无机-有机杂化硫属化合物[Mn(1,2-dap)2(H2O)]2(μ-Sn2Q6)(Q=S、Se)和[Mn(tren)]2(μ-Sn2S6)的合成、晶体 结构与性能
Solvothermal Syntheses, Crystal Structures and Properties of [Mn(1,2-dap)2(H2O)]2(μ-Sn2Q6) (Q=S, Se) and [Mn(tren)]2(μ-Sn2S6)
作者单位E-mail
张慧苹 济宁学院化学与化工系, 山东省高校无机化学重点实验室, 曲阜 273155  
雷晓武 济宁学院化学与化工系, 山东省高校无机化学重点实验室, 曲阜 273155 xwlei_jnu@163.com 
摘要: 采用溶剂热方法合成了3个多元硫属化合物[Mn(1,2-dap)2(H2O)]2(μ-Sn2Q6)(Q=S (1)和 Se (2))和[Mn(tren)]2(μ-Sn2S6) (3),用X-射线单晶衍射测定了化合物的结构, 并通过红外光谱、紫外-可见漫反射光谱对其进行了表征.单晶结构解析表明, 化合物12都属于正交晶系, Pccn空间群(No.56),晶体结构是由[Mn(1,2-dap)2(H2O)]2+配合物阳离子和[Sn2Q6]4-二聚体通过Mn-Q键连接而成的[Mn(1,2-dap)2(H2O)]2(μ-Sn2Q6)低聚体, 相邻的低聚体之间通过氢键相连形成三维结构.化合物3属于三斜晶系, 晶体结构是由[Mn(tren)]2(μ-Sn2S6)单元通过氢键连接而成的二维结构.紫外-可见漫反射光谱结果显示化合物1,23的带隙分别为2.5, 2.1,2.4 eV,属于半导体材料.
关键词: 硫属化合物  溶剂热合成  晶体结构
基金项目: 国家自然科学基金青年基金(No.21101075和21201081)资助项目.
Abstract: Three thiostannates(Ⅳ) and selenidostannate(Ⅳ), namely, [Mn(1,2-dap)2(H2O)]2(μ-Sn2Q6) (1,2-dap=1,2-diaminopropane, Q=S (1) and Se (2)) and [Mn(tren)]2(μ-Sn2S6) (tren=tris(2-aminoethyl)amine; 3), have been solvothermally synthesized and structurally characterized. Their crystal structures were established by single-crystal X-ray diffraction, IR and UV-Vis spectra. The compounds 1 and 2 crystallize in the orthorhombic system, space group Pccn (No.56). In their structures, [Mn(1,2-dap)2(H2O)]2+ complex cation and [Sn2Q6]4- dimer are interconnected via Mn-Q covalent bonds to form oligomer, which are further interlinked via hydrogen bonds to form 3D H-bonding network structure. Compound 3 crystallizes in the triclinic system, space group P1 (No.2), and features 2D H-bonding network structure based on [Mn(tren)]2(μ-Sn2S6) units. The optical absorption spectra indicate that compounds 1, 2 and 3 are semiconductors with estimated band gaps of 2.5, 2.1 and 2.4 eV, respectively. CCDC: 1024637, 1; 1024638, 2; 1024636, 3.
Keywords: chalcogenometalate  solvothermal reaction  crystal structure
投稿时间:2014-07-18 修订日期:2014-09-16
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张慧苹,雷晓武.无机-有机杂化硫属化合物[Mn(1,2-dap)2(H2O)]2(μ-Sn2Q6)(Q=S、Se)和[Mn(tren)]2(μ-Sn2S6)的合成、晶体 结构与性能[J].无机化学学报,2014,30(12):2832-2838.
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