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[1]胡学雷,姚瑜,肖莉,等.双酚大环双核锰配合物的合成及其晶体结构[J].武汉工程大学学报,2013,(06):7-11.[doi:103969/jissn16742869201306002]
　HU Xue lei,YAO Yu,XIAO Li,et al.Crystal structure and characterization of new binuclear manganese(II)complex based on polyaza imino macrocyclic ligand[J].Journal of Wuhan Institute of Technology,2013,(06):7-11.[doi:103969/jissn16742869201306002]
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双酚大环双核锰配合物的合成及其晶体结构(/HTML)
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《武汉工程大学学报》[ISSN:1674-2869/CN:42-1779/TQ]

卷:
期数:
2013年06期
页码:
7-11
栏目:
化学与化学工程
出版日期:
2013-06-30

文章信息/Info

Title:
Crystal structure and characterization of new binuclear manganese(II)complex based on polyaza imino macrocyclic ligand
文章编号:
16742869(2013)06000705
作者:
胡学雷; 姚瑜; 肖莉; 孟美娜; 潘志权
武汉工程大学化工与制药工程学院，绿色化工过程教育部重点实验室，湖北省新型反应器与绿色化学工艺重点实验室，湖北 武汉 430074
Author(s):
HU Xuelei;  YAO Yu;  XIAO Li;  MENG Meina; PAN Zhiquan
School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Key Laboratory for Green Chemical Processof Ministry of Education, Hubei Key Laboratory of Novel Reactor and Green Chemical Technology,Wuhan 430074,China
关键词:
大环双核锰配合物; 合成; 晶体结构; 电喷雾质谱
Keywords:
macrocyclic binuclear manganese complex; synthese; crystal structure; electrospraymass spectrometry
分类号:
O641
DOI:
103969/jissn16742869201306002
文献标志码:
A
摘要:
为了进一步考察模板法合成双酚大环过渡金属配合物的最佳反应条件和形成的双核配合物的结构特征，以1,3-丙二胺、2,6-二甲酰基对甲苯酚、二氯化锰为原料通过\[2+2\] 模板缩合反应合成了一个新的双酚多氮亚胺大环双核锰配合物，通过红外光谱、电喷雾质谱对其性质进行了表征，用X射线晶体结构分析研究了其晶体结构.晶体结构分析研究表明配合物属单斜晶系，空间群为P2(1)/c，晶胞参数为a=0.749 44(8)纳米, b=1.045 84(11)纳米,c=1.636 57(18)纳米,β=93.854(2)°, Mr=583.27,V=1.279 8(2)立方纳米,Z=2,Dc=1.514 克/立方厘米, F(000)=596,R=0.039 7和wR=0.111 2.目标配合物由一个失去两个酚基氢离子的大环配体、两个锰离子和两个氯离子组成，每个锰离子分别位于分室大环配体各一侧，呈五配位四方锥构型，其中在一侧的两个亚胺氮原子和两个酚基氧原子组成四方锥的底平面，而氯离子位于四方锥的顶点位置.晶体结构分析和电喷雾质谱均证明了双核实体的存在和目标双核配合物具有较高的稳定性.
Abstract:
With the aim of finding the best conditions for the synthesis of binuclear macrocyclic complexes by the template reaction and better understanding their structures, the title compound， a new binuclear manganese (II) complex based on a polyaza imino macrocyclic ligand was prepared by\[2+2\] template condensation of 1,3diaminopropane with 2,6diformyl4methylphenol in the presence of manganese(II) chloride, and characterized by infrared spectra, and electrospray mass spectra. Its crystal and molecular structure was determined by Xray diffraction methods. The crystal crystallizes in the monoclinic system, space group P2 (1)/c with a = 0.749 44(8) nm, b=1.045 84(11) nm, c=1.636 57(18) nm, β = 93.854(2)°, Mr = 583.27, V = 1.279 8(2) nm3, Z = 2, Dc = 1.514 g/cm3, F(000) = 596, R = 0.039 7 and wR = 0.111 2. The complex is composed of a dihydrogen deposed polyaza imino macrocyclic ligand, two manganese (II) ions and two chlorides. Each manganese ion is located in one of the two compartments of the macrocyclic ligand and fivecoordinated in a square pyramidal geometry in which two oxygen and two nitrogen atoms of macrocycle build the basal plane of the pyramid, and the chloride ion is located at the top of the pyramid. Study of Xray diffraction methods and electrospraymass spectrometry confirms that the binuclear entity exists in the complex and the title complex is very stable.

参考文献/References:

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备注/Memo

备注/Memo:
收稿日期：20130417基金项目：湖北省自然科学基金重点项目（2011CDA048）作者简介：胡学雷（1967）, 男，湖北黄冈人，教授，博士，硕士研究生导师.研究方向：配位化学和药物合成.
更新日期/Last Update: 2013-07-11