晶体数据审稿意见-使用溶剂遮掩但未给出说明

DJ_Tokyo

当一个晶体数据采用了溶剂遮掩（使用PLATON[1]的PLATON SQUEEZE[2]或者Olex2[3]的Solvent Mask[4]），但相关信息未填入CIF[5]或者未在论文（正文或支持信息）中描述时，有可能会遇到如下审稿意见：

审稿意见	大意
A solvent mask has been used, but nothing regarding this process  has been reported in the CIF. This is not acceptable. You must provide  information regarding the estimated number and nature of the masked moieties.  The relevant information should be readily available from the TGA/DSC  results, the knowledge of the crystallisation conditions and, finally, from  the number of masked electrons, the size of the void and the relative  position of electron density peaks before the mask was applied.	已使用溶剂遮掩，但CIF中没有关于该过程的任何报道。这是不可接受的。您必须提供有关遮掩部分的估计数量和性质的信息。相关信息应易于从热重分析/差示扫描量热法结果、结晶条件信息以及最后从遮掩电子的数量、空隙的大小和施加遮掩之前电子密度峰的相对位置获得。
The reported formulae must contain the masked moieties, leading to  the incorrect reporting of many follow-on quantities like the density,  molecular mass, F000 and absorption coefficient μ.	所报道的分子式必须包含遮掩部分，导致许多后续量（如密度、分子量、F000和吸收系数μ）的报告不正确。

视频讲解请参阅：

晶体数据审稿意见-使用溶剂遮掩但未给出说明：https://www.bilibili.com/video/BV1EJ4m1G7uv

案例参考

晶体结构扣除溶剂后在论文中的描述

参考资料

去除无序溶剂对计算结构因子的贡献

参考文献

[1](a) Spek, A. L.Single-Crystal Structure Validation with the Program PLATON. J. Appl. Cryst. 2003, 36, 7–13. DOI:10.1107/S0021889802022112. (b) Spek, A. L. Structure Validation in Chemical Crystallography. Acta Cryst.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.

[2]Spek, A. L. PLATON SQUEEZE: A Toolfor the Calculation of the Disordered Solvent Contribution to the CalculatedStructure Factors. Acta Cryst. 2015, C71, 9–18. DOI: 10.1107/S2053229614024929.

[3]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.

[4]Spek, A. L.; van der Sluis, P. BYPASS: an Effective Method for the Refinementof Crystal Structures Containing Disordered Solvent Regions. Acta Cryst.1990, A46, 194–201. DOI:10.1107/S0108767389011189.

[5](a) Hall, S. R.; Allen, F. H. Brown, I. D. The Crystallographic InformationFile (CIF): a New Standard Archive File for Crystallography. Acta Cryst. 1991, A47, 655–685. DOI: 10.1107/S010876739101067X. (b) Hall, S. R. TheSTAR File: A New Format for Electronic Data Transfer and Archiving. J. Chem. Inf. Comput. Sci. 1991, 31, 326–333. DOI: 10.1021/ci00002a020.(c) Hall, S. R.; Spadaccini, N. The STAR File: Detailed Specifications. J. Chem. Inf. Comput. Sci. 1994, 34, 505–508. DOI: 10.1021/ci00019a005.