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| GUI: Olex2[1] Refinement: SHELXL[2] |
案例来源：Dalton Trans. 2024, 53, 7424–7429. DOI[3]: 10.1039/d4dt00386a.CCDC[4]: 2300780. | | There if 1 structure in this paper. We examined this file: 2300780**1** (CCDC 2300780) Thank you for your replies and updated model, which is much better. But, as readily seen from the residual density plot, this structure is still unfinished. Also, the partially occupied diamine-coordinated Cu now makes no sense – with fully occupied N atoms but only partially occupied 'rest of the ligand'. I pointed this out in the previous review: there is water *and* the ligand. Please fix these issues. The final residual density map must be much 'cleaner' than now. Was this crystal *really* 1 mm big? Thank you. Structure 1 (CCDC 2300780): C10 H65 Cu3 K3 N12 Na Nb19 O78 Te2 These CheckCif A and B alerts are raised by this structure. This is for your information only - you may wish to address these issues before re-submitting your cif file to the CCDC. 220_ALERT_2_B NonSolvent Resd 1 O Ueq(max)/Ueq(min) Range 6.5 Ratio 420_ALERT_2_B D-H Bond Without Acceptor O4W –H4WB. Please Check 420_ALERT_2_B D-H Bond Without Acceptor O7W –H7WB. Please Check 420_ALERT_2_B D-H Bond Without Acceptor O10W –H10B. Please Check Please Check The crystal size is reported as 1 x 0.5 x 0.2 mm. | 本文共有1个结构。我们检查了这个文件：2300780**1**（CCDC 2300780）谢谢你的回复和更新的模型，它好多了。但是，从残余密度图中可以很容易地看出，该结构仍未完成。此外，部分占据的二胺配位的Cu现在没有意义——N原子完全占据，但“配体的其余部分”只有部分占据。我在之前的审查中指出：此处为水和配体。请解决这些问题。最终的残余密度图必须比现在“干净”得多。这个晶体真的有1毫米大吗？非常感谢。 结构1 (CCDC 2300780): C10 H65 Cu3 K3 N12 Na Nb19 O78 Te2 该结构触发这些CheckCif A和B警报。这仅供您参考——你可能希望在将您的CIF文件重新提交给CCDC之前解决这些问题。 220_ALERT_2_B NonSolvent Resd 1 O Ueq(max)/Ueq(min) Range 6.5 Ratio 420_ALERT_2_B D-H Bond Without Acceptor O4W –H4WB. Please Check 420_ALERT_2_B D-H Bond Without Acceptor O7W –H7WB. Please Check 420_ALERT_2_B D-H Bond Without Acceptor O10W –H10B. Please Check 请检查报告为1 x 0.5 x 0.2 mm的晶体尺寸。 |
上述审稿意见中对晶体尺寸提出了疑问，认为晶体尺寸中有一个方向的尺寸为1毫米太大了，让作者确认这一点，这个根据实际情况修改或说明即可。 另外一个则是有关乙二胺配位的铜这个片段的问题，在该片段中，乙二胺的两个氮原子占有率为1（full occupied），而两个碳原子占有率则为0.5（partially occupied），这在化学上显然没有意义（按这个占有率来理解，这里是0.5个乙二胺和2个“0.5个氨”），如图1所示。 ▲图1 有问题的乙二胺占有率 审稿人指出，这里应该是水和乙二胺都有，也就是水和乙二胺混占无序，按照审稿人的建议进行处理，如图2所示，该处大概是0.36403个乙二胺和2个“（1-0.36403）个水”。 ▲图2 水和乙二胺混占无序处理结果 相关视频： 晶体数据审稿意见-水和乙二胺混占无序(Dalton Trans)：https://www.bilibili.com/video/BV1n1421r7dw 如需论文和已发表CIF文件，请从以下链接下载： （1） 链接：https://pan.quark.cn/s/a835d2c46ede 提取码：DQNA （2） 链接：https://pan.baidu.com/s/1v6F61sBWrzO5CIszNs8VPg 提取码：lz3o | [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。 |
如需PDF文档，请从以下链接下载： 通过网盘分享的文件：晶体数据审稿意见-水和乙二胺混占无序.pdf
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发表于 2025-7-20 08:02:27
