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化学学报
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化学学报 ›› 2005, Vol. 63 ›› Issue (19): 1795-1801. 上一篇    下一篇

研究论文

(H2teta)2{[Ni(teta)][Fe(CN)6]2}•17H2O (teta＝5,7,7,12,14,14-Hexa-methyl-1,4,8,11-tetraazacyclotetradecane)超分子化合物的合成、晶体结构和磁性质研究

袁爱华*,1，沈小平2，周虎1，陆路德3   

  1. (1江苏科技大学材料科学与工程学院 镇江 212003)
    (2江苏大学化学化工学院 镇江 212013)
    (3南京理工大学材料化学实验室 南京 210094)
  • 投稿日期:2005-02-18 修回日期:2005-06-08 发布日期:2010-12-10
  • 通讯作者: 袁爱华

Synthesis, Crystal Structure and Magnetic Property of a Supermolecule (H2teta)2{[Ni(teta)][Fe(CN)6]2}•17H2O (teta＝5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecan

YUAN Ai-Hua*,1, SHEN Xiao-Ping2, ZHOU Hu1, LU Lu-De3   

  1. (1 School of Material Science and Engineering, Jiangsu University of Science and Technology, Zhenjiang 212003)
    (2 School of Chemistry and Chemical Engineering, Jiangsu Univer-sity, Zhenjiang 212013)
    (3 Material Chemistry Laboratory, Nanjing University of Science and Technology, Nanjing 210094)
  • Received:2005-02-18 Revised:2005-06-08 Published:2010-12-10
  • Contact: YUAN Ai-Hua

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将Ni(teta)(ClO4)2 (teta＝5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)的DMF溶液和K3[Fe(CN)6]的水溶液在填充了琼脂冻胶的U型管中通过扩散反应, 得到了标题化合物(H2teta)2{[Ni(teta)][Fe(CN)6]2}•17H2O, 该化合物晶体属三斜晶系, 空间群P1, 晶胞参数为a＝0.9998(2) nm, b＝1.5514(3) nm, c＝1.6647(4) nm, α＝114.15(2)°, β＝100.91(2)°, γ＝93.42(2)°, V＝2.2863(10) nm3, z＝1, Dc＝1.196 g•cm－3, F(000)＝890, μ＝5.84 cm－1, GOF＝0.894, R1＝0.0582, wR2＝0.1446 [I＞2σ(I)]. 该化合物的基本单元由2个[H2teta]2＋阳离子、1个{[Ni(teta)][Fe(CN)6]2}4－阴离子和17个水分子组成, 它们之间通过N—H…N氢键而形成具有二维平面结构的超分子化合物. 1.8～300 K变温磁化率研究表明, 化合物中三核体系Fe (s＝1/2)-Ni (s＝1)-Fe (s＝1/2)中心原子间通过氰基桥联而发生强的铁磁相互作用, 磁参数J＝4.33 cm－1, g＝2.6, θ＝60 K. 通过TG-DTG测定了配合物的热稳定性.

关键词: [Ni(teta)]2＋, 氰基桥联, 超分子化合物, 晶体结构, 磁性质

The title compound (H2teta)2{[Ni(teta)][Fe(CN)6]2}•17H2O was obtained by slow diffusion of an aqueous solution of K3[Fe(CN)6] and a DMF solu-tion of [Ni(teta)](ClO4)2 through a U-tube containing agar at room temperature. The compound crystallizes in the triclinic space group P1 with a＝0.9998(2) nm, b＝1.5514(3) nm, c＝1.6647(4) nm, α＝114.15(2)°, β＝100.91(2)°, γ＝93.42(2)°, V＝2.2863(10) nm3, z＝1, Dc＝1.196 g•cm－3, F(000)＝890, μ＝5.84 cm－1, GOF＝0.894, R1＝0.0582, wR2＝0.1446 [I＞2σ(I)]. Its structure con-sists of two cations of [H2teta]2＋, one trinuclear anion of {[Ni(teta)][Fe(CN)6]2}4－ and seventeen water molecules, which are held together by the N—H…N hydrogen bonds to form a two-dimensional supramolecule. The variable temperature magnetic susceptibility, measured in the 1.8～300 K range, indicates the presence of a strong ferromagnetic interaction through the cyanide bridge in trinuclear system Fe (s＝1/2)-Ni (s＝1)-Fe (s＝1/2) with magnetic parameters J＝4.33 cm－1, g＝2.6, θ＝60 K. The thermal stability of the complex was studied by TG-DTG.

Key words: [Ni(teta)]2＋, cyano-bridged, supramolecule, crystal structure, magnetic property