{"title":"rac-4-碘-5-甲氧基[2.2]甲酰脲的晶体结构；一种罕见的具有平面手性的卤代甲环乙烷实例","authors":"Marco Blangetti, D. O’Shea","doi":"10.2116/xraystruct.36.45","DOIUrl":null,"url":null,"abstract":"A racemic mixture of planar chiral 4-iodo-5-methoxy[2.2]metacylophane ( 2 ) was synthesized by the low-temperature directed ortho aryl metalation of 5-methoxy[2.2]metacyclophane ( 1 ) and subsequent in situ reaction with iodine. The crystal structure was determined by the single-crystal X-ray diffraction method at 100 K. The compound crystallized in an orthorhombic system and was characterized as: Pca 2 1 , a = 13.5690(2), b = 14.2212(2), c = 7.5004(1)Å, Z = 4, V = 1447.33(4)Å 3 . The crystal structure was solved by direct methods and refined by full-matrix least-squares","PeriodicalId":23922,"journal":{"name":"X-ray Structure Analysis Online","volume":" ","pages":""},"PeriodicalIF":0.1000,"publicationDate":"2020-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Crystal Structure of rac-4-Iodo-5-methoxy[2.2]metacylophane; A Rare Example of a Halogenated Metacyclophane with Planar Chirality\",\"authors\":\"Marco Blangetti, D. O’Shea\",\"doi\":\"10.2116/xraystruct.36.45\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"A racemic mixture of planar chiral 4-iodo-5-methoxy[2.2]metacylophane ( 2 ) was synthesized by the low-temperature directed ortho aryl metalation of 5-methoxy[2.2]metacyclophane ( 1 ) and subsequent in situ reaction with iodine. The crystal structure was determined by the single-crystal X-ray diffraction method at 100 K. The compound crystallized in an orthorhombic system and was characterized as: Pca 2 1 , a = 13.5690(2), b = 14.2212(2), c = 7.5004(1)Å, Z = 4, V = 1447.33(4)Å 3 . The crystal structure was solved by direct methods and refined by full-matrix least-squares\",\"PeriodicalId\":23922,\"journal\":{\"name\":\"X-ray Structure Analysis Online\",\"volume\":\" \",\"pages\":\"\"},\"PeriodicalIF\":0.1000,\"publicationDate\":\"2020-11-10\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"X-ray Structure Analysis Online\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.2116/xraystruct.36.45\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q4\",\"JCRName\":\"CRYSTALLOGRAPHY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"X-ray Structure Analysis Online","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.2116/xraystruct.36.45","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q4","JCRName":"CRYSTALLOGRAPHY","Score":null,"Total":0}
引用次数: 0
摘要
采用5-甲氧基[2.2]元环烷(1)的低温定向邻芳基金属化反应，与碘原位反应，合成了平面手性4-碘-5-甲氧基[2.2]元环烷(2)的外消旋混合物。在100 K下用单晶x射线衍射法测定了晶体结构。该化合物在正交晶系中结晶，表征为:Pca 21, a = 13.5690(2)， b = 14.2212(2)， c = 7.5004(1)Å， Z = 4, V = 1447.33(4)Å 3。晶体结构采用直接法求解，并用全矩阵最小二乘法进行细化
Crystal Structure of rac-4-Iodo-5-methoxy[2.2]metacylophane; A Rare Example of a Halogenated Metacyclophane with Planar Chirality
A racemic mixture of planar chiral 4-iodo-5-methoxy[2.2]metacylophane ( 2 ) was synthesized by the low-temperature directed ortho aryl metalation of 5-methoxy[2.2]metacyclophane ( 1 ) and subsequent in situ reaction with iodine. The crystal structure was determined by the single-crystal X-ray diffraction method at 100 K. The compound crystallized in an orthorhombic system and was characterized as: Pca 2 1 , a = 13.5690(2), b = 14.2212(2), c = 7.5004(1)Å, Z = 4, V = 1447.33(4)Å 3 . The crystal structure was solved by direct methods and refined by full-matrix least-squares
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