Developments of SASS-NMR methods and the spectrometer

SASS-NMR方法和光谱仪的发展

• 批准号: 63840015
• 负责人: TERAO Takehiko
• 金额: $ 8.7万
• 依托单位: KYOTO UNIVERSITY
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Developmental Scientific Research
• 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-63840015/
• 关键词: SASS; powder pattern; chemical shift anisotropy; ferrocene; Powder Pattern; 固体NMR; SASS法

1.A spectrometer for SASS-NMR was built.2.Computer programs for execution of SASS-NMR, control of various systems, and data manipulation were made. A simulation program of 1D and 2D powder patterns were also made for the data analysis.3.SASS-NMR was successfully performed-using a test sample.4.3D SASS-NMR was developed, which was applied to study small vibrations in calcium formate.5.lD SASS-NMR techniques for separately obtaining individual powder patterns for chemically distinct nuclei using selective rf irradiation and switching of the spinner axis were proposed, which considerably save time compared with the previous 2D approaches. A method has been applied for simultaneously obtaining all of the C-1 chemical -shift powder patterns in p-diacetylbenzene.6.The individual powder patterns due to C-13 chemical shift anisotropy in guest ferrocene molecules of , , and cyclodextrin-ferrocene clathrates were separately obtained using SASS-NMR. Enclathrated ferrocene molecules were concluded to undergo C5 rotation. precessio and libration.

1.建立了SASS-NMR谱仪。编写了SASS-NMR的计算机程序，控制各种系统和数据操作。并编制了一维和二维粉末形貌的仿真程序进行数据分析。使用测试样品成功地进行了SASS-NMR。开发了3d SASS-NMR，用于研究钙形成中的微小振动。提出了利用选择性射频辐照和旋转轴开关分别获得化学不同核的单独粉末模式的lD SASS-NMR技术，与以前的二维方法相比，该技术大大节省了时间。采用了一种同时得到对二乙酰苯中所有C-1化学位移粉末模式的方法。利用SASS-NMR分别获得了二茂铁客体分子中由于C-13化学位移各向异性而形成的粉末模式。包合的二茂铁分子进行了C5旋转。进动和振动。

项目成果

T. Yamabe, S. Yamanaka, K. Tanaka, T. Terao, S. Maeda, and S. Yata: "^<13>C solid-state NMR study of polyacenic materials" Phys. Rev. B37, 5808 (1988).

T. Yamabe、S. Yamanaka、K. Tanaka、T. Terao、S. Maeda 和 S. Yata：“多并苯材料的^ 13 C 固态核磁共振研究” Phys。

F. Imashiro, D. Kuwabara, T. Nakai, and T. Terao: "Study on conformations of n-alkanes in urea inclusion compounds using CH dipolar switching-angle sample spinning nuclear magnetic resonance and MM2 molecular mechanics calculations" J. Chem. Phys., 90, 33

F. Imashiro、D. Kuwabara、T. Nakai 和 T. Terao：“利用 CH 偶极转换角样品旋转核磁共振和 MM2 分子力学计算研究尿素包合物中正烷烃的构象” J. Chem。

T.Nakai: Chem.Phys.Lett.145. 90-94 (1988)

T.Nakai：化学物理快报145。

T.Yamabe: "^<13>C Solid-state NMR Study of polyacenic materials" Phys.Rev.B. 37. 5808-5810 (1988)

T.Yamabe：“多并苯材料的^ 13 C固态NMR研究”Phys.Rev.B。

T. Nakai, T. Terao, H. Shirakawa: "Determination of ^<13>C chemical shift tensor orientations in cis and trans polyacetylene by measurements of two-dimensional NMR powder patterns in rotating solids" Chem. Phys. Lett., 145, 90 (1988).

T. Nakai、T. Terao、H. Shirakawa：“通过测量旋转固体中的二维NMR粉末图案来确定顺式和反式聚乙炔中的^ 13 C化学位移张量取向”Chem。