Probing 15N-15N Correlations in g-C3N4 Samples with Solid-State NMR SHA+ Pulse Sequence

doi:10.11938/cjmr20160301

Abstract

Abstract:

The performance of solid-state NMR proton-driven spin-diffusion (PDSD) and second-order Hamiltonian among analogous nuclei plus (SHA+) sequences for probing ¹⁵N-¹⁵N through-space correlations in ¹⁵N-labelled g-C₃N₄ samples were compared at high magnetic fields with moderate magic angle spinning (MAS) frequencies. It was found that, relative to the PDSD sequence, the SHA+ sequence is more efficient in terms of yielding polarization transfer between the ¹⁵N atoms as long as one of the nitrogen atoms bonds to protons. The results are useful in guiding the choice of solid-state nuclear magnetic resonance (SS-NMR) sequences for studying nitrogen-doped carbon-based materials.

Key words: solid-state nuclear magnetic resonance (SS-NMR), homo-nuclear correlation, long-range correlation, SHA+

CLC Number:

O482.53

YAN Xiao-jing, HU Bing-wen. Probing ¹⁵N-¹⁵N Correlations in g-C₃N₄ Samples with Solid-State NMR SHA+ Pulse Sequence[J]. Chinese Journal of Magnetic Resonance, 2016, 33(3): 361-367.

References

[1] Castellani F, van Rossum B, Diehl A, et al. Structure of a protein determined by solid-state magic-angle-spinning NMR spectroscopy[J]. Nature, 2002, 420(6 911): 98-102.

[2] Lange A, Becker S, Seidel K, et al. A concept for rapid protein-structure determination by solid-state NMR spectroscopy[J]. Angew Chem Int Ed Engl, 2005, 44(14): 2 089-2 092.

[3] Wasmer C, Lange A, van Melckebeke H, et al. Amyloid fibrils of the HET-s (218-289) Prion form a b solenoid with a triangular hydrophobic core[J]. Science, 2008, 319(5 869): 1 523-1 526.

[4] Lange A, Giller K, Hornig S, et al. Toxin-induced conformational changes in a potassium channel revealed by solid-state NMR[J]. Nature, 2006, 440(7 086): 959-962.

[5] Renault M, Cukkemane A, Baldus M. Solid-state NMR spectroscopy on complex biomolecules[J]. Angew Chem Int Ed Engl, 2010, 49(45): 8 346-8 357.

[6] Hong M, Zhang Y, Hu F H. Membrane protein structure and dynamics from NMR spectroscopy[J]. Annu Rev Phys Chem, 2012, 63: 1-24.

[7] Tycko R. Solid-state NMR studies of amyloid fibril structure[J]. Annu Rep Phys Chem, 2011, 62: 279-299.

[8] Takegoshi K, Nakamura S, Terao T. ¹³C-¹H dipolar-assisted rotational resonance in magic-angle spinning NMR[J]. Chem Phys Lett, 2001, 344(5): 631-637.

[9] Takegoshi K, Nakamura S, Terao T. ¹³C-¹H dipolar-driven ¹³C-¹³C recoupling without ¹³C rf irradiation in nuclear magnetic resonance of rotating solids[J]. J Chem Phys, 2003, 118(5): 2 325-2 341.

[10] Weingarth M, Masuda Y, Takegoshi K, et al. Sensitive ¹³C-¹³C correlation spectra of amyloid fibrils at very high spinning frequencies and magnetic fields[J]. J Biomol NMR, 2011, 50(2): 129-136.

[11] Weingarth M, Bodenhausen G, Tekely P. Broadband carbon-13 correlation spectra of micro crystalline proteins in very high-magnetic fields[J]. J Am Chem Soc, 2009, 131(39): 13 937-13 939.

[12] Weingarth M, Demco D E, Bodenhausen G, et al. Improved magnetization transfer in solid-state NMR with fast magic angle spinning[J]. Chem Phys Lett, 2009, 469(4, 5, 6): 342-348.

[13] Hu B W, Lafon O, Trébosc J, et al. Broad-band homo-nuclear correlations assisted by ¹H irradiation for bio-molecules in very high magnetic field at fast and ultra-fast MAS frequencies[J]. J Magn Reson, 2011, 212(2): 320-329.

[14] Hu B W, Trébosc J, Lafon O, et al. Very-long-distance correlations in proteins revealed by solid-state NMR spectroscopy[J]. Chem Phys Chem, 2012, 13(16): 3 585-3 588.

[15] Scholz I, van Beek J D, Ernst M. Operator-based Floquet theory in solid-state NMR[J]. Solid State Nucl Magn Reson, 2010, 37(3, 4): 39-59.

[16] Leskes M, Akbey Ü, Oschkinat H, et al. Radio frequency assisted homo-nuclear recoupling, a Floquet description of homo-nuclear recoupling via surrounding hetero-nuclei in fully protonated to fully deuterated systems[J]. J Magn Reson, 2011, 209(2): 207-219.

[17] Jurgens B, Irran E, Senker J, et al. Melem (2,5,8-Triamino-tri-s-triazine), an important intermediate during condensation of melamine rings to Graphitic Carbon Nitride: synthesis, structure determination by X-ray powder diffractometry, solid-state NMR, and theoretical studies[J]. J Am Chem Soc, 2003, 125(34): 10 288-10 300.

[18] Bak M, Rasmussen J T, Nielsen N C. SIMPSON: A general simulation program for solid-state NMR spectroscopy[J]. J Magn Reson, 2000, 147(2): 296-330.

[19] Bak M, Nielsen N C. REPULSION: A novel approach to efficient powder averaging in solid-state NMR[J]. J Magn Reson, 1997, 125(1): 132-139.

[20] Fung B M, Khitrin A K, Ermolaev K. An improved broadband decoupling sequence for liquid crystals and solids[J]. J Magn Reson, 2000, 142(1): 97-101.

[21] Lotsch B V, Dçblinger M, Sehnert J, et al. Unmasking melon by a complementary approach employing electron diffraction, solid-state NMR spectroscopy, and theoretical calculations; structural characterization of a carbon nitride polymer[J]. Chem Eur J, 2007, 13(17): 4 969-4 980.

[22] Vosegaard T. Challenges in numerical simulations of solid-state NMR experiments: Spin exchange pulse sequences[J]. Solid State Nucl Magn Reson, 2010, 38(4): 77-83.

Probing ¹⁵N-¹⁵N Correlations in g-C₃N₄ Samples with Solid-State NMR SHA+ Pulse Sequence

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