晶体数据还原示例46(孪晶拆分-B级警报PLAT973)

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晶体数据还原示例46(孪晶拆分-B级警报PLAT973)

案例来源：CCDC[1] 2409825‒2409826. DOI[2]: 10.5517/ccdc.csd.cc2lwm9f;10.5517/ccdc.csd.cc2lwmbg.

案例结构如图1所示（由ChemBioDraw[3]绘制）。

▲图1 案例结构

该结构的晶体衍射图如图2所示（由APEX4[4]呈现），由钼靶测试，曝光时间为2秒。

▲图2 衍射图

按默认设置（信噪比阈值为10.00，从3轮数据，每轮20帧sfrm中收集衍射点）收集到865个衍射点，添加限制条件后剩下289个衍射点用于中指标化，结果如图3所示，指标化率在60%左右。

▲图3 指标化结果

按此默认结果进行数据还原，结果如图4所示（由Olex2[5]呈现，验证报告由PLATON[6]呈现），精修指标都还不错，但金属附近的残余峰触发了一个B级警报PLAT973（参阅推文“CheckCIF-PLAT973”）。

▲图4 CCDC 2409826结果

其倒易空间点阵的3个正方向如图5所示。

▲图5 倒易空间点阵

对其做孪晶拆分，将865个衍射点分为两组，分别为408和457个衍射点，如图6所示。

▲图6 衍射点分组

这2组衍射点指标化结果如图7所示。

▲图7 拆分的衍射点的指标化结果

孪晶拆分后，结果如图8所示，无AB级警报，虽然R因子比上面略高。

▲图8 CCDC 2409825结果

视频操作演示请参阅：

单晶结构解析练习364(孪晶拆分-文献案例)：

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参考文献

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