CheckCIF-B级警报PLAT971和973(金属附近残余峰-孪晶拆分)

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CheckCIF-B级警报PLAT971和973(金属附近残余峰-孪晶拆分)

案例来源：CCDC[1] 2278815. Inorg. Chem. 2024, 63, 18365−18378. DOI[2]:10.1021/acs.inorgchem.4c02316.

案例结构如图1所示（由ChemBioDraw[3]绘制）。

▲图1 案例结构

如图2所示（由Olex2[4]呈现），各项精修指标均不错，但Max Peak = 3.2（在金属附近）触发了三个B级警报PLAT971（参阅推文“CheckCIF-PLAT971”）和PLAT973（参阅推文“CheckCIF-PLAT973”）。

▲图2 案例结构情况

如图3所示，PLATON[5]为检测到孪晶法则，但这不能排除孪晶情况，另外线性吸收系数较低，因此在吸收校正修改Mu*r值作用不大。

▲图3 PLATON孪晶法则检测结果

在APEX4[6]中得到晶胞后查看倒易空间点阵，如图4‒6所示，显然是孪晶。

▲图4 倒易空间点阵A轴方向视图

▲图5 倒易空间点阵B轴方向视图

▲图6 倒易空间点阵C轴方向视图

于是对其做孪晶拆分处理，最后得到的结果如图7所示，Max Peak = 1.3，不再有上述B级警报PLAT971和PLAT973。

▲图7 孪晶拆分处理结果

视频操作演示请参阅：

单晶结构解析练习292(数据还原-文献案例-孪晶拆分)：https://www.bilibili.com/video/BV166UwYPENC

数据下载：

论文和CIF：

链接:https://pan.baidu.com/s/1jlhLzbm5vUWVi5zDmSqP5g

提取码: 7ssy

CCDC2278815（Lu）：

链接: https://pan.baidu.com/s/1uchO8fjgeAGReqCSNm_2ew

提取码: 1nb5

参考文献

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[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]    (a) Spek, A. L. Single-Crystal Structure Validation with theProgram PLATON. J. Appl. Cryst. 2003, 36, 7–13. DOI: 10.1107/S0021889802022112. (b) Spek, A. L. StructureValidation in Chemical Crystallography. ActaCryst. 2009, D65, 148–155. DOI:10.1107/S090744490804362X. (c) Spek, A. L. What Makes a Crystal Structure Report Valid? Inorg. Chim. Acta 2018, 470, 232–237. DOI:10.1016/j.ica.2017.04.036. (d) Spek, A. L. checkCIFValidation ALERTS: What They Mean and How to Respond. Acta Cryst. 2020, E76, 1–11. DOI: 10.1107/S2056989019016244.

[6]    Bruker (2021). APEX4 (Version 2021.4-1).Program for Data Collection on Area Detectors. 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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链接: https://pan.baidu.com/s/1zpUvQjfmWEki1qNPWeHvyg 提取码: jtku