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Capturing the Precise Structure of Liquids: The Crystalline Sponge Method for an Undergraduate Laboratory Course
Journal of Chemical Education ( IF 2.5 ) Pub Date : 2023-12-08 , DOI: 10.1021/acs.jchemed.3c00714
Junxi Zou 1 , Xiaoyu Wang 1 , Xuan Liu 1 , Yuan Zheng 1 , Wei Shao 1 , Qing-Wei Zhang 1 , Pingping Zhu 1 , Lingling Li 1
Journal of Chemical Education ( IF 2.5 ) Pub Date : 2023-12-08 , DOI: 10.1021/acs.jchemed.3c00714
Junxi Zou 1 , Xiaoyu Wang 1 , Xuan Liu 1 , Yuan Zheng 1 , Wei Shao 1 , Qing-Wei Zhang 1 , Pingping Zhu 1 , Lingling Li 1
Affiliation
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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.
中文翻译:
捕捉液体的精确结构:本科生实验课程的结晶海绵法
结晶海绵方法可以直接、精确地测定液体和气体目标的分子结构,因此被认为是晶体学领域的革命性突破。为了让本科生接触这种尖端技术,我们开发了一个全面的实验室实验,其反应条件和表征系统地为学生量身定制,以温和且易于理解的方式进行。在本实验中,学生研究分别以苯甲腈、水杨酸甲酯和(三氟甲氧基)苯为溶剂,制备结晶海绵状网络络合物{[(ZnI 2 ) 3 ( TPT) 2 ]· x (溶剂化物)} n。将在苯甲腈中获得的结晶海绵暴露于环己烷中进行溶剂交换,得到{[(ZnI 2 ) 3 (TPT) 2 ]· x (环己烷)} n,并通过IR和GC-MS监测进展。所有四种晶体均在显微镜下进行评估并进行单晶 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,分层实验旨在为学生提供灵活性并最适合他们的个人需求和资源。该实验已在我校进行了三个学期。它可以刷新学生对晶体学的理解,并帮助他们在未来的工作中取得优异的成绩,特别是在合成化学、药物研发等方面。
更新日期:2023-12-08
中文翻译:
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捕捉液体的精确结构:本科生实验课程的结晶海绵法
结晶海绵方法可以直接、精确地测定液体和气体目标的分子结构,因此被认为是晶体学领域的革命性突破。为了让本科生接触这种尖端技术,我们开发了一个全面的实验室实验,其反应条件和表征系统地为学生量身定制,以温和且易于理解的方式进行。在本实验中,学生研究分别以苯甲腈、水杨酸甲酯和(三氟甲氧基)苯为溶剂,制备结晶海绵状网络络合物{[(ZnI 2 ) 3 ( TPT) 2 ]· x (溶剂化物)} n。将在苯甲腈中获得的结晶海绵暴露于环己烷中进行溶剂交换,得到{[(ZnI 2 ) 3 (TPT) 2 ]· x (环己烷)} n,并通过IR和GC-MS监测进展。所有四种晶体均在显微镜下进行评估并进行单晶 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,分层实验旨在为学生提供灵活性并最适合他们的个人需求和资源。该实验已在我校进行了三个学期。它可以刷新学生对晶体学的理解,并帮助他们在未来的工作中取得优异的成绩,特别是在合成化学、药物研发等方面。