothermal Synthesis and Characterzation of (1,4-DABH2)Cd2Sb2S6 with Layer Structure | |
| 摘要: 利用溶剂热方法合成了层状多硫代锑(Ⅲ)酸镉(Ⅱ)化合物(1,4-DABH2)Cd2Sb2S6 (1)(1,4-DAB=1,4-丁二胺),并通过红外光谱、热重分析对其进行了表征,用X-射线衍射测定了化合物的单晶结构。单晶解析表明,化合物属正交晶系,Cmca空间群,Mr=750.77,a=0.860 3(5) nm,b=0.898 7(6) nm,c=2.273(2) nm,V=1.758(2) nm3,Z=4,λ=0.071 073 nm,R=0.032,wR=0.106 7。晶体结构中含有六元环的Cd2SbS3和八元环的Cd2Sb2S4的阴离子网络层状[CdSbS3]nn-,双质子化的有机阳离子在阴离子层之间以氢键N-H…S形式连接。另外紫外-可见漫反射光谱研究表明,化合物为半导体。 | |
| 关键词: 溶剂热合成 多硫代锑酸盐 晶体结构 表征 | |
| 基金项目: 教育部科学技术研究重点项目(No.210041);内蒙古自然科学基金(No.20080404MS021)资助项目。 | |
| Abstract: A multiple thioantimonate compound, (1,4-DABH2)Cd2Sb2S6 (1) (1,4-DAB=1,4-diaminobutane) , was solvothermally synthesized at 160 ℃ and characterized by IR and TGA. Its crystal structure analysis reveals the compound was determined by single crystal X-ray diffraction. The crystal structure is orthorhombic in the space group Cmca. Crystallographic data: Mr=750.77, a=0.860 3(5) nm, b=0.898 7(6) nm, c=2.273(2) nm, V=1.758(2) nm3, Z=4, λ=0.071 073 nm, R=0.032 0, wR=0.106 7. The compound features two-dimensional (2D) grid layer of [CdSbS3]nn- with six-membered Cd2SbS3 rings and eight-membered Cd2Sb2S4 rings. The doubly protonated organic cations are located at the interlayer spaces of [CdSbS3]nn- and form extensive N-H…S hydrogen bonds. In addition, UV-Vis diffusion reflectance spectra suggest that the compound is semiconductor with estimated band gap 2.10 eV. CCDC: 879803. | |
| Keywords: solvothermal synthesis multiple thioantimonate crystal structure characterization | |
| 投稿时间：2012-07-25 修订日期：2013-02-04 | |
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| 刚刚,白音孟和,王晓靖,娜仁吉如嘎,徐效清,白乌云,斯琴达莱.层状多硫代锑(Ⅲ)酸镉(Ⅱ)化合物(1,4-DABH2)Cd2Sb2S6的溶剂热合成与表征[J].无机化学学报,2013,29(5):979-984. | |
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