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本文所用图形用户界面（GUI，Graphical UserInterface）：Olex2[1] 本文所用结构精修程序：SHELXL[2] 案例来源：J. Mater. Chem. A, 2024, doi: 10.1039/d3ta07946e. CCDC[3]：2309587 这是前段时间求助的一个数据，如图1–2所示。 ▲图1 问题描述和信息交流 ▲图2 问题描述和信息交流 该晶体数据的审稿意见如下： StructureCMOF-3 (CCDC 2309587): C226 H Br5 Cu16 I16 N21 TheMS does not mention the change in the structure of the sponge, the structurelooks like a preliminary working version. Please have a look if there has beenan error here, this structure is definitely not for publication in this form.Please check all the cif alerts. TheseCheckCif A and B alerts are raised by this structure: 031_ALERT_4_ARefined Extinction Parameter Within Range ...... 0.000 Sigma 080_ALERT_2_AMaximum Shift/Error ............................ 4.15 Why ? 183_ALERT_1_AMissing _cell_measurement_reflns_used Value .... Please Do ! 184_ALERT_1_AMissing _cell_measurement_theta_min Value ...... Please Do ! 185_ALERT_1_AMissing _cell_measurement_theta_max Value ...... Please Do ! 214_ALERT_2_AAtom C036 (Anion/Solvent) ADP max/min Ratio 6.7 prolat 216_ALERT_3_ADisordered C185# (An/Solv) ADP max/min Ratio 9.9 Note 369_ALERT_2_ALong C(sp2)-C(sp2) Bond C0AE - C09H . 1.68 Ang. 699_ALERT_1_AMissing _exptl_crystal_description Value ....... Please Do ! 201_ALERT_2_BIsotropic non-H Atoms in Main Residue(s) ....... 1 Report 212_ALERT_2_BADP of Atom C77 is N.P.D. or (nearly) 2D . Please Check 216_ALERT_3_BDisordered C187# (An/Solv) ADP max/min Ratio 7.6 Note 241_ALERT_2_BHigh 'MainMol' Ueq as Compared to Neighbors of C0AF Check 241_ALERT_2_BHigh 'MainMol' Ueq as Compared to Neighbors of C05C Check 241_ALERT_2_BHigh 'MainMol' Ueq as Compared to Neighbors of C06V Check 241_ALERT_2_BHigh 'MainMol' Ueq as Compared to Neighbors of C073 Check 241_ALERT_2_BHigh 'MainMol' Ueq as Compared to Neighbors of C58 Check 241_ALERT_2_BHigh 'MainMol' Ueq as Compared to Neighbors of C098 Check 342_ALERT_3_BLow Bond Precision on C-C Bonds ............... 0.03539 Ang. 351_ALERT_3_BLong C-H (X0.96,N1.08A) C4 - H5B . 1.21 Ang. 368_ALERT_2_BShort C(sp2)-C(sp2) Bond C06J - C077 . 1.12 Ang. 368_ALERT_2_BShort C(sp2)-C(sp2) Bond C09E - C088 . 1.13 Ang. 369_ALERT_2_BLong C(sp2)-C(sp2) Bond C06S - C059 . 1.60 Ang. 369_ALERT_2_BLong C(sp2)-C(sp2) Bond C08G - C090 . 1.60 Ang. 369_ALERT_2_BLong C(sp2)-C(sp2) Bond C09E - C061 . 1.61 Ang. 733_ALERT_1_BTorsion Calc 179(15), Rep 179(99) ...... 6.67 s.u.-R 987_ALERT_1_BThe Flack x is >> 0 - Do a BASF/TWIN Refinement Please Check TheUeq values of the following atoms are extremely large(Ueq = > 0.15). Eitherthe occupancy is set too high for these atom, or you might need to explore thepossibility that these atoms are involved in some form of disorder: C073 Br12C036 C47 C09H C098 C77. Theabsorption coefficient is given as 11.786. Absorption correction must becarried out and reported correctly. Tmax is reported as ? and Tmin is given as?. The absorption correction type is reported as '?'. Additional Info: Thecrystal size is given as ? x ? x ? mm^3.) Thefollowing cif items regarding the unit cell determination are missing: _cell_measurement_reflns_used _cell_measurement_theta_min _cell_measurement_theta_max Pleasesupply values for these items. Theshape of the crystal is not provided in the _exptl_crystal_description sectionof the cif. Theshape of the crystal is not provided in the _exptl_crystal_description sectionof the cif. Thecolour of the crystal is not provided in the _exptl_crystal_colour section ofthe cif. Theshape of the crystal is not provided in the _exptl_crystal_description sectionof the cif. Thecolour of the crystal is not provided in the _exptl_crystal_colour section ofthe cif. Thecrystal size is reported as ? x ? x ? mm^3. Thefollowing cif items regarding the software used in this structure determinationare missing: _computing_data_collection _computing_structure_solution _computing_molecular_graphics _computing_publication_material _computing_publication_material _diffrn_measurement_device_type Pleasesupply values for these items. ▲图3 投稿时的数据情况 后经优化的结果如图4所示。 ▲图4 重新处理结果 处理完的结果还剩下两个B级警报，于是对其做了解释，如图5所示。 ▲图5 最终验证报告 视频操作演示请参阅 晶体数据审稿意见-大量AB级警报的解决：https://www.bilibili.com/video/BV1Ks421K7wT 参考文献 [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. [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 ofSHELX. Acta Cryst. 2008, A64, 112–122. (c) Sheldrick, G. M.Crystal structure refinement with SHELXL.Acta Cryst. 2015, C71, 3–8. (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. [3](a) Allen, F. H. The Cambridge Structural Database: a quarter of a millioncrystal structures and rising. ActaCryst. 2002, B58, 380–388. (b) Allen, F. H. TheCambridge Structural Database: a quarter of a million crystal structures andrising. Acta Cryst. 2016, B72, 171–179.
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-大量AB级警报的解决.pdf
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发表于 2025-5-11 07:16:52
