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机构地区:[1]南京化工职业技术学院应用化学系,江苏南京210048
出 处:《实验室研究与探索》2014年第6期69-71,102,共4页Research and Exploration In Laboratory
摘 要:正丁胺盐酸盐、冠醚(18C6)和氯化锌在甲醇溶液中常温反应得到一种新颖的冠醚超分子包合物。该化合物为一种有机无机金属盐,其分子内通过正丁胺冠醚季铵盐与三氯一水合锌阴离子达到电荷平衡。晶体学分析该化合物属于手性正交空间群(P212121),其晶胞参数为a=85.73(6)nm,b=165.0l(11)nm,C=182.85(12)nm,V=25870(3)nm^3,α=β=γ=90.0。和Z=4(293(2)K)。该包合物中氯化锌阴离子的配位方式很特别,其中有一份子的中性水分子与中心原子锌原子配位形成了三氯一水合锌离子,阴离子通过0-H…Cl氢键形成一维彩带(梯状)堆积结构。利用红外、粉末XRD确认单晶结构与粉末结构为同一物质。通过对其粉末进行压片测试变温介电性质,表明其没有明显的介电变化,该测试结果说明了在-180~423K测试温度变化范围内没有发生相变。热力学分析证实该分子能在自然界中稳定存在,也就说明了三氯一水合锌离子能够在室温下稳定存在。The reaction of propane butan-l-amine hydrochloride, 18-crown-6 and divalence zincic chloride in methanol solution yields an unusual supramolecular structure. The butan-l-amine cation sits on the cavity of 18-crown-6, and forms a [ (C4H12 N ) (18-crown-6)] ^+ supramolecular cation structure, which is introduced as the counter cation of (ZnOCL3H2) - anions. It is interesting that the coordination mode of the anion is very special. The stacks are fused into pseudo-sheets by way of the O-H ... C1 hydrogen bonds, which are established between discrete tetrahedral aqua- trichloro-zincate(II) anions and result in a novel one-dimensional ribbon-like structure. IR and X-ray powder diffraction (XRD) spectroscopy and mass spectrometry confirm its formation. Temperature- and frequency-dependent dielectric constant of compound 1 are measured and show no distinct dielectric anomaly, which suggests no phase transition within the measured temperature range (-180-423 K). Thermogravimetric analysis confirms the molecules can exist stably. In other words , the anions can exist stably.
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