| GUI: Olex2[1] Structure refinement: SHELXL[2] |
案例来源：CCDC[3] 2097152. Org.Lett. 2021, 23, 6455−6460.DOI[4]:10.1021/acs.orglett.1c02266. 案例结构如图1所示。 ▲图1 结构式 如图2所示，取代环己烯的诸多碳原子椭球形变严重，两个最大的残余峰与CHCH片段成交叉形分布。 ▲图2 椭球形变严重的取代环己烯片段 其实残余峰的分布以及椭球形变方向都提示了无序方案，设计的无序方案如图3所示。 ▲图3 无序方案 按照无序方案，对相关原子进行二组分无序处理，结果如图4所示。 ▲图4 无序处理结果 为保持结构稳定，添加了一些键长键角限制和各向异性位移参数限制，如图5所示。 ▲图5 限制指令 视频演示操作请参阅： 单晶结构解析练习184(数据还原-文献案例-无序处理)：https://www.bilibili.com/video/BV1Nn4xezEat 如需数据进行练习，请从以下链接下载： 提取码: drsv | [1] Dolomanov, O. V.; Bourhis, L. J.; Gildea, R. J.; Howard, J. A. K.; Puschmann, H. OLEX2: A Complete Structure Solution, Refinement and Analysis Program. J. Appl. Cryst. 2009, 42, 339–341. DOI: 10.1107/S0021889808042726. [2] (a) Sheldrick, G. M. SHELXL-2019/3, Program for Crystal Structure Refinement, University of Göttingen, Germany, 2019. (b) Sheldrick, G. M. A Short History of SHELX. Acta Cryst. 2008, A64, 112–122. DOI: 10.1107/S0108767307043930. (c) Sheldrick, G. M. Crystal Structure Refinement with SHELXL. Acta Cryst. 2015, C71, 3–8. DOI: 10.1107/S2053229614024218. (d) Lübben, J.; Wandtke, C. M.; Hübschle, C. B.; Ruf, M.; Sheldrick, G. M.; Dittrich, B. Aspherical scattering factors for SHELXL – model, implementation and application. Acta Cryst. 2019, A75, 50–62. DOI: 10.1107/S2053273318013840. [3] (a) Allen, F. H. The Cambridge Structural Database: a quarter of a million crystal structures and rising. Acta Cryst. 2002, B58, 380–388. DOI: 10.1107/S0108768102003890. (b) Allen, F. H. The Cambridge Structural Database: a quarter of a million crystal structures and rising. Acta Cryst. 2016, B72, 171–179. DOI: 10.1107/S2052520616003954. [4] (a) International Organization for Standardization (2012). ISO 26324:2012. Information and Documentation – Digital Object Identifier System. http://www.iso.org/iso/catalogue_detail.htm?csnumber=43506. (b) McDonald J. D.; Levine-Clark, M. Encyclopedia of Library and Information Sciences. Fourth Edition, CRC Press, 2017. DOI: 10.1081/e-elis4. (c) Liu, J. Digital Object Identifier (DOI) and DOI Services: An Overview. Libri 2021, 71, 349‒360. DOI: 10.1515/libri-2020-0018. (d) International Organization for Standardization (2022). ISO 26324:2022. Information and Documentation – Digital Object Identifier System. https://www.iso.org/standard/81599.html |
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