基于Ni(mnt)_2离子对配合物的合成及其晶体结构

Synthesis and Crystal Structure of a Novel Ion-pair Complex Based on Ni(mnt)_2 Ion

以2-(3'-吡啶基)-4,4,5,5-四甲基咪唑啉-1-氧基自由基和碘甲烷在THF中回流反应制得阳离子配体{[H3CPy Mz OHOCH3]2+(2),H3CPy Mz OHOCH3=3-(1-羟基-3-氧甲基-4,4,5,5-四甲基)咪唑基-1-甲基吡啶};2与K2Ni(mnt)2在乙腈中反应合成了一个新的阴阳离子对配合物{[Ni(mnt)2](H3CPy Mz OHOCH3)2·CH3CN·I2(1),mnt=丁二腈烯二硫醇阴离子},其结构经IR,元素分析和X-射线单晶衍射表征。1(CCDC:846 605)属单斜晶系,空间群P21/c,晶胞参数a=20.612(4),b=7.188 6(14),c=18.309(4),β=107.15(3)°,V=2 592.4(9)3,Z=2。1中阴阳离子分别形成完全分立的柱状堆积结构,在阴离子堆积柱内,Ni(Ⅱ)形成了均匀的一维链。

The cationic ligand{ [H3CPy Mz OHOCH3]2 ＋（2）,[H3CPy Mz OHOCH3]=[3-（1-hydroxyl-3-methoxyl-4,4,5,5-tetramethyl） midazol-1-methylpyridinium]} was prepared by reflux of 2-（3＇-pyridyl）-4,4,5,5-tetramethyl-imidazoline-1-oxyl with methyl iodide in THF. A novel ion-pair complex{ [Ni（mnt）2]（H3 CPy Mz OHOCH3）2·CH3CN·I2（1）,mnt = maleonitriledithiolate} was synthesized by reaction of 2 with K2Ni（mnt）2in acetonitrile. The structure was characterized by IR,elemental analysis and X-ray single crystal diffraction. 1（CCDC： 846 605） belongs to monoclinic system,space group P21/ c with a = 20. 612（4） ,b = 7. 188 6（14） ,c = 18. 309（4） ,β = 107. 15（3） °,V = 2 592. 4（9） 3,Z = 2. The anions and cations of 1 form completely segregated stacking columns in the solid state,and the [Ni（mnt）2]2-form uniform 1D linear chain.