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

引用本文: 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. doi: 10.3969/j.issn.1001-4861.2013.00.176 shu

Citation: GANG Gang, BAIYIN Meng-He, WANG Xiao-Jing, NAREN Ji-Ru-Ga, XU Xiao-Qing, BAI Wu-Yun, SIQIN Da-Lai. Solvothermal Synthesis and Characterzation of (1,4-DABH₂)Cd₂Sb₂S₆ with Layer Structure[J]. Chinese Journal of Inorganic Chemistry, 2013, 29(5): 979-984. doi: 10.3969/j.issn.1001-4861.2013.00.176 shu

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

通讯作者: 白音孟和,E-mail:baiymh@imnu.edu.cn

基金项目:
教育部科学技术研究重点项目(No.210041) (No.210041)

内蒙古自然科学基金(No.20080404MS021)资助项目。 (No.20080404MS021)

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,M_r=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]_n^n-,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

English

Solvothermal Synthesis and Characterzation of (1,4-DABH₂)Cd₂Sb₂S₆ with Layer Structure

1.
1. College of Chemistry & Environmental Science, Inner Mongolia Normal University, Huhhot 010022, China;

Corresponding author: 白音孟和,E-mail:baiymh@imnu.edu.cn

Received Date: 25 July 2012
Fund Project:
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: M_r=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]_n^n- with six-membered Cd₂SbS₃ rings and eight-membered Cd₂Sb₂S₄ rings. The doubly protonated organic cations are located at the interlayer spaces of [CdSbS₃]_n^n- 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.

Key words:

solvothermal synthesis;multiple thioantimonate;crystal structure;characterization

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

通讯作者: 白音孟和,E-mail:baiymh@imnu.edu.cn

English

Solvothermal Synthesis and Characterzation of (1,4-DABH₂)Cd₂Sb₂S₆ with Layer Structure

Corresponding author: 白音孟和,E-mail:baiymh@imnu.edu.cn

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