Junxi Zou, Xiaoyu Wang, Xuan Liu, Yuan Zheng, Wei Shao, Qing-Wei Zhang*, Pingping Zhu* and Lingling Li*,
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引用次数: 0
摘要
晶体海绵法可以直接精确地测定液态和气态目标物的分子结构,因此被认为是晶体学领域的革命性突破。为了让本科生接触到这一前沿技术,我们开发了一个综合实验室实验,其中的反应条件和表征系统地为学生量身定做,以一种温和、易于接受的方式进行。在本实验中,学生们分别以苯腈、水杨酸甲酯和(三氟甲氧基)苯为溶剂,研究网络状配合物{[(ZnI2)3(TPT)2]-x(solvate)}n结晶海绵的制备。在苯甲腈中得到的晶体海绵在环己烷中进行溶剂交换,得到{[(ZnI2)3(TPT)2]-x(环己烷)}n,并通过红外光谱和气相色谱-质谱监测其进展。所有四种晶体都在显微镜下进行了评估,并进行了单晶 X 射线衍射 (SC-XRD) 分析。学生有机会学习 SHELX、Olex2 和 Mercury 等科学软件,并对海绵和液体分子进行结构分析和可视化表示。此外,分层实验的设计为学生提供了灵活性,最适合他们的个人需求和资源。该实验已在我校开展了三个学期。它可以加深学生对晶体学的理解,帮助他们在未来的工作中,特别是在合成化学、药物研发等方面取得优异成绩。
Capturing the Precise Structure of Liquids: The Crystalline Sponge Method for an Undergraduate Laboratory Course
The crystalline sponge method allows for direct and precise molecular structure determination of liquid and gaseous targets and thus has been recognized as a revolutionary breakthrough in crystallography. To expose undergraduates to this cutting-edge technique, we have developed a comprehensive laboratory experiment with reaction conditions and characterizations systematically tailored for students to perform in a mild and accessible way. In this experiment, students investigate the preparation of networked complexes {[(ZnI2)3(TPT)2]·x(solvate)}n as crystalline sponges with benzonitrile, methyl salicylate, and (trifluoromethyoxy)benzene as solvent, respectively. Crystalline sponges obtained in benzonitrile were exposed to solvent exchange in cyclohexane to afford {[(ZnI2)3(TPT)2]·x(cyclohexane)}n, and the progress was monitored by IR and GC-MS. All four crystals were evaluated under a microscope and subjected to single crystal X-ray diffraction (SC-XRD) analysis. The students are provided with the opportunity to learn about scientific software, such as SHELX, Olex2, and Mercury, and carry out structure analysis and visual representation of the sponges and liquid molecules. Moreover, hierarchical experiments have been designed to provide flexibility to students and best fit their individual needs and resources. The experiment has been carried out for three semesters in our school. It may refresh students’ understanding of crystallography and help them excel in future endeavors especially like synthetic chemistry, pharmaceutical R&D, etc.
期刊介绍:
The Journal of Chemical Education is the official journal of the Division of Chemical Education of the American Chemical Society, co-published with the American Chemical Society Publications Division. Launched in 1924, the Journal of Chemical Education is the world’s premier chemical education journal. The Journal publishes peer-reviewed articles and related information as a resource to those in the field of chemical education and to those institutions that serve them. JCE typically addresses chemical content, activities, laboratory experiments, instructional methods, and pedagogies. The Journal serves as a means of communication among people across the world who are interested in the teaching and learning of chemistry. This includes instructors of chemistry from middle school through graduate school, professional staff who support these teaching activities, as well as some scientists in commerce, industry, and government.