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来自62年晶体的(3a,5,7a,7b,9a,10,12a,12b)-7b-羟基-4,4,7a,9a,12a-五甲基-10-[(2')-6-甲基庚-2-基]-2,8,9-三氧代-十八氢苯并[]茚并-[4,5-]氮杂环庚三烯-5-基乙酸酯的绝对结构

Absolute structure of (3a,5,7a,7b,9a,10,12a,12b)-7b-hy-droxy-4,4,7a,9a,12a-penta-methyl-10-[(2')-6-methyl-heptan-2-yl]-2,8,9-trioxo-octa-deca-hydro-benzo[]indeno-[4,5-]azepin-5-yl acetate from 62-year-old crystals.

作者信息

Suescun Leopoldo, Heinzen Horacio

机构信息

Cryssmat-Lab/DETEMA, Facultad de Química, Universidad de la República, Av., Gral., Flores 2124, Montevideo 11800, Uruguay.

Departamento de Química Orgánica, Facultad de Química, Universidad de la República, Av. Gral. Flores 2124, Montevideo 11800, Uruguay.

出版信息

Acta Crystallogr E Crystallogr Commun. 2019 Aug 23;75(Pt 9):1348-1351. doi: 10.1107/S205698901901140X. eCollection 2019 Sep 1.

Abstract

The structure of the title compound, CHNO, was determined from 62-year-old crystals at room temperature and refined with 100 K data in a monoclinic (2) space group. This compound with a triterpenoid structure, now confirmed by this study, played an important role in the determination of the structure of lanosterol. The mol-ecules pack in linear O-H⋯O hydrogen-bonded chains along the short axis (), while parallel chains display weak van der Waals inter-actions that explain the needle-shaped crystal morphology. The structure exhibits disorder of the flexible methyl-heptane chain at one end of the main mol-ecule with a small void around it. Crystals of the compounds were resistant to data collection for decades with the available cameras and Mo α radiation single-crystal diffractometer in our laboratory until a new instrument with Cu α radiation operating at 100 K allowed the structure to be solved and refined.

摘要

标题化合物CHNO的结构是在室温下从62年的晶体中确定的,并在单斜晶系(2)空间群中用100K数据进行了精修。这种具有三萜结构的化合物,现已被本研究证实,在羊毛甾醇结构的确定中发挥了重要作用。分子沿短轴()以线性O-H⋯O氢键链堆积,而平行链显示出弱范德华相互作用,这解释了针状晶体形态。该结构在主分子一端的柔性甲基庚烷链处表现出无序,周围有一个小空隙。在我们实验室中,几十年来,使用现有的相机和钼α辐射单晶衍射仪对该化合物的晶体进行数据收集时都遇到了困难,直到一台在100K下运行的具有铜α辐射的新仪器才使得该结构得以解析和精修。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/340d/6727055/e475971edecd/e-75-01348-fig1.jpg

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