审稿意见-正确的晶胞下进行数据还原2

DJ_Tokyo

审稿意见-正确的晶胞下进行数据还原2

文本所用软件/程序

Data process and reduce: APEX4[1]    GUI: Olex2[2]    Structure solution: SHELXT[3]    Structure refinement: SHELXL[4]    Space group determination: XPREP[5]

案例来源：Dalton Trans. 2023, 52, 13146–13153. DOI[6]: 10.1039/d3dt02460a.CCDC[7]: 2262745.

审稿意见

大意

Structure 2 (CCDC 2262745): C50 H72 Cl4 Co2 N4       - Again looking at the  HKLF instruction it seems that the cell has been changed after the initial  integration, the data should really be reintegrated in the correct cell. This  may also help to improve the Rint and reduce the number of reflections  needing to be omitted. Given that the BASF is 0.5 it would be worth checking  the space group when reintegrating and checking that one of the cell axes is  not currently doubled.    - Removing the  restraints suggests that perhaps there is some unmodelled disorder present in  the ethyl chains that should be modelled, if still the case once the data  have been reintegrated.       Answer: The data have been reintegrated and the space group was  corrected to be Pnma, and thus no twin law needed in the refinement. And the  new cif file have been updated in CCDC.

结构2 (CCDC 2262745):  C50 H72 Cl4 Co2 N4       查看HKLF指令，看起来在最初积分之后晶胞已改变，数据应当在正确晶胞下重新积分。这可能也有助于改善Rint，并可降低需要忽略的衍射点数量。给定的BASF为0.5，值得在重新积分时检查空间群，并检查其中一个晶轴不是当前晶轴的两倍。          移除限制表明，乙基链存在未建模的无序，如果数据重新积分后仍旧如此，因对其进行建模。             答复：数据已重新积分，并将空间群修正为Pnma，此时精修中无需孪晶法则。新的CIF文件已在CCDC中更新。

如图1所示，HKLF指令中包含变换矩阵（transformationmatrix），审稿人认为当前晶胞在积分之后发生了变化，要求重新在正确的设置下进行数据还原，使用OMIT指令忽略了很多衍射点，审稿人认为重新积分数据可能就不需要使用OMIT指令来忽略衍射点，另外数据中包含了孪晶法则指令TWIN和批比例因子BASF，实际上结构中整个配体存在特殊无序，以上这些都需要重新进行数据处理来进行检查和解决。

▲图1 CCDC 2262745结构投稿状态

后重新还原数据，更正了空间群，虽然整个配体仍存在无序，不过不要孪晶法则，HKLF指令后也没有变换矩阵，需要忽略的衍射点也少了，如图2所示。

▲图2 CCDC 2262745结构发表状态

视频演示操作请参阅：

审稿意见-为什么要在正确的晶胞下进行数据还原2：https://www.bilibili.com/video/BV1pz4y1K7sj

如需论文文档和晶体数据用于练习，可从以下链接下载：

（1）

链接：https://pan.quark.cn/s/ccc189b6258a

提取码：tVn8

（2）

链接：https://pan.baidu.com/s/1lYM2NGtwK8yUd8TnNMknog

提取码：crrw

参考文献

[1] Bruker (2021).  APEX4 (Version 2021.4-1). Program for Data Collection on Area  Detectors. Bruker AXS Inc., Madison, Wisconsin, USA.    [2] 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.    [3] Sheldrick, G.  M. SHELXT – Integrated Space-Group  and Crystal Structure Determination. Acta  Cryst. 2015, A71, 3–8. DOI:  10.1107/S2053273314026370.    [4] (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.    [5] Bruker (2014). XPREP (Version 2014/2), Program for Space Group Determination.  Bruker AXS Inc., Madison, Wisconsin, USA.    [6] (a) International Organization for Standardization  (2012). ISO 26324:2012. Information and  Documentation – Digital Object Identifier System.  http://www.iso.org/iso/catalogue_detail.htm?csnumber=43506. (b) International  Organization for Standardization (2022). ISO 26324:2022. Information and Documentation – Digital Object Identifier System.  https://www.iso.org/standard/81599.html    [7] (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。