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Related Concept Videos

¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR01:15

¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR

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The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one proton, the remaining eleven protons are replaced by deuterium. The deuterium substitution avoids the possible peak splitting caused by the spin-spin coupling between the adjacent protons. The remaining proton flips between the axial and equatorial positions.
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¹H NMR: Complex Splitting01:13

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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.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied...
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2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)01:19

2D NMR: Heteronuclear Single-Quantum Correlation Spectroscopy (HSQC)

1.4K
Heteronuclear single-quantum correlation spectroscopy (HSQC) is a 2D NMR technique that reveals one-bond correlations between hydrogen and a heteronucleus. The HSQC experiment is similar to the heteronuclear correlation experiment (HETCOR) but is more sensitive. In the HSQC spectrum, the proton chemical shift is plotted on the horizontal F2 axis, while the 13C chemical shift is plotted on the vertical F1 axis. The corresponding proton and 13C spectra are also shown. The HSQC contour plot does...
1.4K
¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)01:20

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1.6K
When proton-coupled carbon-13 spectra are simplified by a broadband proton decoupling technique, structural information about the coupled protons is lost. Distortionless enhancement by polarization transfer (DEPT) is a technique that provides information on the number of hydrogens attached to each carbon in a molecule. While the DEPT experiment utilizes complex pulse sequences, the pulse delay and flip angle are specifically manipulated. The resulting signals have different phases depending on...
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NMR Spectroscopy: Chemical Shift Overview01:15

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3.1K
The position of the absorption signal of a sample is reported relative to the position of the signal of tetramethylsilane (TMS), which is added as an internal reference while recording spectra. The difference between the absorption frequencies of the sample and TMS (in Hz) is divided by the spectrometer operating frequency (in MHz) to obtain a dimensionless quantity called the chemical shift. It is reported on the δ (delta) scale and expressed in parts per million.
For instance, the proton...
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¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution

1.3K
At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the...
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Discerning two-dimensional metal halide perovskite moieties using solid-state NMR fingerprints.

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Solid-state NMR spectroscopy (ssNMR) reveals distinct spectral fingerprints for low-dimensional perovskites. This technique differentiates structural motifs, aiding the development of advanced optoelectronic materials.

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Area of Science:

  • Materials Science
  • Solid-State Chemistry
  • Spectroscopy

Background:

  • Low-dimensional perovskites are promising for optoelectronics.
  • Their electronic properties depend on crystal structure and molecular packing.
  • Understanding inorganic connectivity is key for material improvement.

Purpose of the Study:

  • To compare the structural motifs of two perovskites using ssNMR.
  • To elucidate the relationship between ssNMR response and perovskite structure.
  • To highlight ssNMR as a complementary characterization technique.

Main Methods:

  • Solid-state NMR (ssNMR) spectroscopy on Ruddlesden-Popper and Dion-Jacobson phases.
  • Static and magic angle spinning conditions up to 42 kHz.
  • Spin relaxation time measurements and DFT calculations.

Main Results:

  • ssNMR (13C, 15N, 207Pb) provides unique spectral fingerprints for different perovskite connectivities.
  • Distinct spectra correlate with specific inorganic framework arrangements.
  • ssNMR effectively distinguishes between flat and corrugated layered perovskites.

Conclusions:

  • ssNMR offers a deeper understanding of 2D perovskite structural variations.
  • This technique is valuable for identifying local spatial arrangements in perovskites.
  • ssNMR complements traditional diffraction methods for perovskite characterization.