数据还原导向不同空间群案例2

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数据还原导向不同空间群案例2

案例来源：CCDC[1] 2384326, 2404887‒2404888.Chem. Commun. 2024, DOI[2]: 10.1039/d4cc05446f.

其结构如图1所示（由ChemBoiDraw[3]绘制）。

▲图1 案例结构

该晶体的衍射图如图2所示（由APEX4[4]呈现），曝光时间为2秒。

▲图2 两个晶体的衍射图

按默认设置（信噪比阈值10.00，3轮数据每轮20幅sfrm）收集到434个衍射点，对衍射点限制后以154个衍射点进行指标化，程序默认选择第一个晶胞，将收集衍射点设置为每轮50幅衍射图，收集到1048个衍射点，对衍射点限制后以425个，衍射点进行指标化，程序默认选择第三个晶胞，如图3所示。

▲图3 两个数据指标化结果

到了BravaisLattice步骤时，前者（CCDC 2404888）是Monoclinic P而后者（CCDC 2384326/2404887）是Monoclinic C，如图4所示，两个晶胞参数a轴和c轴互换。

▲图4 Bravais Lattice结果

在XPREP[5]中，CCDC2404888确定为第14号空间群P21/c，CCDC 2384326/2404887确定为第15号空间群C2/c，如图5所示。

▲图5 两个数据空间群确定情况

如图6−7所示（由Olex2[6]呈现），CCDC 2404888不对称单元ASU（asymmetry unit）中为完整的一个分子结构，CCDC 2384326/2404887 ASU中为半个分子结构，需要对此操作得到完整分子结构。

▲图6 CCDC 2404888 ASU结构

▲图7 CCDC 2384326/2404887 ASU结构

视频操作演示请参阅：

单晶结构解析练习318(数据还原-文献案例)：https://www.bilibili.com/video/BV1V1z7YCEAm

如需数据进行练习，请从以下链接下载：

链接: https://pan.baidu.com/s/1qSMNIk72orZh1MSEHqOQQA

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参考文献

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[2]    (a) International Organization forStandardization (2012). ISO 26324:2012. Informationand 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

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

[5]    Bruker (2014). XPREP (Version 2014/2), Programfor Space Group Determination. Bruker AXS Inc., Madison, Wisconsin, USA.

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