Nitrogen-15 NMR spectra of the complexes and ] , each containing 15N at natural abundance, were obtained by indirect detection (HMQC) using phosphorus as the observed nucleus. Data collection times varied from 4 h to 4 d depending upon the accuracy of the estimated value of 2J(31P,15N) used to opti
Detection of Natural Abundance Nitrogen-15 through Phosphorus-31 Using Pulsed Field Gradients
✍ Scribed by Rodrigo J. Carbajo; Fernando López-Ortiz
- Publisher
- Elsevier Science
- Year
- 2001
- Tongue
- English
- Weight
- 79 KB
- Volume
- 148
- Category
- Article
- ISSN
- 1090-7807
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✦ Synopsis
NMR characterization of natural abundance (15)N in phosphorus-nitrogen compounds can be performed through (31)P using inverse detection methods. When the (31)P-(15)N scalar coupling is small, its observation is greatly disturbed by the residual signal coming from the 99.6% abundant (14)N isotopomer that usually is not completely suppressed by the phase cycle of the sequence. The combined use of pulsed field gradients to suppress this residual signal and the enhanced sensitivity (31)P, (15)N[(1)H]-esHSQC experiment affords artifact-free spectra with good signal-to-noise ratio, which allows the accurate measurement of (15)N NMR parameters such as chemical shifts and coupling constants with the benefits of phosphorus detection.
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