sup 13 C- sup 31 P cross polarization between isolated spin pairs in organophosphorus substances: Intramolecular structure and internuclear distance determinations in spinning solids

Cross polarization between dilute effectively isolated {sup 13}C-{sup 31}P spin pairs provides a unique method to examine selectively the microenvironment around the phosphorus atom in organophosphorus substances. Strong oscillations occur during cross polarization between these isolated spin pairs...

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Bibliographic Details
Published in:Journal of the American Chemical Society 1990-10, Vol.112:21
Main Authors: Hagaman, E.W., Ho, P.C., Brown, L.L., Schell, F.M., Woody, M.C.
Format: Article
Language:English
Subjects:
400201 - Chemical & Physicochemical Properties
656002 - Condensed Matter Physics- General Techniques in Condensed Matter- (1987-)
CALCULATION METHODS
CARBON 13
CARBON ISOTOPES
CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY
DATA
DISPERSIONS
EVEN-ODD NUCLEI
EXPERIMENTAL DATA
INFORMATION
INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY
ISOTOPES
LIGHT NUCLEI
MAGNETIC RESONANCE
MIXTURES
NUCLEAR MAGNETIC RESONANCE
NUCLEI
NUMERICAL DATA
ODD-EVEN NUCLEI
ORGANIC COMPOUNDS
ORGANIC PHOSPHORUS COMPOUNDS
PHOSPHORUS 31
PHOSPHORUS ISOTOPES
RESONANCE
SOLID SOLUTIONS
SOLUTIONS
STABLE ISOTOPES
STRUCTURAL CHEMICAL ANALYSIS
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Summary:Cross polarization between dilute effectively isolated {sup 13}C-{sup 31}P spin pairs provides a unique method to examine selectively the microenvironment around the phosphorus atom in organophosphorus substances. Strong oscillations occur during cross polarization between these isolated spin pairs in MAS experiments on microcrystalline powders. The oscillation frequency is proportional to the {sup 13}C-{sup 31}P dipolar interaction and hence allows specific internuclear distance determinations on powder samples. Maximum carbon signal intensity and experimental simplicity are achieved in double cross polarization (DCP)/MAS {sup 13}C NMR experiments that impose a short T{sub 1p} on the {sup 31}P magnetization by {sup 31}P radio frequency phase modulation. This experimental stratagem suppresses cross-polarization oscillations and yields simple exponential kinetics for the transfer process. It also relaxes the tolerance on the match condition and MAS speed for cross polarization between weakly coupled dipole pairs.
ISSN:0002-7863
1520-5126
DOI:10.1021/ja00177a001