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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29 案例88： 本来是按照如图88所示（由ChemBioDraw[1]绘制），在催化剂的作用下使化合物A和化合物B反应生成化合物C，然而实验后处理完，培养晶体进行单晶X射线衍射（SC-XRD,single-crystal X-ray diffraction）实验得到晶体数据，经结构解析发现该晶体结构为单质硫/硫单质 [2]（S8, Octathiocane, CAS: 10544-50-0.CCDC [3]: 1161500[2a], 1161501 [2b],267383 [2c], 757275 [2d],1161502-1161505 [2d], 757277 [2e], 856708 [2f],862658 [2g], 1555239 [2h], 1555240[2i], 1934705 [2j],1947735 [2k], 1992592 [2l], 2015061 [2m],1992592 [2n], 2097464 [2o], 2241156 [2p],2267093 [2q], 2150895 [2r], 2082127 [2s],2339024 [2t], 2415401 [2u], 930773 [2v],2474521 [2w], 2588694 [2x],2589570 [2y]），可能是反应中的副产物。
▲图88 案例88反应示意图 相关视频： 单晶结构解析练习791(非预期结构)：https://www.bilibili.com/video/BV1ybeB6iE1t 案例89： 本来是按照如图89所示，利用四水合硝酸镉（Cd(NO3)2·4H2O, Cadmium nitrate tetrahydrate, CAS: 10022-68-1）和配体反应以N,N-二甲基甲酰胺 [4]（DMF, N,N-dimethylformamide,CAS: 68-12-2, CCDC: 102756 [4a], 1869635–1869638[4b], 1869744–1869752 [4b]）和水[5]（H2O, water, CAS: 7732-18-5, CCDC: 2080050–2080051）作为溶剂在一定条件下反应，以期得到含该配体的镉配合物，然而所得红棕色晶体经SC-XRD实验得到晶体数据，经结构解析发现该晶体结构为碳酸镉 [6]（CdCO3, Cadmium carbonate, CAS: 513-78-0, CCDC:156740 [6a], 156755[6a], 20181 [6b], 33662 [6c], 2589924[6d]），其中碳酸根可能来自DMF分解产生（参阅推文“DMF和DEF会为晶体结构带来什么”），也可能是空气中二氧化碳（CO2, Carbon dioxide, CAS: 124-38-9）进入体系中生成。
▲图89 案例89反应示意图 相关视频： 单晶结构解析练习795(CAP数据还原-非预期结构-非正定)：https://www.bilibili.com/video/BV1RhaP6JEi2 案例90： 本来是按照如图90所示，利用氯(二甲基硫化)金(I)/氯化(二甲硫醚)金(I) [7]（Me2SAuCl, Chloro(dimethyl sulfide)gold(I), CAS: 29892-37-3,CCDC: 1169763 [7a], 2116322–2116324 [7b], 2426918 [7c]）和双(对甲氧基苯基)氧化膦（Bis(4-methoxyphenyl)phosphineoxide, CAS: 15754-51-5）以及其他成分以甲苯 [8]（Tol,toluene, CAS: 108-88-3, CCDC: 1273751 [8a], 1273752 [8b], 1273753 [8c], 725245 [8d], 1430464–1430470 [8e], 2377542 [8f]）和正己烷[9]（C6H14, n-hexane,CAS: 110-54-3, CCDC: 103189）作为溶剂在一定条件下反应，以期得到多核金簇合物，然而所得晶体经SC-XRD实验得到晶体数据，经结构解析发现该晶体结构为双核金化合物。
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