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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >The physical properties and unusual pyrolysis behaviour of a supramolecular complex of β-cyclodextrin and potassium ferrioxalate
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The physical properties and unusual pyrolysis behaviour of a supramolecular complex of β-cyclodextrin and potassium ferrioxalate

机译：β-环糊精与亚铁酸钾的超分子复合物的物理性质和异常的热解行为

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摘要

The thermal pyrolysis behaviour of a complex of β-cyclodextrin (CD) and potassium ferrioxalate (PF) was analyzed using gas chromatography coupled to time-of-flight mass spectrometry. Two rare inorganic ions: CO _2 ~(2+) and O _4 ~+, neither of which was found in the cases of free β-CD and PF, were synchronously observed during the decomposition of the complex. Our observations led to proposed formation mechanisms of the ions, in which the structural transformation of a metastable intermediate ion (C _2H _4O _3 ~+) was employed to qualitatively explain our data. Besides this, the formation, structure and magnetic properties of the complex were evaluated carefully. First, XPS analysis indicates a decrease of electron densities of Fe(iii) ions in the presence of β-CD. We think that this is due to an effect of the noncovalent complexation between PF and β-CD. This gives an indication on the effect of second sphere coordination of β-CD on the electronic structure of the Fe(iii) in the first coordination sphere. Second, structural changes in stacking modes and morphologies provide further support for the noncovalent complexation. For example, the surface feature of the complex gives us an impression that both β-CD and PF are evenly dispersed with each other. Also, the complex presents a uniform sponge-like porous nanostructure with diameters of less than 50 nm. This seems to be an important reason for those changes that occurred in the thermal analysis. Finally, the result of magnetic experiments implies that the coordination compound PF upon complexation with β-CD will experience a gradual decrease in magnetization with the increase of magnetic fields. These observations have significant implications for a better understanding of the importance of the construction and deconstruction of a second sphere coordination in modifying the physical properties of an σ-coordination compound.
机译：使用气相色谱-飞行时间质谱法分析了β-环糊精（CD）和亚铁酸钾（PF）的复合物的热解行为。在复合物分解过程中，同步观察到两种稀有无机离子：CO _2〜（2+）和O _4〜+，在游离β-CD和PF的情况下均未发现。我们的观察导致提出了离子的形成机理，其中使用了亚稳态中间离子（C _2H _4O _3〜+）的结构转化来定性地解释我们的数据。除此之外，还仔细评估了复合物的形成，结构和磁性。首先，XPS分析表明在存在β-CD的情况下Fe（i​​ii）离子的电子密度降低。我们认为这是由于PF和β-CD之间的非共价复合作用所致。这表明了β-CD的第二球配位对第一配位球中Fe（iii）电子结构的影响。其次，堆叠模式和形态的结构变化为非共价复合提供了进一步的支持。例如，配合物的表面特征给我们的印象是β-CD和PF彼此均匀分散。而且，该复合物呈现出直径小于50nm的均匀的海绵状多孔纳米结构。这似乎是热分析中发生这些变化的重要原因。最后，磁性实验的结果表明，配位化合物PF与β-CD络合后，随着磁场的增加，其磁化强度将逐渐降低。这些观察结果对更好地理解构造和解构第二球配位在修改σ配位化合物的物理性质中的重要性具有重要意义。

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