SHELXT解析失败SHELXS救场案例

DJ_Tokyo

SHELXT解析失败SHELXS救场案例

文本所用软件/程序

GUI: Olex2[1]    Structure solution: SHELXT[2],  SHELXS[3]    Structure refinement: SHELXL[4]

最近解析某个晶体结构，运行SHELXT进行解析，在进行了48次尝试结构解析耗时213.726秒，空间群确定耗时37.227秒耗时后，得到一团乱麻，如图1所示。

▲图1 SHELXT解析结果

而后，换用SHELXS程序，用直接法（Direct Methods[5]）进行解析，仅耗时1.4秒，给出的结果可以明显看出结构框架，如图2所示，在此基础上进行结构指认确定原子类型，往下解析即可。

▲图2 SHELXS解析结果

最终解析结果如图3所示，虽然繁琐，但还比较顺利。

▲图3 最终处理结果

视频讲解请参阅：

SHELXT解析失败SHELXS救场案例：https://www.bilibili.com/video/BV1oqtFeREfL

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. DOI: 10.1107/S0021889808042726.    [2] Sheldrick, G.  M. SHELXT – Integrated Space-Group  and Crystal Structure Determination. Acta  Cryst. 2015, A71, 3–8. DOI:  10.1107/S2053273314026370.    [3] Sheldrick, G.  M. SHELXS-97, Program for Crystal Structure Solution. University of Göttingen,  Germany, 1997.    [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] (a) Sheldrick,  G. M. Phase Annealing in SHELX-90:  Direct Methods for Larger Structures. Acta  Cryst. 1990, A46, 467–473. DOI: 10.1107/S0108767390000277. (b) Sheldrick, G. M.; Usón, I. Advances in direct  methods for protein crystallography. Curr.  Opin. Struct. Biol. 1999, 9, 643–648. DOI:  10.1016/S0959-440X(99)00020-2.  (c) Sheldrick, G. M., Hauptman, H. A., Weeks, C. M., Miller, R. & Usón,  I. International Tables for  Crystallography, Vol. F, edited by E. Arnold and M. Rossmann, pp. 333  345. Dordrecht: Kluwer Academic Publishers, 2001. (d) Giacovzaao, C. Phasing in Crystallography. Oxford:  IUCr/Oxford University Press, 2014.

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