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

核磁共振动力结构分析方法的进展及其应用

• 批准号: 63470005
• 负责人: TERAO Takehiko
• 金额: $ 5.06万
• 依托单位: KYOTO UNIVERSITY
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for General Scientific Research (B)
• 财政年份: 1988
• 资助国家: 日本
• 起止时间: 1988 至 1989
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-63470005/
• 关键词: SASS; deoxycholic acid; cyclodextrin; ferrocene; chemical shift anisotropy; フェロセン; MM2分子力場計算; SASS; 固体NMR; 2次元粉末スペクトル

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.

利用3DSASS核磁共振技术测量了甲酸钙中两种不等价甲酸盐离子的C-H偶极/C-13化学位移2D粉末图。2D粉末图案显示了微妙的振动诱导的多极耦合张量的不对称性，以及各向异性振动的方向。这一方法对于小幅度运动的研究是有用的。3.提出了利用选择性射频辐射和旋转轴切换来分离获得化学上不同核的单独粉末图案的1D核磁共振技术，与以前的2D方法相比，大大节省了时间。4.用SASS NMR分别观察了包裹在脱氧胆酸中的客体二茂铁分子的C-13化学位移粉末图案。5.用SASS NMR分离观察了客体二茂铁分子和环糊精化合物的C-13化学位移粉末图案。6.对脱氧胆二茂铁和环糊精二茂铁化合物进行了MM2分子力学计算。

项目成果

G. C. Chingas, C. J. Lee, E. Lippmaa, K. T. Mueller, A. Pines, A. Samoson, B. Q. Sun, D. Suter, and T. Terao: "New angles in sample spinning" Proceeding of the XXIV Congress Ampere, Poznan, 1988, D62 (1988).

G. C. Chingas、C. J. Lee、E. Lippmaa、K. T. Mueller、A. Pines、A. Samoson、B. Q. Sun、D. Suter 和 T. Terao：“样品纺丝的新角度”第 24 届安培会议记录，波兹南，1988 年

T.Nakai: J.Chem.Phys.88. 6049-6058 (1988)

T.Nakai：J.Chem.Phys.88。

T.Nakai: "Influence of small-amplitude motions on two-dimensional N.M.R.Powder patterns Anisotropic vibrations in calcium formate" Mol.Phys.67. 839-847 (1989)

T.Nakai：“小振幅运动对甲酸钙中二维 N.M.R.Powder 图案各向异性振动的影响”Mol.Phys.67。

寺尾武彦: "高分子における固体二次元NMR" 高分子. 39. 230-233 (1990)

Takehiko Terao：“聚合物中的固态二维 NMR”Polymer 39. 230-233 (1990)。

T.Yamabe: Phys.Rev.B. 37. 5808-5810 (1988)

T.Yamabe：Phys.Rev.B。