| Project/Area Number |
04453014
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| Research Category |
Grant-in-Aid for General Scientific Research (B)
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| Allocation Type | Single-year Grants |
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| Research Field |
構造化学
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| Research Institution | KYOTO UNIVERSITY |
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Principal Investigator |
TERAO Takehiko Kyoto Univ.Science, Professor, 理学部, 教授 (50093274)
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| Co-Investigator(Kenkyū-buntansha) |
KUBO Atushi Kyoto Univ.Science, Instructor, 理学部, 助手 (20205115)
IMASHIRO Fumio Kyoto Univ.Science, Instructor, 理学部, 助手 (30108980)
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| Project Period (FY) |
1992 – 1993
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| Project Status |
Completed (Fiscal Year 1993)
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| Budget Amount *help |
¥7,200,000 (Direct Cost: ¥7,200,000)
Fiscal Year 1993: ¥1,000,000 (Direct Cost: ¥1,000,000)
Fiscal Year 1992: ¥6,200,000 (Direct Cost: ¥6,200,000)
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| Keywords | 2D solid state NMR / chemical shift tensor |
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| Research Abstract |
1. The NMR spectrometer was improved for measurements of two-dimensional wideline spectra. Asimulation program was developed for analyzing two-dimensional wideline spectra.
2. Amethod for measurements of two-dimensional wideline spectra due to the chemical shift tensors of two C^<13>N nuclei and their dipolar interactions was developed. It was applied to DL-mandelic acid with 10%-doubly-enriched methin and carboxyl carbons ; the principal values and principal axis directions of the two chemical shift tensors and the bond length between the two carbons were obtained from the experiment and the spectral simulation.
3. A general simulation program was developed by which spectra or magnetization behavior of a homonuclear or heteronuclear system in a static (powder or single crystal) or rotating sample for various pulse sequences (involving finite pulse width effects) of 1D or 2D NMR can be calculated without approximation theories.
4. In the cholic acid inclusion compound enclathrating gamma-valerolactone with C^<13>N-enriched methyl, two-dimensional exchange NMR was done ; cross peaks between the C^<13>NH_3 signals of the S and R enantiomers of gamma-valerolactone were observed. This origin was concluded to be spin diffusion between the two enantiomers. This fact indicates that the S and R enantiomers are microscopically mixed in the cholic acid channels, denying the reported result of X-ray diffraction that only the S enantiomer is enclathrated.
5. The two-dimensional C^<13>N chemical shift/C-H dipolar powder pattern of enriched indole-4 carbon in L-tryptophan was measured under off-magic angle spinning. From the results, the principal values and principal axis directions of the C^<13>N chemical shift tensor and the C-H bond distances were determined.
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