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Related Concept Videos

Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or radiofrequency pulses to manipulate and observe two distinct nuclear spins. One important application of double resonance is spin decoupling, which selectively suppresses coupling with one type of nucleus while observing the NMR signal from another nucleus, simplifying the spectrum and enhancing resolution.
Spin decoupling is usually achieved by...
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When protons A and X are coupled, their nuclear spin energy levels are slightly modified. This is because the energy required to excite proton A to a spin state parallel to proton X is slightly different from the energy required for it to become anti-parallel to spin X. Consequently, there are two possible excitation frequencies for A (A1 and A2), depending on the spin state of X, and vice versa. The mutual nature of coupling implies that the difference between frequencies A1 and A2, indicated...
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Interpreting ¹H NMR Signal Splitting: The (n + 1) Rule01:10

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In the AX proton spin system, proton A can sense the two spin states of a coupled proton X, resulting in a doublet NMR signal with two peaks of equal (1:1) intensity. When proton A is coupled to two equivalent protons (AX2 spin system), the spin states of each X can be aligned with or against the external field, creating three possible scenarios. This results in a 1:2:1  triplet signal, where the central peak corresponds to the chemical shift of A and is twice as large or intense as the...
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Nuclear Overhauser Enhancement (NOE)01:07

Nuclear Overhauser Enhancement (NOE)

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Irradiation of a spin-active nucleus causes an increase or decrease in the signal intensity of neighboring nuclei that are not necessarily chemically bonded or involved in J-coupling.  This phenomenon, called the Nuclear Overhauser Enhancement (NOE), results from through-space interactions between the nuclear spins. The NOE effect decreases with increasing internuclear distance and is generally not observed beyond 4 angstroms. In NOE, dipole-dipole interactions between neighboring...
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A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
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Insensitive Nuclei Enhanced by Polarization Transfer (INEPT)01:15

Insensitive Nuclei Enhanced by Polarization Transfer (INEPT)

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Insensitive Nuclei Enhanced by Polarization Transfer (INEPT) is an advanced Nuclear Magnetic Resonance (NMR) technique specifically designed to detect and enhance the signals of low-abundance nuclei, such as carbon-13 and nitrogen-15, in small molecules. The fundamental principle behind INEPT is the transfer of polarization from a more abundant and highly polarizable nucleus, typically hydrogen-1, to the low-abundance nucleus of interest. This process effectively boosts the NMR signal of the...
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Aldoximes enable proton-relayed NMR hyperpolarisation.

Naomi E Leydman1, Philip L Norcott1

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Chemical Communications (Cambridge, England)
|August 19, 2024
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Para-hydrogen interactions can hyperpolarise Nuclear Magnetic Resonance (NMR) signals. This study shows oximes coordinated to iridium can be reversibly hyperpolarised, with geometry impacting activity, and signals transferred via proton exchange.

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Area of Science:

  • Chemistry
  • Nuclear Magnetic Resonance Spectroscopy
  • Catalysis

Background:

  • Nuclear Magnetic Resonance (NMR) signal enhancement is crucial for improving sensitivity in various applications.
  • Para-hydrogen (PH) is a valuable precursor for hyperpolarisation techniques, enabling significant signal amplification.
  • Oximes are versatile organic compounds with potential applications in catalysis and sensing.

Purpose of the Study:

  • To investigate the hyperpolarisation of oximes using para-hydrogen and an iridium catalyst.
  • To determine the influence of oxime E/Z geometry on the hyperpolarisation process.
  • To explore the signal transfer capabilities of hyperpolarised oximes via proton exchange.

Main Methods:

  • Coordination of oximes to an iridium complex.
  • Hyperpolarisation of the coordinated oximes using para-hydrogen.
  • Analysis of NMR signal enhancement and relaxation times.
  • Investigation of E/Z isomer effects on hyperpolarisation efficiency.
  • Proton exchange experiments to assess signal transfer.

Main Results:

  • Oximes can be reversibly hyperpolarised through coordination to an iridium complex.
  • The E/Z geometry of the oxime significantly impacts the hyperpolarisation activity.
  • Hyperpolarised oximes successfully transferred enhanced signals via proton exchange.
  • The iridium-oxime system demonstrated efficient and reversible hyperpolarisation.

Conclusions:

  • Iridium-catalysed para-hydrogen hyperpolarisation is effective for oximes.
  • Oxime geometry is a critical factor in achieving efficient hyperpolarisation.
  • Hyperpolarised oximes can act as transient sources of enhanced NMR signals, with potential for broader applications.