| 手性镝(III)-酒石酸配合物的合成、单晶转换及热稳定性研究 |
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| 引用本文： | 李丽,郑剑锋,赵明霞,冯思思.手性镝(III)-酒石酸配合物的合成、单晶转换及热稳定性研究[J].人工晶体学报,2021,50(1):106-112. |
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| 作者姓名： | 李丽 郑剑锋 赵明霞 冯思思 |
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| 作者单位： | 1.山西工程技术学院矿业工程系,阳泉 045000;2.山西大学分子科学研究所,化学生物学与分子工程教育部重点实验室,太原 030006 |
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| 基金项目： | 山西省高等学校科技创新项目(2019L0985) |
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| 摘 要： | 以2,3-二乙酰对甲苯-D-酒石酸(D-H2DTTA)为原料,与金属Dy(III)盐反应,经过单晶-单晶转换,得到一种新的酒石酸(H2tar)配合物Dy(Htar)3(H2O)3]n(1),对该配合物用元素分析、红外光谱、X-射线单晶衍射、粉末衍射以及差热-热重等进行了表征。晶体结构分析表明,配合物1属三方晶系,R3空间群,晶胞参数为a=b=2.723 16(14) nm,c=0.762 75(6) nm,α=β=90.00°,γ=120.00°,V=4.898 5 (6) nm3,Z=3, 剑桥晶体数据库(Cambridge Crystallographic Data Centre, CCDC)编号为1498504。配合物中的金属Dy3+分别与三个酒石酸离子配体Htar-上的六个氧原子和三个配位水分子上的三个氧原子配位,形成九配位三帽三棱柱构型。配合物1在c方向上通过O1和O5原子连接成一维链状结构,相邻Dy3+之间的距离为0.762 8(1) nm。配合物1是由Dy(HDTTA)3(CH3OH)3]n经单晶-单晶转换过程得到,其转换过程包括酯基水解及水分子取代两类反应。配合物1具有一定的热稳定性,45~166 ℃失去配位水分子,高于166 ℃配合物骨架坍塌。
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| 关 键 词： | 酒石酸 Dy(III)配合物 单晶-单晶转换 热稳定性 |
| 收稿时间： | 2020-09-09 |
Synthesis,Single Crystal Transformation and Thermal Stability of Chiral Dysprosium (III)-Tartaric Acid Complex |
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| LI Li,ZHENG Jianfeng,ZHAO Mingxia,FENG Sisi.Synthesis,Single Crystal Transformation and Thermal Stability of Chiral Dysprosium (III)-Tartaric Acid Complex[J].Journal of Synthetic Crystals,2021,50(1):106-112. |
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| Authors: | LI Li ZHENG Jianfeng ZHAO Mingxia FENG Sisi |
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| Affiliation: | 1. Department of Mining Engineering, Shanxi Institute of Technology, Yangquan 045000, China;2. Key Laboratory of Chemical Biology and Molecular Engineering of the Education Ministry, Institute of Molecular Science, Shanxi University, Taiyuan 030006, China |
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| Abstract: | The new complex Dy(Htar)3(H2O)3]n(1) was synthesized by the single crystal to single crystal transformation method using(+)-di-p-toluoyl-D-tartaric acid (D-H2DTTA) as raw material and reaction with mentalic Dy(III) salt. The complex was characterized by elemental analysis, IR spectroscopy, single crystal X-ray diffraction, powder X-ray diffraction analysis and thermogravimetric analysis and differential thermal analysis(TGA-DTA). The results of X-ray crystallographic analysis indicate that complex 1 belongs to trigonal system, space group R3 with a=b=2.723 16(14) nm, c=0.762 75(6) nm, α=β=90.00°, γ=120.00°, V=4.898 5 (6) nm3, Z=3, and Cambridge Crystallographic Data Centre (CCDC) number is 1498504. Each Dy3+ is surrounded by six O atoms from three Htar- ligands and three O atoms from three coordinated water molecules, forming a tricapped trigonal prism geometry with nine coordination property. Complex 1 exhibits an infinite one dimensional chain structure connected by O1 and O5 along c axis, with the Dy…Dy distance of 0.762 8(1) nm. Complex 1 was obtained through single crystal to single crystal transformation process from Dy(HDTTA)3(CH3OH)3]n, which includes ester hydrolysis and water molecules substitution two reactions. Complex 1 has a certain thermal stability. After taking off the coordinated water molecules in the range of 45~166 ℃, the skeleton of 1 begins to collapse with increasing temperature above 166 ℃. |
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| Keywords: | tartaric acid Dy(III) complex single crystal to single crystal transformation thermal stability |
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