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Two-dimensional Ca-43-H-1 correlation solid-state NMR spectroscopy

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Two-dimensional Ca-43-H-1 correlation solid-state NMR spectroscopy. / Wong, Alan; Laurencin, Danielle; Dupree, Ray et al.
In: Solid State Nuclear Magnetic Resonance, Vol. 35, No. 1, 01.02.2009, p. 32-36.

Research output: Contribution to Journal/MagazineJournal articlepeer-review

Harvard

Wong, A, Laurencin, D, Dupree, R & Smith, ME 2009, 'Two-dimensional Ca-43-H-1 correlation solid-state NMR spectroscopy', Solid State Nuclear Magnetic Resonance, vol. 35, no. 1, pp. 32-36. https://doi.org/10.1016/j.ssnmr.2008.11.002

APA

Wong, A., Laurencin, D., Dupree, R., & Smith, M. E. (2009). Two-dimensional Ca-43-H-1 correlation solid-state NMR spectroscopy. Solid State Nuclear Magnetic Resonance, 35(1), 32-36. https://doi.org/10.1016/j.ssnmr.2008.11.002

Vancouver

Wong A, Laurencin D, Dupree R, Smith ME. Two-dimensional Ca-43-H-1 correlation solid-state NMR spectroscopy. Solid State Nuclear Magnetic Resonance. 2009 Feb 1;35(1):32-36. doi: 10.1016/j.ssnmr.2008.11.002

Author

Wong, Alan ; Laurencin, Danielle ; Dupree, Ray et al. / Two-dimensional Ca-43-H-1 correlation solid-state NMR spectroscopy. In: Solid State Nuclear Magnetic Resonance. 2009 ; Vol. 35, No. 1. pp. 32-36.

Bibtex

@article{d8e7c377178440f0bb92561fdb4d2551,
title = "Two-dimensional Ca-43-H-1 correlation solid-state NMR spectroscopy",
abstract = "Calcium-43 (nuclear spin, S = 7/2) is an NMR insensitive low-gamma quadrupolar nucleus and up until recently only one-dimensional solid-state Ca-43 NMR spectra have been reported. Through-space correlation experiments are challenging between spin-1/2 and low-gamma quadrupolar nuclei because of the intrinsically weak dipolar interaction and the often-low natural abundance of the quadrupolar nucleus. Rotary-resonance recoupling (R-3) has recently been used to re-introduce hetero-nuclear dipolar interactions for sensitive high-gamma quadrupolar nuclei, but has not yet been applied in the case of low-gamma half-integer quadrupolar nuclei. Here an effective and robust 2D H-1-Ca-43 NMR correlation experiment combining the R-3 dipole-recoupling scheme with 2D HMQC is presented. It is demonstrated that the weak Ca-43-H-1 dipolar coupling in hydroxyapatite and oxy-hydroxyapatite can be readily re-introduced and that this recoupling scheme is more efficient than conventional cross-polarization transfer. Moreover, three Ca-43-H-1 dipolar coupled calcium environments are clearly resolved in the structurally unknown oxy-hydroxyapatite. This local information is not readily available from other techniques such as powder XRD and high resolution electron microscopy. R-3-HMQC is also a desirable experiment because the set-up is simple and it can be applied using conventional multi-resonance probes. (C) 2008 Elsevier Inc. All rights reserved.",
keywords = "Ca-43 NMR, Low-gamma, Hetero-nuclear correlation NMR spectroscopy, Dipolar interaction, R-3-HMQC, Hydroxyapatite, Oxy-hydroxyapatite",
author = "Alan Wong and Danielle Laurencin and Ray Dupree and Smith, {Mark E.}",
year = "2009",
month = feb,
day = "1",
doi = "10.1016/j.ssnmr.2008.11.002",
language = "English",
volume = "35",
pages = "32--36",
journal = "Solid State Nuclear Magnetic Resonance",
issn = "1527-3326",
publisher = "ACADEMIC PRESS INC ELSEVIER SCIENCE",
number = "1",

}

RIS

TY - JOUR

T1 - Two-dimensional Ca-43-H-1 correlation solid-state NMR spectroscopy

AU - Wong, Alan

AU - Laurencin, Danielle

AU - Dupree, Ray

AU - Smith, Mark E.

PY - 2009/2/1

Y1 - 2009/2/1

N2 - Calcium-43 (nuclear spin, S = 7/2) is an NMR insensitive low-gamma quadrupolar nucleus and up until recently only one-dimensional solid-state Ca-43 NMR spectra have been reported. Through-space correlation experiments are challenging between spin-1/2 and low-gamma quadrupolar nuclei because of the intrinsically weak dipolar interaction and the often-low natural abundance of the quadrupolar nucleus. Rotary-resonance recoupling (R-3) has recently been used to re-introduce hetero-nuclear dipolar interactions for sensitive high-gamma quadrupolar nuclei, but has not yet been applied in the case of low-gamma half-integer quadrupolar nuclei. Here an effective and robust 2D H-1-Ca-43 NMR correlation experiment combining the R-3 dipole-recoupling scheme with 2D HMQC is presented. It is demonstrated that the weak Ca-43-H-1 dipolar coupling in hydroxyapatite and oxy-hydroxyapatite can be readily re-introduced and that this recoupling scheme is more efficient than conventional cross-polarization transfer. Moreover, three Ca-43-H-1 dipolar coupled calcium environments are clearly resolved in the structurally unknown oxy-hydroxyapatite. This local information is not readily available from other techniques such as powder XRD and high resolution electron microscopy. R-3-HMQC is also a desirable experiment because the set-up is simple and it can be applied using conventional multi-resonance probes. (C) 2008 Elsevier Inc. All rights reserved.

AB - Calcium-43 (nuclear spin, S = 7/2) is an NMR insensitive low-gamma quadrupolar nucleus and up until recently only one-dimensional solid-state Ca-43 NMR spectra have been reported. Through-space correlation experiments are challenging between spin-1/2 and low-gamma quadrupolar nuclei because of the intrinsically weak dipolar interaction and the often-low natural abundance of the quadrupolar nucleus. Rotary-resonance recoupling (R-3) has recently been used to re-introduce hetero-nuclear dipolar interactions for sensitive high-gamma quadrupolar nuclei, but has not yet been applied in the case of low-gamma half-integer quadrupolar nuclei. Here an effective and robust 2D H-1-Ca-43 NMR correlation experiment combining the R-3 dipole-recoupling scheme with 2D HMQC is presented. It is demonstrated that the weak Ca-43-H-1 dipolar coupling in hydroxyapatite and oxy-hydroxyapatite can be readily re-introduced and that this recoupling scheme is more efficient than conventional cross-polarization transfer. Moreover, three Ca-43-H-1 dipolar coupled calcium environments are clearly resolved in the structurally unknown oxy-hydroxyapatite. This local information is not readily available from other techniques such as powder XRD and high resolution electron microscopy. R-3-HMQC is also a desirable experiment because the set-up is simple and it can be applied using conventional multi-resonance probes. (C) 2008 Elsevier Inc. All rights reserved.

KW - Ca-43 NMR, Low-gamma, Hetero-nuclear correlation NMR spectroscopy, Dipolar interaction, R-3-HMQC, Hydroxyapatite, Oxy-hydroxyapatite

U2 - 10.1016/j.ssnmr.2008.11.002

DO - 10.1016/j.ssnmr.2008.11.002

M3 - Journal article

VL - 35

SP - 32

EP - 36

JO - Solid State Nuclear Magnetic Resonance

JF - Solid State Nuclear Magnetic Resonance

SN - 1527-3326

IS - 1

ER -