| GUI: Olex2[1] Structure refinement: SHELXL[2] |
案例来源：New J. Chem. 2024, 48, 14690–14696. DOI[3]: 10.1039/d4nj02131b. CCDC[4]: 2353118. | Q: In some structures, 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. | 问：在某些结构中，使用了溶剂遮掩，但CIF中没有关于这一过程的报道。这是不可接受的。您必须提供有关被遮掩部分的估计数量和性质的信息。相关信息应易于从TGA/DSC结果、结晶条件的信息中获得，最后从施加遮掩前的遮掩电子数量、孔隙大小和电子密度峰的相对位置中获得。 | | A: All solvents have been modelled for all structures in revised CIFs which were updated in CCDC. | 答：所有结构中的所有溶剂均已得到建模，并在CCDC中更新了修正的CIF。 |
| Q:"The chemical formula must be consistent with the atomic content specified by the _atom_site_ information, and match the _chemical_formula_weight. If atoms are missing from the atomic model (e.g. unlocated H atoms or solvent molecules suppressed by the 'SQUEEZE' or similar approach), the moiety and sum formulae should state the assumed overall formula." https://journals.iucr.org/c/services/cif/reqdata.html | 问：化学式必须与_atom_site_信息指定的原子内容一致，并与_chemical_formula_weight相匹配。如果原子模型中缺失原子（例如，没有定位氢原子，或者溶剂被“SQUEEZE”或类似方法抑制），部分分子式以及总和分子式应当指明假定总体分子式。 | | A: All solvents have been modelled for all structures in revised CIFs which were updated in CCDC. | 答：所有结构中的所有溶剂均已得到建模，并在CCDC中更新了修正的CIF。 |
| Q:**230530b_0m_a** (CCDC 2353117) Please report the solvent masking properly (see above) | 问：**230530b_0m_a** (CCDC 2353117) 请正确报道溶剂遮掩（见上文） | | A: The solvent n-hexane has been modelled in the revised CIF, which has been updated in CCDC. | 答：正己烷溶剂已建模，并在CCDC中更新了修正的CIF。 |
晶体结构中溶剂也是结构组成部分，使用溶剂遮掩程序将其遮掩掉的确方便，但溶剂遮掩后需要做相应说明和描述，否则可能会得到上述类似审稿意见。笔者个人一致推崇的是，溶剂能够建模的尽量建模。类似的审稿意见可参阅推文“晶体数据审稿意见-溶剂能建模的应当建模而不是遮掩了事”或视频“晶体数据审稿意见-溶剂能建模的应当建模而不是遮掩了事：https://www.bilibili.com/video/BV1KT421Y7Jq”。 相关视频： 晶体数据审稿意见-溶剂遮掩不如建模省事：https://www.bilibili.com/video/BV1Pz421i7kd | [1] 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. [2] (a) Sheldrick, G. M. SHELXL-2019/3, Program for Crystal Structure Refinement, University of Göttingen, Germany, 2019. (b) Sheldrick, G. M. A Short History of SHELX. Acta Cryst. 2008, A64, 112–122. DOI: 10.1107/S0108767307043930. (c) Sheldrick, G. M. Crystal Structure Refinement with SHELXL. Acta Cryst. 2015, C71, 3–8. DOI: 10.1107/S2053229614024218. (d) Lübben, J.; Wandtke, C. M.; Hübschle, C. B.; Ruf, M.; Sheldrick, G. M.; Dittrich, B. Aspherical scattering factors for SHELXL – model, implementation and application. Acta Cryst. 2019, A75, 50–62. DOI: 10.1107/S2053273318013840. [4] (a) Allen, F. H. The Cambridge Structural Database: a quarter of a million crystal structures and rising. Acta Cryst. 2002, B58, 380–388. DOI: 10.1107/S0108768102003890. (b) Allen, F. H. The Cambridge Structural Database: a quarter of a million crystal structures and rising. Acta Cryst. 2016, B72, 171–179. DOI: 10.1107/S2052520616003954. |
| 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。 |
|
发表于 2025-7-4 07:50:32
