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Efficient End-Capping Synthesis of Neutral Donor-Acceptor [2]Rotaxanes Under Additive-Free and Mild Conditions

机译:无添加剂和温和条件下中性给体-受体[2]轮烷的高效封端合成

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摘要

Control over phase stabilities during synthesis processes is of great importance for both fundamental studies and practical applications. We describe herein a facile strategy for the synthesis of Cu2Se with phase selectivity through a simple solvothermal method. In the presence and absence of SbCl3, monoclinic -Cu2Se and cubic -Cu2Se can be synthesized, respectively. The formation of -Cu2Se requires optimization of the Cu/Se molar ratio in the starting reagents, the reaction temperature, as well as the timing for the addition of SbCl3. Differential scanning calorimetry of the synthesized -Cu2Se has shown that a part of it undergoes a phase transition to -Cu2Se at 135 degrees C, and that this phase transition is irreversible on cooling to ambient temperature. Kinetic studies have revealed that in the presence of Sb species the kinetically favored -Cu2Se transforms to the thermodynamically favored -Cu2Se. In this -to- phase transition process, the distribution of Cu ions in -Cu2Se, as determined by the Cu/Se ratio and temperature, is likely to play a crucial role.
机译:合成过程中相稳定性的控制对于基础研究和实际应用都非常重要。我们在这里描述了一种通过简单的溶剂热法合成具有选择性的Cu2Se的简便策略。在存在和不存在SbCl3的情况下,可以分别合成单斜晶-Cu2Se和立方晶-Cu2Se。 -Cu2Se的形成需要优化起始试剂中的Cu / Se摩尔比,反应温度以及添加SbCl3的时间。合成的-Cu2Se的差示扫描量热法显示,一部分-Cu2Se在135摄氏度时经历了向-Cu2Se的相变,并且该相变在冷却至环境温度时不可逆。动力学研究表明,在存在Sb的情况下,动力学上受支持的-Cu2Se转变为热力学上受支持的-Cu2Se。在此相变过程中,由Cu / Se之比和温度确定的-Cu2Se中Cu离子的分布可能起关键作用。

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