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化学学报
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化学学报 ›› 2010, Vol. 68 ›› Issue (06): 487-492. 上一篇    下一篇

研究论文

混价四核铜(I/II)配合物[Cu2L2][Cu(pht)2]2的合成、晶体结构及性质研究

胡喜兰1，施鹏飞1，许兴友*,1,2，尹福军1，杨芹1，王大奇3   

  1. (1淮海工学院配位化学研究所 连云港 222005)
    (2淮阴工学院生命科学与化学工程学院 淮安 223003)
    (3聊城大学化学化工学院 聊城 252059)
  • 投稿日期:2009-08-28 修回日期:2009-10-10 发布日期:2010-03-28
  • 通讯作者: 胡喜兰 E-mail:huxilan@hhit.edu.cn

Synthesis, Structure and Property of Mixed-valence Tetranuclear Copper Complex [Cu2L2]•[Cu(pht)2]2

Hu Xilan1 Shi Pengfei1 Xu Xingyou*,1,2 Yin Fujun1 Yang Qin1 Wang Daqi3   

  1. (1 Research Section of Coordination Chemistry, Huaihai Institute of Technology, Lianyungang 222005)
    (2 School of Life Scientific and Chemical Engineering, Huaiyin Institute of Technology, Huai an 223003)
    (3 College of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059)
  • Received:2009-08-28 Revised:2009-10-10 Published:2010-03-28
  • Contact: Hu Xi-Lan E-mail:huxilan@hhit.edu.cn

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报道四核铜配合物[Cu2L2][Cu(pht)2]2 [Hpht: 苯妥英, 即5,5-二苯基-2,2咪唑烷酮; L: N-(3-氨基丙基)二乙醇胺]的溶剂热合成、晶体结构及其性质研究. 该晶体属单斜晶系, P21/n空间群, 晶胞参数: a＝0.9240(1) nm, b＝2.4559(2) nm, c＝1.5572(2) nm, β＝97.489(2)o, V＝3.5035(7) nm3, Dc＝1.499 Mg/m3 (g/cm3), Z＝2, F(000)＝1636, μ＝1.270 mm－1, R1＝0.0503, wR2＝0.1135 [I＞2σ(I)], GOF＝1.014. XPS结合X射线单晶结构分析, 表明该配合物分子有混价铜组成, 包括两个Cu(I)和两个Cu(II), 其中每个Cu(I)分别与两个苯妥英配体提供的氮原子配位, N—Cu(I)—N的夹角为177.1°, 每个Cu(II)与L配体的五个配位原子配位(N2O3), 形成一个稍变形四方锥结构, 两个Cu(II)通过N-(3-氨基丙基)二乙醇胺中的一个羟基氧桥连接形成双核阳离子, 琼脂扩散法测试结果表明配合物、配体和铜盐对3种受试细菌均有一定的活性. 配合物与DNA的相互作用测定研究表明, 该配合物是以插入方式与小牛胸腺DNA结合.

关键词: 铜(I/II)配合物, 合成, 晶体结构, 性质研究

The title complex [CuL2]•[Cu(pht)2]2 (Hpht＝5,5-diphenylhydantoin, i.e. phenytoin; L＝N-(3-aminopropyl)diethanolamine) has been synthesized solvent-thermally and characterized by elemental analysis, IR, TG-DSC and single-crystal X-ray diffraction. The crystal of the copper complex belongs to monoclinic system with space group P21/n, a＝0.9240(1) nm, b＝2.4559(2) nm, c＝1.5572(2) nm, α＝γ＝90°, β＝97.489(2)°, V＝3.5035(7) nm3, Dc＝1.499 Mg/m3 (g/cm3), Z＝2, F(000)＝1636, μ＝1.270 mm－1, R1＝0.0503, wR2＝0.1135 [I＞2σ(I)] and GOF＝1.014. The XPS and single-crystal X-ray diffraction data demonstrated that the complex is a mixed valence one, including two Cu(I) and two Cu(II) metal centers. The Cu(I) atom is coordinated by two nitrogen atoms from two phenytoin ligands, and the angle of N—Cu(I)—N was 177.1°. The Cu(II) atom adopts a distorted CuN2O3 square-pyramidal configuration when coordinated with two L ligands, dinuclear cation is constructed by the connection of Cu(II) and O atoms from the bridging hydroxyl groups of L. The complex was valued for its antimicrobial activity by diffusion test in vitro. It was found to be active against the three test bacterial organisms. The interaction between the complex and CT-DNA was studied by UV spectroscopy, fluorescence spectroscopy and viscosity measurements, which confirmed the intercalation of the complex into DNA double helixes.

Key words: copper(I/II) complex, synthesis, crystal structure, property

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