Developments of analytical methods of dynamical structures by NMR and their applications

1.研制了本课题所需的探针和计算机软件。2.用3DSASS NMR方法测量了甲酸钙中两个不等价甲酸根离子的C-H偶极/C-13化学位移二维粉末谱。2D粉末图案可视化了偶极耦合张量的微妙振动诱导的不对称性和各向异性振动的方向。这种方法对于小振幅运动的研究是有用的。3.提出了使用选择性射频照射和旋转器轴的切换来分别获得化学上不同的核的单独粉末图案的1D NMR技术，与以前的二维方法相比，这大大节省了时间。用SASS NMR分别观察到客体二茂铁分子包合在脱氧胆酸中的位移谱。用SASS NMR分别观察到包合的客体二茂铁分子和环糊精包合物的粉末位移谱。6.对脱氧胆酸-二茂铁包合物和环糊精-二茂铁包合物进行了MM 2分子力学计算。

l.A probe and a computer software necessary for this project were made.2.The C-H dipolar/C-13 chemical shift 2D powder patterns for the two inequivalent formate ions in calcium formate were measured using 3D SASS NMR. The 2D powder pattern visualizes the subtle vibtationally- induced asymmetry of the dopolar coupling tensor, and the direction of anisotropic vibtaion. This approach is useful for studies of small- amplitude motions.3.lD NMR techniques for separately obtaining individual powder patterns for chemically distinct nuclei using selective rf irradiation and switching of the spinner axis are proposed, which considerably save time compared with the previous 2D approaches.4.The C-13 chemical-shift powder pattern of guest ferrocene molecule enclathrated in deoxycholic acid was separately observed by SASS NMR.5.The C-13 chemical-shift powder patterns of the guest ferrocene molecules enclathrated in and cyclodextrin compounds were separatel observed by SASS NMR.6.MM2 molecular mechanics calculations for deoxycholic-ferrocene and cyclodextrin-ferrocene inclusion compounds were performed.