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洛哌丁胺一水合物的重新测定。

Redetermination of loperamide monohydrate.

作者信息

Jasinski Jerry P, Guild Curtis J, Dayananda A S, Yathirajan H S, Ramesha A R

出版信息

Acta Crystallogr Sect E Struct Rep Online. 2012 Feb 1;68(Pt 2):o539-40. doi: 10.1107/S1600536812003091. Epub 2012 Jan 31.

Abstract

The structure of the title compound {systematic name: 4-[4-(4-chloro-phen-yl)-4-hy-droxy-piperidin-1-yl]-N,N-dimethyl-2,2-di-phenyl-butanamide monohydrate}, C(29)H(33)ClN(2)O(2)·H(2)O, has been redetermined at 170 (2) K. The redetermination is of significantly higher precision than the previous structure determination at room temperature and includes the H-atom coordinates that were not included in the previous report [Germain et al. (1977 ▶). Acta Cryst. B33, 942-944]. It consists of a piperidin-1-yl ring in a distorted chair conformation, with the N,N-dimethyl-α,α-diphenyl-butyramide and the 4-chloro-phenyl and hy-droxy groups bonded in para positions and an external water mol-ecule within the asymmetric unit. The dihedral angles between the mean plane of the piperidine ring and the 4-chloro-phenyl and two benzene rings are 83.4 (5), 76.4 (2) and 85.9 (2)°, respectively. The two benzene rings are inclined to one another by 50.8 (6)°. In the crystal, mol-ecules are linked by O-H⋯O and O-H⋯N hydrogen bonds and weak C-H⋯O intermolecular interactions, forming an infinite two-dimensional network along [110].

摘要

标题化合物{系统名称:4-[4-(4-氯苯基)-4-羟基哌啶-1-基]-N,N-二甲基-2,2-二苯基丁酰胺一水合物},C(29)H(33)ClN(2)O(2)·H(2)O的结构已在170(2)K下重新测定。此次重新测定的精度明显高于之前在室温下的结构测定,且包括了之前报告中未包含的H原子坐标[Germain等人(1977 ▶)。Acta Cryst. B33, 942 - 944]。它由一个处于扭曲椅式构象的哌啶-1-基环组成,N,N-二甲基-α,α-二苯基丁酰胺以及4-氯苯基和羟基连接在对位,不对称单元内还有一个外部水分子。哌啶环的平均平面与4-氯苯基和两个苯环之间的二面角分别为83.4(5)、76.4(2)和85.9(2)°。两个苯环彼此倾斜50.8(6)°。在晶体中,分子通过O-H⋯O和O-H⋯N氢键以及弱的C-H⋯O分子间相互作用相连,沿[110]形成无限二维网络。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/495d/3275278/26178f36de95/e-68-0o539-fig1.jpg

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