...
  • 主题
高级搜索  >
历史搜索 清空历史
首页> 外文期刊>The journal of physical chemistry, B. Condensed matter, materials, surfaces, interfaces & biophysical >Solid-State NMR Analysis of a Complex Crystalline Phase of Ronacaleret Hydrochloride
【24h】

Solid-State NMR Analysis of a Complex Crystalline Phase of Ronacaleret Hydrochloride

机译：盐酸罗纳卡莱特复合晶体相的固态NMR分析

获取原文
获取原文并翻译 | 示例
           
页面导航
  • 摘要
  • 著录项
  • 相似文献
  • 相关主题

摘要

A crystalline phase of the pharmaceutical compound ronacaleret hydrochloride is studied by solid-state nuclear magnetic resonance (SSNMR) spectroscopy and single-crystal X-ray diffraction. The crystal structure is determined to contain two independent cationic molecules and chloride anions in the asymmetric unit, which combine with the covalent structure of the molecule to yield complex SSNMR spectra. Experimental approaches based on dipolar correlation, chemical shift tensor analysis, and quadrupolar interaction analysis are employed to obtain detailed information about this phase. Density functional theory (DFT) calculations are used to predict chemical shielding and electric field gradient (EFG) parameters for comparison with experiment. ~1H SSNMR experiments performed at 16.4 T using magic-angle spinning (MAS) and homonuclear dipolar decoupling provide information about hydrogen bonding and molecular connectivity that can be related to the crystal structure. ~(19)F and ~(13)C assignments for the Z' = 2 structure are obtained using DFT calculations, ~(19)F homonuclear dipolar correlation, and ~(13)C—~(19)F heteronuclear dipolar correlation experiments. ~(35)C1 MAS experiments at 16.4 T observe two chlorine sites that are assigned using calculated chemical shielding and EFG parameters. SSNMR dipolar correlation experiments are used to extract ~1H-~(13)C, ~1H-~(15)N, ~1H~(19)F, ~(13)C-~(19)F, and ~1H-~(35)Cl through-space connectivity information for many positions of interest. The results allow for the evaluation of the performance of a suite of SSNMR experiments and computational approaches as applied to a complex but typical pharmaceutical solid phase.
机译：通过固态核磁共振（SSNMR）光谱和单晶X射线衍射研究了药用化合物盐酸罗卡那利的结晶相。确定晶体结构在不对称单元中包含两个独立的阳离子分子和氯阴离子，它们与分子的共价结构结合以产生复杂的SSNMR光谱。采用基于偶极相关性，化学位移张量分析和四极相互作用分析的实验方法来获得有关该相的详细信息。密度泛函理论（DFT）计算用于预测化学屏蔽和电场梯度（EFG）参数，以便与实验进行比较。使用魔角旋转（MAS）和同核偶极解耦在16.4 T下进行的〜1H SSNMR实验提供了有关氢键和与晶体结构相关的分子连接性的信息。使用DFT计算，〜（19）F同核偶极相关性和〜（13）C ~~（19）F异核偶极相关性实验获得Z'= 2结构的〜（19）F和〜（13）C分配。 。在16.4 T的〜（35）C1 MAS实验中观察到两个氯位点，这些位点是使用计算出的化学屏蔽和EFG参数分配的。 SSNMR偶极相关实验用于提取〜1H-〜（13）C，〜1H-〜（15）N，〜1H〜（19）F，〜（13）C-〜（19）F和〜1H- 〜35个Cl的空间连通性信息，用于许多感兴趣的位置。结果允许评估应用于复杂但典型的药物固相的一系列SSNMR实验和计算方法的性能。

著录项

相似文献

  • 外文文献
  • 中文文献
  • 专利
获取原文

客服邮箱：kefu@zhangqiaokeyan.com

京公网安备：11010802029741号 ICP备案号：京ICP备15016152号-6 六维联合信息科技 (北京) 有限公司©版权所有

  • 客服微信

  • 服务号