首页|非洛地平新晶型的结构解析及Hirshfeld表面分析

非洛地平新晶型的结构解析及Hirshfeld表面分析

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目的:制备非洛地平新的晶型(晶型Ⅴ),对新晶型的分子构象、晶体堆积和氢键网络进行解析,并对非洛地平晶型Ⅰ及晶型Ⅴ的分子间作用力差异及形成机制进行探究.方法:采用溶剂缓慢挥发法制备非洛地平晶型Ⅴ,通过单晶X射线衍射得到晶型Ⅴ的晶体学参数及三维立体结构,通过红外光谱、拉曼光谱和Hirshfeld表面分析法对2 种晶型的分子间氢键作用力进行分析.结果:单晶X射线衍射分析结果表明,晶型Ⅴ属单斜晶系,P21/c空间群,每个不对称单元包含有一个非洛地平分子,晶胞参数:a =11.252 8Å,b =9.601 8Å,c =16.401 9Å,β =92.688°.Hirshfeld 表面分析结果显示晶型Ⅰ与晶型Ⅴ具有相似的相互作用力,H…H作用力为主要贡献,但各作用力大小之间存在差异.结论:非洛地平分子通过吡啶N原子与甲酯基上的羰基O原子以N1-H1…O2 氢键相连接,Hirshfeld表面分析法可以直观、可视化地揭示晶体结构中各分子间的相互作用.
Hirshfeld surface and structural analysis of new crystal form of felodipine
Objective:To prepare a new crystal form(Form Ⅴ)of felodipine,analyze the molecular conformation,crystal stacking and hydrogen bond network of Form Ⅴ,and explore the intermolecular force difference and formation mechanism between Form Ⅰ and Form Ⅴ of felodipine.Methods:A new crystal form of felodipine(Form Ⅴ)was prepared by solvent slow evaporation method.The crystal parameters and three-dimensional structure of Form Ⅴ were obtained by single crystal X-ray diffraction.The intermolecular hydrogen bond forces of the two forms were analyzed by infrared spectroscopy,Raman spectroscopy and Hirshfeld surface analysis.Results:X-ray diffraction analysis showed that Form Ⅴ belongs to monoclinic system,P21/c space group,and each asymmetric unit contains a felodipine molecule.The unit cell parameters are:a =11.2528Å,b =9.6018Å,c =16.4019Å,β =92.688°.The results of Hirshfeld surface analysis showed that Form Ⅰ and Form Ⅴ have similar interaction force,H…H force is the main contribution,but there are differences among the magnitudes of the forces.Conclusion:Felodipine molecules are connected with carbonyl O atoms on methyl ester groups by N1-H1…O2 hydrogen bonds through pyridine N atoms.Hirshfeld surface analysis can reveal the interaction between molecules in the crystal structure intuitively and visually.

felodipinepolymorphismhydrogen bondHirshfeld surface analysisX ray diffraction analysis

田雅雯、郭伟、孙嘉汝、董雪晴、李元春、杨彩琴

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河北医科大学药学院,石家庄 050017

非洛地平 多晶型 氢键 Hirshfeld表面分析 X射线衍射分析

河北省自然科学基金资助项目

H2020206128

2024

中国新药杂志
中国医药科技出版社 中国医药集团总公司 中国药学会

中国新药杂志

CSTPCD北大核心
影响因子:1.039
ISSN:1003-3734
年,卷(期):2024.33(1)
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