Petr A. Buikin, Alexander Korlyukov, Elizaveta Kulikova, Roman Novikov, A. Vologzhanina
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引用次数: 0
摘要
利用固态 15N、13C 和 35Cl NMR 光谱以及多温同步 X 射线粉末衍射技术,我们获得了盐酸利匹韦林的单斜 C 型 (N6H19C22)Cl,并对其进行了表征。标题化合物在室温(295.0(2) K)和低温(100.0(2) K)下均为单斜晶系(空间群 C2/c,#15)结晶。在室温下,其参数如下:a = 19.43051(3),b = 13.09431(14),c = 17.10254(18)埃,β = 109.3937(7),V = 4104.48(9)埃3,Z = 8。阳离子的折叠分子构象与游离碱基 rilpivirine 相似,但氰基乙烯基的布局除外。阴离子利用 N-H⋯Cl 键将阳离子连接到平行于晶体学 c 轴的无限链上,其中氨基和质子化的嘧啶环都参与了 H 键连接。粉末图样已提交给国际粉末衍射中心(ICDD),以便纳入粉末衍射文件™ (PDF®)。
Crystal structure of rilpivirine hydrochloride, N6H19C22Cl
A monoclinic C form of rilpivirine hydrochloride, (N6H19C22)Cl, has been obtained and characterized using solid-state 15N, 13C, and 35Cl NMR spectroscopy and multitemperature synchrotron X-ray powder diffraction. The title compound crystallizes in the monoclinic system (space group C2/c, #15) at both room (295.0(2) K) and low (100.0(2) K) temperatures. At room temperature, the following parameters are a = 19.43051(3), b = 13.09431(14), c = 17.10254(18) Å, β = 109.3937(7), V = 4104.48(9) Å3, and Z = 8. The folded molecular conformation of the cation is similar with that of free base rilpivirine with the exception of cyanovinyl group disposition. The anion links cations to infinite chains parallel to the crystallographic c axis using N–H⋯Cl bonds where both amino groups and the protonated pyrimidine ring take part in the H-bonding. The powder patterns have been submitted to the ICDD for inclusion in the Powder Diffraction File™ (PDF®).
期刊介绍:
Powder Diffraction is a quarterly journal publishing articles, both experimental and theoretical, on the use of powder diffraction and related techniques for the characterization of crystalline materials. It is published by Cambridge University Press (CUP) for the International Centre for Diffraction Data (ICDD).