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晶体数据审稿意见-严重的残余峰(Chem) 案例来源：CCDC[1] 2360390. Chem 2025, 11, 102392. DOI[2]: 10.1016/j.chempr.2024.102392. 案例结构如图1所示（由ChemBioDraw[3]绘制）。 ▲图1 案例结构 审稿意见： XRD:compound 5: There is a very highresidual electron density peak, which cannot be accounted for by absorption ortruncation (as suggested by the authors) - this can only reliably explainelectron density peaks of up to 5% of the electron density of the heavy element.In the current case, the electron density peak is even closer to a carbon atomthan to the heavy atom! In the current state, the XRD data can only serve as aproof of connectivity in the best case. This would need to be clearlycommunicated and no bonding parameters could be discussed reliably. 大意： X射线衍射：化合物5：有一个非常高的残余电子密度峰，这不能用吸收效应或截断效应来解释（如作者所建议的那样）——这只能可靠地解释高达重元素电子密度5%的电子密度峰。在目前的情况下，该电子密度峰更接近碳原子，而不是重原子！在目前的状态下，X射线衍射数据只能在最好的情况下作为连通性的证明。这需要明确传达，并且无法可靠地讨论任何键合参数。 上述审稿意见主要是说结构中存在很大的残余峰，这不能用吸收效应或者截断效应来解释，这需要进行说明，并且该数据无法用于可靠地讨论键长键角等参数，只能用来表明化合物结构。 如图2所示（由Olex2[4]呈现），有一个很大的残余峰Q1（Max Peak = 4.9）在靠近碳原子的附近，按Ctrl+M查看其差值电子密度图，如图3所示，结构中间烯基片段附近差值电子密度图严重异常。 ▲图2 最大残余峰 ▲图3 差值电子密度图 笔者帮忙将中间烯基片段由原来的二组分无序处理成三组分无序，并建模了甲苯溶剂，残余峰从4.6降为1.9，如图4所示。 ▲图4 笔者第一次处理结果 返稿后，二审意见如下： **5** - The Te at the same positions should haveEXYZ and EADP applied to maintain sensible values. - It looks like the omitted reflections wereomitted before the refinement was completed and they don't look like they needto be omitted. - The molecule is extensively disordered withsome slight issues, however the authors note this and do not discuss geometricparameters so this is alright. Details of the disorder modelling should beadded to the cif. 大意： -处于相同位置的Te应当应用EXYZ和EADP以保持合理值。 -看起来忽略的衍射点在精修完成之前就忽略了，它们看起来不需要忽略。 -分子大量无序，存在一些轻微问题，但作者注意到了这一点，没有讨论几何参数，这是正确的。 无序建模的详情应当添加到CIF中。 按审稿人要求处理即可，第一点，对于处于同一位置的Te原子，使用SHELXL[5]指令EXYZ（参阅推文“SHELXL指令之EXYZ”）和EADP（参阅推文“SHELXL指令之EADP”）使其原子坐标和原子各向异性位移参数相同，如图5所示，在Olex2中施加EXYZ约束的原子椭球上会有“EXYZ”字样。 ▲图5 对相同位置的Te应用EXYZ和EADP约束 第二点是说在精修中使用SHELXL指令OMIT（参阅推文“SHELXL指令之OMIT”）忽略了一些衍射点，如图6所示，要求将这些衍射点恢复，按要求将这些OMIT指令从ins文件中删除，重新精修即可。 ▲图6 忽略衍射点的OMIT指令 最后，是要求将无序建模详情添加到CIF[6]中，按要求将其添加到CIF中“_refine_special_details”条目即可，如图7所示。（注意：CIF中每行不要超过80个字符，因此要及时换行。） ▲图7 CIF中添加的无序建模详情 视频讲解请参阅： 晶体数据审稿意见-严重的残余峰(Chem)：https://www.bilibili.com/video/BV19SXSYTE9Y 论文PDF和CIF文件： 提取码: b6cz 参考文献 [1] (a) Allen, F. H.The Cambridge Structural Database: A Quarter of a Million Crystal Structuresand Rising. Acta Cryst. 2002, B58, 380–388. DOI:10.1107/S0108768102003890. (b) Groom, C. R.; Bruno, I. J.; Lightfoot, M.P.; Ward, S. C. The Cambridge Structural Database. 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