晶体数据还原示例48(孪晶拆分-奇怪残余峰触发B级警报PLAT094和PLAT097)

DJ_Tokyo

晶体数据还原示例48(孪晶拆分-奇怪残余峰触发B级警报PLAT094和PLAT097)

案例来源：CCDC[1] 2348820. Chem. Sci. 2024, 15, 20315‒20327.DOI[2]: 10.1039/d4sc04197f.

案例结构如图1所示（由ChemBioDraw[3]绘制）。

▲图1 案例结构

正常还原解析后，在结构片段附近有很大的残余峰，如图2所示（由Olex2[4]呈现）。

▲图2 结构片段附近残余峰

Max Peak高达7.2，由此触发了两个B级警报PALT094（参阅推文“CheckCIF-PLAT094”）和PLAT097（参阅推文“CheckCIF-PLAT097”），如图3所示。

▲图3 B级警报

于是按照推文“APEX4孪晶拆分步骤”方法用APEX4[5]对其做了孪晶拆分处理，使用HKLF4格式文件精修，其Max Peak为1.6，如图4所示，而使用HKLF5格式文件精修，则Max Peak为1.3，并且R因子更低，如图5所示。

▲图4 孪晶拆分-HKLF4格式文件精修结果

▲图5 孪晶拆分-HKLF5格式文件精修结果

视频讲解和操作演示请参阅：

单晶结构解析练习494(文献案例-数据还原-孪晶拆分)：https://www.bilibili.com/video/BV1ppPPeEEHY

如需数据进行练习，请从以下链接下载：

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参考文献

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[2]    (a) InternationalOrganization 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 Libraryand Information Sciences. Fourth Edition, CRC Press, 2017. DOI: 10.1081/e-elis4. (c) Liu, J. Digital ObjectIdentifier (DOI) and DOI Services: An Overview. Libri 2021, 71, 349‒360. DOI:10.1515/libri-2020-0018. (d) International Organization forStandardization (2022). ISO 26324:2022. Informationand Documentation – Digital Object Identifier System.https://www.iso.org/standard/81599.html

[3]    (a) Klein, F. M.CS ChemDraw Pro,1 Version 3.1 for Windows. J.Chem. Inf. Comput. Sci. 1995, 35, 166–167. DOI: 10.1021/ci00023a026. (b)Cousins, K. R. ChemDraw 6.0 Ultra CambridgeSoft Corporation, 100 Cambridge ParkDrive, Cambridge, MA 02140. http://www.camsoft.com. Commercial Price:  $1395.Academic Price:  $699. J. Am. Chem. Soc. 2000, 122, 10257–10258. DOI: 10.1021/ja0047572.(c) Buntrock, R. E. ChemOffice Ultra 7.0. J.Chem. Inf. Comput. Sci. 2002, 42, 1505–1506. DOI: 10.1021/ci025575p. (d) Li, Z.; Wan, H.; Shi, Y.;Ouyang, P. Personal Experience with Four Kinds of Chemical Structure DrawingSoftware: Review on ChemDraw, ChemWindow, ISIS/Draw, and ChemSketch. J. Chem.Inf. Comput. Sci. 2004, 44, 1886–1890. DOI: 10.1021/ci049794h.(e) Mendelsohn, L. D. ChemDraw8 Ultra, Windows and Macintosh Versions. J.Chem. Inf. Comput. Sci. 2004, 44, 2225–2226. DOI: 10.1021/ci040123t. (f) Cousins, K. R. ChemDrawUltra 9.0. CambridgeSoft, 100 CambridgePark Drive, Cambridge, MA 02140. www.cambridgesoft.com. See Web site for pricing options. J. Am. Chem. Soc. 2005, 127, 4115–4116. DOI:10.1021/ja0410237. (g) Zielesny, A. Chemistry Software PackageChemOffice Ultra 2005. J. Chem. Inf.Model. 2005, 45, 1474–1477. DOI:10.1021/ci050273j. (h) Mills, N. ChemDraw Ultra 10.0 CambridgeSoft, 100CambridgePark Drive, Cambridge, MA 02140. www.cambridgesoft.com. CommercialPrice:  $1910 for download, $2150 for CD-ROM; Academic Price:  $710 fordownload, $800 for CD-ROM. J. Am. Chem.Soc. 2006, 128, 13649–13650. DOI: 10.1021/ja0697875. (i) Kerwin, S. M.ChemBioOffice Ultra 2010 Suite. J. Am. Chem.Soc. 2010, 132, 2466–2467. DOI: 10.1021/ja1005306. (j) Milne, G. W. A. SoftwareReview of ChemBioDraw 12.0. J. Chem. Inf.Model. 2010, 50, 2053. DOI:10.1021/ci100385n. (k) Narayanaswamy, V. K.; Rissdörfer, M.; Odhav, B.Review on CambridgeSoft ChemBioDraw Ultra 13.0v. Int. J. Theor. Appl. Sci. 2013,5, 43–49.

[4]    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.

[5]    Bruker (2021). APEX4 (Version 2021.4-1). Program for Data Collection on AreaDetectors. Bruker AXS Inc., Madison, Wisconsin, USA.

声明：本文仅代表个人观点，笔者学识有限，资料整理过程中可能存在疏漏错误，请不吝指正。

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