无序示例-吲哚环二重无序

DJ_Tokyo

相关软件或概念：Olex2[1] (Version: Olex2-1.5); SHELXL[2] (Version: SHELXL-2019/3); PLATON[3] (Version: 60124)

案例结构信息：CCDC2338985, DOI: 10.5517/ccdc.csd.cc2jhx43. (合成文献：Inorg.Chem. 2013,52, 9549–9556. DOI: 10.1021/ic401515q.)

该结构中吲哚环的苯环碳原子椭球拉长形变——其实整个吲哚环中距离吲哚2-位碳原子越远的原子其椭球形变越严重，而其形变方向皆为绕吲哚2-位碳原子的圆弧形，如图1所示。

▲图1 吲哚环原子形变情况

这种情况可以考虑对吲哚环原子做绕吲哚2-位碳原子在吲哚环平面内旋转的二重无序处理，如图2所示，R1从4.89%降为4.72%，wR2从12.09%降为11.50%，两个组分的原子椭球较无序处理之前更加合理。

▲图2 吲哚环二重无序处理结果

相关视频请参阅：

单晶结构解析练习84(数据还原)：https://www.bilibili.com/video/BV1pJ4m1h7gt

参考文献

[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.

[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 ofSHELX. Acta Cryst. 2008, A64, 112–122. (c) Sheldrick, G. M.Crystal structure refinement with SHELXL.Acta Cryst. 2015, C71, 3–8. (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.

[3] (a) Spek, A. L. Single-crystal structure validationwith the program PLATON. J. Appl.Cryst. 2003, 36, 7–13. (b) Spek,A. L. Structure validation in chemical crystallography. Acta Cryst. 2009, D65, 148–155. (c) Spek, A. L. What makes a crystal structure reportvalid? Inorg. Chim. Acta 2018, 470, 232–237. (d) Spek, A. L. checkCIFvalidation ALERTS: what they mean and how to respond. Acta Cryst. 2020, E76, 1–11.

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