有机杂化硫代碲酸盐化合物(H_2en)TeS_3和[Ni(en)_3]TeS_3的溶剂热合成与表征

Solvothermal Synthesis and Characterization of Two Thio-Tellurite(H_2en)TeS_3 and [Ni(en)_3]TeS_3

用低温溶剂热法合成了2种分立结构的有机杂化硫代碲(Ⅳ)酸盐化合物(H2en)TeS3(1)和[Ni(en)3]TeS3(2)(en=乙二胺),通过X-射线单晶衍射,红外光谱,元素分析等手段对它们的结构进行了表征。晶体结构解析结果表明:2个化合物均属单斜晶系,空间群分别为P21和P21/c。化合物1和2具有孤立三角锥[TeS3]2-阴离子,化合物1的平衡阳离子为双质子化乙二胺[H2en]2+,阴离子基团[TeS3]2-和阳离子基团[H2en]2+之间通过N-H…S氢键连接。化合物2的阳离子基团为过渡金属Ni与乙二胺的配合物[Ni(en)3]2+。另外,对该2种晶体进行了紫外-可见漫反射光谱测试和热重分析。

Two organic hybrid tellurite（Ⅳ） sulfide compound （Hzen）TeS3 （1） and [Ni （en）3]TeS3 （2） （en = ethylenediamine） were Solvothermally synthesized and structurally characterized by elemental analysis, singlecrystal and powder X-ray diffraction, IR, TGA and UV-Vis diffuse reflectance spectroscopy. Compound 1 and 2 crystallizes in the monoclinic space group P21 and P21/c. Both composed of the discrete trigonal-pyramidal [TeS3]^2- anion with complex cations [Hzen]/＋or [Ni（en）3]^2＋ as counterions. In the compound 1, the bio-protonated amine of [H2en]^2＋ and [TeS3]^2- are connected by N-H...S hydrogen bonds. In the compound 2, the Ni^2＋ is octahedral coordination geometry coordinated by six N atoms from three ethylenediamine ligands. CCDC： 927921, 1; 927922,2.