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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28 案例82： 本来是按照如图82所示（由ChemBioDraw [1]绘制），以三价铝和配体在N,N-二甲基甲酰胺 [2]（DMF, N,N-dimethylformamide,CAS: 68-12-2, CCDC [3]: 102756 [2a], 1869635–1869638 [2b],1869744–1869752 [2b]）、甲酸 [4]（HCOOH, formic acid, CAS: 64-18-6, CCDC: 1159366 [4a], 1159366 [4b],640128 [4c]）和硝酸[5]（HNO3, nitric acid, CAS: 7697-37-2, CCDC:754934–754936）作为溶剂在一定条件下反应，以期得到含该配体的铝配合物，然而所得晶体经单晶X射线衍射（SC-XRD, singlecrystal X-ray diffraction）实验得到晶体数据，经结构解析发现晶体实际结构为[(HCOO)2Al(OH)]n，显然，在该反应条件下，配体未与金属铝结合。
▲图82 案例82反应示意图 相关视频： 单晶结构解析练习780(非预期结构)：https://www.bilibili.com/video/BV19iMW65EVX 案例83： 本来是按照如图83所示，利用高碘酸铵（NH4IO4, Ammonium periodate, CAS: 13446-11-2,CCDC: 2564212）与化合物A在一定条件下反应，以期得到化合物B，然而所得晶体经SC-XRD实验得到晶体数据，经结构解析发现晶体实际结构为高碘酸铵，显然，在该反应条件下，二者未发生反应。
▲图83 案例83反应示意图 相关视频： 单晶结构解析练习781(非预期结构)：https://www.bilibili.com/video/BV1meML6CEKA 案例84： 本来是按照如图84所示，利用[1,1'-联萘]-2,2'-二胺 [6]（BINAM, [1,1'-binaphthalene]-2,2'-diamine,CAS: 4488-22-6; CCDC: 217436 [6a], 1018249 [6b], 1111523 [6c]）和某金属溴化物以乙醇 [7]（EtOH, ethanol, CAS: 64-17-5, CCDC: 1150324 [7a], 1150325 [7b]）和氢溴酸在一定条件反应，以期得到含该配体的金属化合物，然而所得晶体经SC-XRD实验得到晶体数据，经结构解析发现晶体实际结构为[1,1'-联萘]-2,2'-二胺二氢溴酸盐的乙醇溶剂化物。
▲图84 案例84反应示意图 相关视频： 单晶结构解析练习784(非预期结构-无序处理)：https://www.bilibili.com/video/BV11SKu6HEds 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. ChemistrySoftware Package ChemOffice 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)Borrmann, H.; Persson, I.; Sandström, M.; Stålhandske, C. M. V. The Crystal andLiquid Structures of N,N-Dimethylthioformamide and N,N-DimethylformamideShowing a Stronger Hydrogen Bonding Effect for C–H⋯S than of C–H⋯O. J.Chem. Soc. Perkin Trans. 2 2000, 393–402. DOI:10.1039/a904531g. (b) Ratajczyk, P.; Sobczak, S.; Katrusiak, A. High-PressureStructure and Properties of N,N-Dimethylformamide (DMF). Cryst.Growth Des. 2019, 19, 896–901. DOI: 10.1021/acs.cgd.8b01452. [3] (a)Allen, F. H. The Cambridge Structural Database: A Quarter of a Million Crystal Structuresand Rising. Acta Cryst. 2002, B58, 380–388. DOI:10.1107/S0108768102003890. (b) Groom, C. R.; Bruno, I. J.; Lightfoot, M.P.; Ward, S. C. The Cambridge Structural Database. Acta Cryst. 2016, B72, 171–179. DOI:10.1107/S2052520616003954. (c) Mitchell, J.; Robertson, J. H.; Raithby,P. R. Cambridge Crystallographic Data Centre (CCDC). Comprehensive Coordination Chemistry III 2021, 413–437. DOI:10.1016/B978-0-12-409547-2.14829-2. [4] (a)Holtzberg, F.; Post, B.; Fankuchen, I. The Crystal Structure of Formic Acid. ActaCryst. 1953, 6, 127–130. DOI:10.1107/S0365110X53000478. (b) Nahringbauer, I. A Reinvestigation of theStructure of Formic Acid (at 98 K). Acta Cryst. 1978, B34,315–318. DOI: 10.1107/S0567740878002940. (c) Allan,D. R.; Clark, S. J. Impeded Dimer Formation in the High-Pressure CrystalStructure of Formic Acid. Phys. Rev. Lett. 1999, 82, 3464–3467.DOI: 10.1103/PhysRevLett.82.3464. [5] Allan, D. R.; Marshall,W. G.; Francis, D. J.; Oswald, I. D. H.; Pulham, C. R.; Spanswick, C. TheCrystal Structures of the Low-Temperature and High-Pressure Polymorphs ofNitric Acid. Dalton Trans. 2010, 39, 3736–3743. DOI: 10.1039/b923975h. [6] (a) Jones, M. D.;Almeida Paz, F. A.; Davies, J. E.; Johnson, B. F. G. (R)-(+)-2,2′-Diamino-1,1′-binaphthyl.Acta Cryst. 2003, E59, o910–o912. DOI: 10.1107/S1600536803011681. (b) Murru,S.; Srivastava, R. S.; Fronczek, F. R. CCDC 1018249: Experimental CrystalStructure Determination. CSD Commun. 2014, DOI: 10.5517/cc135krl. (c) Gridunova,G. V.; Furmanova, N. G.; Shklover, V. E.; Struchkov, Yu. T.; Ezhkova, Z. I.; Chayanov,B. A. Kristallografiya, 1982, 27, 477. [7] (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 of theHigh-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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