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首页> 美国卫生研究院文献>Wiley-Blackwell Online Open >Halometallate Complexes of Germanium(II) and (IV): Probing the Role of Cation Oxidation State and Halide on the Structural and Electrochemical Properties
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Halometallate Complexes of Germanium(II) and (IV): Probing the Role of Cation Oxidation State and Halide on the Structural and Electrochemical Properties

机译：锗（II）和（IV）的卤代金属盐配合物：探讨阳离子氧化态和卤化物对结构和电化学性质的作用

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The GeIV chlorometallate complexes, [EMIM]2[GeCl6], [EDMIM]2[GeCl6] and [PYRR]2[GeCl6] (EMIM=1-ethyl-3-methylimidazolium; EDMIM=2,3-dimethyl-1-ethylimidazolium; PYRR=N-butyl-N-methylpyrrolidinium) have been synthesised and fully characterised; the first two also by single-crystal X-ray diffraction. The imidazolium chlorometallates exhibited significant C–H⋅⋅⋅Cl hydrogen bonds, resulting in extended supramolecular assemblies in the solid state. Solution 1H NMR data also showed cation–anion association. The synthesis and characterisation of GeII halometallate salts [EMIM][GeX3] (X=Cl, Br, I) and [PYRR][GeCl3], including single-crystal X-ray analyses for the homologous series of imidazolium salts, are reported. In these complexes, the intermolecular interactions are much weaker in the solid state and they appear not to be significantly associated in solution. Cyclic-voltammetry experiments on the GeIV species in CH2Cl2 solution showed two distinct, irreversible reduction waves attributed to GeIV–GeII and GeII–Ge0, whereas the GeII species exhibited one irreversible reduction wave. The potential for the GeII–Ge0 reduction was unaffected by changing the cation, although altering the oxidation state of the precursor from GeIV to GeII does have an effect; for a given cation, reduction from the [GeCl3]− salts occurred at a less cathodic potential. The nature of the halide co-ligand also has a marked influence on the reduction potential for the GeII–Ge0 couple, such that the reduction potentials for the [GeX3]− salts become significantly less cathodic when the halide (X) is changed Cl→Br→I.
机译：Ge IV 金属氯酸盐配合物[EMIM] 2 [GeCl6]，[EDMIM] 2 [GeCl6]和[PYRR] 2 [GeCl6]（EMIM = 1-乙基-3-甲基咪唑; EDMIM = 2合成了3-（3-二甲基-1-乙基咪唑鎓； PYRR ＝ N-丁基-N-甲基吡咯烷鎓），并对其进行了充分表征。前两个还通过单晶X射线衍射。咪唑鎓氯金属盐显示出显着的C–H⋅·⋅Cl氢键，从而导致固态的超分子组装扩展。溶液 1 1 H NMR数据也显示阳离子-阴离子缔合。 Ge II 卤代金属盐[EMIM] [GeX3]（X = Cl，Br，I）和[PYRR] [GeCl3]的合成和表征，包括单晶X射线分析报道了一系列咪唑鎓盐。在这些配合物中，分子间的相互作用在固态时要弱得多，它们在溶液中似乎没有明显的联系。在CH2Cl2溶液中的Ge IV 种类的循环伏安法实验显示，归因于Ge IV –Ge II 和Ge < sup> II –Ge 0 ，而Ge II 物种表现出一个不可逆的还原波。尽管改变了前体从Ge IV 到的氧化态，但改变阳离子不会影响Ge II –Ge 0 还原的电势。 Ge II 确实有作用；对于给定的阳离子，[GeCl3] -盐的还原在较低的阴极电位下发生。卤化物配体的性质也对Ge II –Ge 0 对的还原电位有显着影响，从而[GeX3]的还原电位当卤化物（X）变为Cl→Br→I时，-盐的阴极显着减少。

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