Two compounds with 3-methylbenzoic acid(HL) [Co(L)2(4,4'-bipy)]n 1 and [Zn2(L)4(4,4'-bipy)]n 2(L = 3-methylbenzoic acid) have been hydrothermally synthesized directly and characterized by single-crystal X-ray diffraction analysis,elemental analyses,IR spectra and ultraviolet-visible diffuse reflection integral spectra(UV-Vis DRIS).The two compounds are both one-dimensional infinite chains.The structural difference is that 1 is a double-chain structure and 2 is only a single chain one.At the same time,the carboxylate groups adopt different modes in the two compounds,relatively.Additionally,in order to explore the structural characteristic,two-dimen-sional IR spectra are investigated for 1 and 2.Photo-luminescent property of 2 is also researched in detail.
A polyoxovanadium borate [Na(H2O)]2[Na(H2O)2]2[Cu(en)2][V12B18O54(OH)6]·(H3O)2·(H2O)18 1(en = ethylenediamine) has been hydrothermally synthesized and characterized by IR,two-dimensional infrared(2D IR) correlation spectroscopy with magnetic and thermal perturba-tion,thermal IR spectroscopy,thermal gravimetric analysis and single-crystal X-ray diffraction.It crystallizes in triclinic,space group P with a = 12.981(3),b = 13.044(3),c = 14.208(3) ,α = 63.98(3),β = 77.17(3),γ = 14.208(3)°,V = 2001.0(8) 3,Z = 1,Mr = 2518.05,Dc = 2.090 g/cm-1,F(000) = 1255.0,Mu(mm-1) = 1.756,λ(MoKα) = 0.71073 ,R = 0.0625 and wR = 0.1952.In 1,the [V12B18O54(OH)6]8- units are connected by [Cu(en)2]2+,binuclear Na(1) and Na(2) to form a three-dimensional porous framework.
利用程序控温的水热合成法得到了两种含有2,2'-bipy及[M003]簇骼的化合物:[(2,2'-bipy)2(Mo03)3]。(工)和[(2,2'-bipy)(M003)]n(11)。为了阐明这两个化合物结构与谱学的关系,通过XRD、FT-IR、热微扰2D-IR相关光谱、TG分析、SEM、高温红外分析、uV_visDRS光谱和固体荧光光谱研究手段进行研究,进而探讨结构与性能的关系。其XRD说明了化合物I和Ⅱ是纯物相;FTIR的特征振动频率和热微扰2D-IR相关光谱的响应峰与化合物I和Ⅱ的结构解析相一致,2D-IR的同步和异步相关光谱图还确定了化合物I和Ⅱ的钼氧簇骼振动强度随升温变化的先后顺序与高温红外解析相一致;通过TG分析和高温红外分析研究化合物I和Ⅱ的热稳定性;化合物I和Ⅱ的UV Vis DRS光谱显示在225~350 nm有宽的紫外吸收谱带;化合物I和Ⅱ的固体荧光光谱分别在277和295nm的激发下得到的最强发射峰值分别为460和480nm。本文阐明了化合物I和Ⅱ的配位情况,揭示了价电子在分子中相应能级间跃迁的内在规律;还验证了弱相互作用力在配合物的结构框架中不但起稳定作用,而且在耐热性扮演重要的角色。