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★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。 晶体结构不是预期结构案例27 案例79： 本来是按照如图79所示（由ChemBioDraw [1]绘制），利用氰化亚铜（CuICN, Copper(I) cyanide, CAS: 544-92-3）和某配体以二甲亚砜 [2]（DMSO, dimethyl sulfoxide, CAS: 67-68-5, CAS: 1142632 [2a], 1142633 [2b], 285805–285806 [2c], 703489–703491 [2d], 1571260 [2e]）作溶剂在一定条件下反应，以期得到含该配体的铜配合物，然而经后处理，结晶，经单晶X射线衍射实验（SC-XRD,single-crystal X-ray diffraction）得到晶体数据，经结构解析发现所得晶体的结构为[CuII(κO-DMSO)6]n[CuI6(CN)8]n。
▲图79 案例79反应示意图 相关视频： 单晶结构解析练习775(非预期结构-无序处理-CAP数据还原)：https://www.bilibili.com/video/BV12zjA6cEry 案例80： 本来是按照如图80所示，利用溴化铅（PbBr2, Lead(II)bromide, CAS: 10031-22-8）和配体以DMSO、乙醇 [3]（EtOH, ethanol, CAS: 64-17-5, CCDC: 1150324 [3a],1150325 [3b]）和氢溴酸为溶剂在一定条件下反应，以期得到含该配体的铅配合物，然而经后处理，结晶，SC-XRD得到晶体数据，经结构解析发现所得晶体的结构为(PbBr2)3(DMSO)2。
▲图80 案例80反应示意图 相关视频： 单晶结构解析练习776(非预期结构-数据还原-无序处理-残余峰)：https://www.bilibili.com/video/BV1aajx6NEuY 案例81： 本来是按照如图81所示，利用溴化铅和配体以DMSO和氢溴酸为溶剂在一定条件下反应，以期得到含该配体的铅配合物，然而经后处理，结晶，SC-XRD得到晶体数据，经结构解析发现所得晶体的结构为PbBr2(DMSO)2。
▲图81 案例81反应示意图 相关视频： 单晶结构解析练习777(非预期结构-数据还原-无序处理-残余峰)：https://www.bilibili.com/video/BV1n87M6iEP6 参考文献 [1] (a)Klein, F. M. CS ChemDraw Pro,1 Version 3.1 for Windows. J. Chem. Inf. Comput. Sci. 1995, 35, 166–167. DOI: 10.1021/ci00023a026. (b)Cousins, K. R. ChemDraw 6.0 Ultra CambridgeSoft Corporation, 100 Cambridge ParkDrive, Cambridge, MA 02140. http://www.camsoft.com. Commercial Price: $1395.Academic Price: $699. J. Am. Chem. Soc. 2000, 122, 10257–10258. DOI: 10.1021/ja0047572.(c) Buntrock, R. E. ChemOffice Ultra 7.0. J. Chem. Inf. Comput. Sci. 2002, 42, 1505–1506. DOI: 10.1021/ci025575p. (d) Li, Z.; Wan, H.; Shi, Y.;Ouyang, P. Personal Experience with Four Kinds of Chemical Structure DrawingSoftware: Review on ChemDraw, ChemWindow, ISIS/Draw, and ChemSketch. J. Chem. Inf. Comput. Sci. 2004, 44, 1886–1890. DOI: 10.1021/ci049794h.(e) Mendelsohn, L. D. ChemDraw8 Ultra, Windows and Macintosh Versions. J. Chem. Inf. Comput. Sci. 2004, 44, 2225–2226. DOI: 10.1021/ci040123t. (f) Cousins, K. R. ChemDrawUltra 9.0. CambridgeSoft, 100 CambridgePark Drive, Cambridge, MA 02140. www.cambridgesoft.com. See Web site for pricing options. J. Am. Chem. Soc. 2005, 127, 4115–4116. DOI:10.1021/ja0410237. (g) Zielesny, A. Chemistry Software PackageChemOffice Ultra 2005. J. Chem. Inf.Model. 2005, 45, 1474–1477. DOI:10.1021/ci050273j. (h) Mills, N. ChemDraw Ultra 10.0 CambridgeSoft, 100CambridgePark Drive, Cambridge, MA 02140. www.cambridgesoft.com. CommercialPrice: $1910 for download, $2150 for CD-ROM; Academic Price: $710 fordownload, $800 for CD-ROM. J. Am. Chem. Soc. 2006, 128, 13649–13650. DOI: 10.1021/ja0697875. (i) Kerwin, S. M.ChemBioOffice Ultra 2010 Suite. J. Am. Chem. Soc. 2010, 132, 2466–2467. DOI: 10.1021/ja1005306. (j) Milne, G. W. A. SoftwareReview of ChemBioDraw 12.0. J. Chem. Inf.Model. 2010, 50, 2053. DOI:10.1021/ci100385n. (k) Narayanaswamy, V. K.; Rissdörfer, M.; Odhav, B.Review on CambridgeSoft ChemBioDraw Ultra 13.0v. Int. J. Theor. Appl. Sci. 2013, 5, 43–49. [2] (a) Thomas, R.; Shoemaker, C. B.; Eriks, K. TheMolecular and Crystal Structure of Dimethyl Sulfoxide, (H3C)2SO.Acta Cryst. 1966, 21, 12–20. DOI: 10.1107/S0365110X66002263.(b) Viswamitra, M. A.; Kannan, K. K. MolecularDimensions and Crystal Structure of Dimethyl Sulphoxide at −60°C. Nature1996, 209, 1016–1017. DOI: 10.1038/2091016a0. (c) Ibberson, R. M. Neutron PowderDiffraction Studies of Dimethyl Sulfoxide. Acta Cryst. 2005, C61,o571–o573. DOI: 10.1107/S010827010502617X. (d) Gajda, R.; Katrusiak, A. Electrostatic Matchingversus Close-Packing Molecular Arrangement in Compressed Dimethyl Sulfoxide(DMSO) Polymorphs. J. Phys. Chem. B 2009, 113, 2436–2442. DOI: 10.1021/jp808987k. (e)Reuter, H. Structural Parameters of Dimethyl sulfoxide, DMSO, at 100 K, Basedon a Redetermination by Use of High-Quality Single-Crystal X-ray Data. ActaCryst. 2017, E73, 1405–1408. DOI: 10.1107/S2056989017012464. [3] (a) Jönsson, P. G. Hydrogen Bond Studies.CXIII. The Crystal Structure of Ethanol at 87 K. Acta Cryst. 1976,B32, 232–235. DOI: 10.1107/S0567740876002653.(b) Allan, D. R.; Clark, S. J. Comparison ofthe High-Pressure and Low-Temperature Structures of Ethanol and Acetic Acid. Phys.Rev. B 1999, 60, 6328. DOI: 10.1103/PhysRevB.60.6328.
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