| 2-甲酰基呋喃苯乙酰腙及其Ni(Ⅱ)配合物的晶体结构及热化学性质 | |
| Crystal Structures and Thermochemical Properties of Phenyl-acetic Acid Furan-2-ylmethylene-hydrazide and Its Ni(Ⅱ) Complex | |
| 摘要: 以苯乙酸甲酯、水合肼和呋喃甲醛为原料,合成了配体2-甲酰基呋喃苯乙酰腙(H2L:C13H12N2O2),再与六水氯化镍反应,制得配合物Ni(HL)2 (1),并对配体及配合物进行了元素分析和X射线单晶衍射结构表征,结果表明,配体晶体属单斜晶系,P21/c空间群,晶胞参数为:a=1.161 9(3) nm,b=1.359 8(3) nm,c=0.792 16(19) nm,β=109.307(4)°;Ni(Ⅱ)配合物晶体属三斜晶系,P1空间群,晶胞参数为:a=0.455 70(14) nm,b=1.094 7(3) nm,c=1.204 8(4) nm,β=98.302(5)°。利用热重实验研究了H2L和1的热稳定性,并计算了各自热分解过程的表观活化能(Ea),发现配合物的热稳定性要远高于配体。采用微量热法研究了H2L及1与小牛胸腺DNA(CT-DNA)的相互作用,实验结果表明,配合物的作用焓值(ΔH)要大于配体的焓值,说明配合物与CT-DNA的作用要比配体与CT-DNA的作用更强。 | |
| 关键词: 酰腙 Ni(Ⅱ)配合物 晶体结构 热稳定性 微量热 | |
| 基金项目: 国家自然科学基金项目(No.21373158,21301139,21103135),陕西省教育厅科研计划项目(No.2013JK0651)资助。 | |
| Abstract: The Phenyl-acetic acid furan-2-ylmethylene-hydrazide (H2L: C13H12N2O2) was synthesized from methyl phenylacetate, hydrazine hydrate and furfural, and then reacted with nickel chloride hexahydrate to form a complex Ni(HL)2 (1). The structures of H2L and 1 were determined by X-ray single crystal diffraction and element analysis.The X-ray single crystal diffraction showed that the crystal of H2L belonged to monoclinic system, space group P21/c with a=1.161 9(3) nm, b=1.359 8(3) nm, c=0.792 16(19) nm, β=109.307(4)° and the crystal of the complex 1 belonged to triclinic system, space group P1 with a=0.455 70(14) nm, b=1.094 7(3) nm, c=1.204 8(4) nm, β=98.302(5)°. Thermal gravity analyses were used to investigate the thermal stabilities of H2L and 1, and the apparent activation energy (Ea) of the decompositions were also calculated, and the results indicated that the complex 1 was more thermal stable than the ligand H2L. The microcalorimetric method was used to study the interactions of H2L and the complex 1 with calf thymus DNA (CT-DNA), and the experimental results showed that the enthalpy change (ΔH) of the complex 1 was greater than that of the ligand H2L, indicating that the complex 1 displayed stronger interaction with CT-DNA than the ligand H2L. CCDC: 909434, H2L; 949203, 1. | |
| Keywords: acylhydrazone Ni(Ⅱ) complex crystal structure thermal stability microcalorimetry | |
| 投稿时间：2014-12-25 修订日期：2015-05-10 | |
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| 杨再文,丁作成,刘向荣,赵顺省,张润兰,杨水兰.2-甲酰基呋喃苯乙酰腙及其Ni(Ⅱ)配合物的晶体结构及热化学性质[J].无机化学学报,2015,31(8):1520-1528. | |
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