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**CHHC and H-1-H-1 magnetization exchange : analysis by experimental solid-state NMR and 11-spin density-matrix simulations.** / Aluas, Mihaela; Tripon, Carmen; Griffin, John M. et al.

Research output: Contribution to Journal/Magazine › Journal article › peer-review

Aluas, M, Tripon, C, Griffin, JM, Filip, X, Ladizhansky, V, Griffin, RG, Brown, SP & Filip, C 2009, 'CHHC and H-1-H-1 magnetization exchange: analysis by experimental solid-state NMR and 11-spin density-matrix simulations', *Journal of Magnetic Resonance*, vol. 199, no. 2, pp. 173-187. https://doi.org/10.1016/j.jmr.2009.04.013

Aluas, M., Tripon, C., Griffin, J. M., Filip, X., Ladizhansky, V., Griffin, R. G., Brown, S. P., & Filip, C. (2009). CHHC and H-1-H-1 magnetization exchange: analysis by experimental solid-state NMR and 11-spin density-matrix simulations. *Journal of Magnetic Resonance*, *199*(2), 173-187. https://doi.org/10.1016/j.jmr.2009.04.013

Aluas M, Tripon C, Griffin JM, Filip X, Ladizhansky V, Griffin RG et al. CHHC and H-1-H-1 magnetization exchange: analysis by experimental solid-state NMR and 11-spin density-matrix simulations. Journal of Magnetic Resonance. 2009 Aug;199(2):173-187. Epub 2009 May 4. doi: 10.1016/j.jmr.2009.04.013

@article{41d523c08c4549cea49a83fb263ccdbe,

title = "CHHC and H-1-H-1 magnetization exchange: analysis by experimental solid-state NMR and 11-spin density-matrix simulations",

abstract = "A protocol is presented for correcting the effect of non-specific cross-polarization in CHHC solid-state MAS NMR experiments, thus allowing the recovery of the H-1-H-1 magnetization exchange functions front the mixing-time dependent buildup of experimental CHHC peak intensity. The presented protocol also incorporates a Scaling Procedure to take into account the effect Of multiplicity of a CH2 or CH3 moiety. Experimental CHHC buildup Curves are presented for L-tyrosine center dot HCl samples where either all OF only one in 10 molecules are U-C-13 labeled. Good agreement between experiment and 11-spin SPINEVOLUTION simulation (including only isotropic H-1 chemical shifts) is demonstrated for the initial buildup (t(mix) <100 mu s) of CHHC peak intensity corresponding to an intramolecular close (2.5 degrees) H-H proximity. Differences in the initial CHHC buildup are observed between the one in 10 dilute and 100% samples for cases where there is a close intermolecular H-H proximity in addition to a close intramolecular H-H proximity. For the dilute sample, CHHC cross-peak intensities tended to significantly lower values for long mixing times (500 mu s) as compared to the 100% sample. This difference is explained as being due to the dependence of the limiting total magnetization on the ratio N-obs/N-tot between the number of protons that are directly attached to a C-13 nucleus and hence contribute significantly to the observed C-13 CHHC NMR signal, and the total number of H-1 spins into the system. H-1-H-1 magnetization exchange Curves extracted from CHHC spectra for the 100% L-tyrosine HCI sample exhibit a clear sensitivity to the root sum squared dipolar coupling, with fast buildup being observed for the shortest intramolecular distances (2.5 angstrom) and slower, yet observable buildup for the longer intermolecular distances (up to 5 angstrom). (C) 2009 Elsevier Inc. All rights reserved.",

keywords = "Solid-state NMR, MAS, CHHC, H-1-H-1 dipolar coupling, Distance constraints, ANGLE-SPINNING NMR, SPECTRIN SH3 DOMAIN, ECHO PULSE-TRAIN, CORRELATION SPECTROSCOPY, ROTATING SOLIDS, MAS NMR, 3D STRUCTURE, INTERNUCLEAR DISTANCES, STRUCTURAL CONSTRAINTS, RESONANCE ASSIGNMENT",

author = "Mihaela Aluas and Carmen Tripon and Griffin, {John M.} and Xenia Filip and Vladimir Ladizhansky and Griffin, {Robert G.} and Brown, {Steven P.} and Claudiu Filip",

year = "2009",

month = aug,

doi = "10.1016/j.jmr.2009.04.013",

language = "English",

volume = "199",

pages = "173--187",

journal = "Journal of Magnetic Resonance",

issn = "1090-7807",

publisher = "Academic Press Inc.",

number = "2",

}

TY - JOUR

T1 - CHHC and H-1-H-1 magnetization exchange

T2 - analysis by experimental solid-state NMR and 11-spin density-matrix simulations

AU - Aluas, Mihaela

AU - Tripon, Carmen

AU - Griffin, John M.

AU - Filip, Xenia

AU - Ladizhansky, Vladimir

AU - Griffin, Robert G.

AU - Brown, Steven P.

AU - Filip, Claudiu

PY - 2009/8

Y1 - 2009/8

N2 - A protocol is presented for correcting the effect of non-specific cross-polarization in CHHC solid-state MAS NMR experiments, thus allowing the recovery of the H-1-H-1 magnetization exchange functions front the mixing-time dependent buildup of experimental CHHC peak intensity. The presented protocol also incorporates a Scaling Procedure to take into account the effect Of multiplicity of a CH2 or CH3 moiety. Experimental CHHC buildup Curves are presented for L-tyrosine center dot HCl samples where either all OF only one in 10 molecules are U-C-13 labeled. Good agreement between experiment and 11-spin SPINEVOLUTION simulation (including only isotropic H-1 chemical shifts) is demonstrated for the initial buildup (t(mix) <100 mu s) of CHHC peak intensity corresponding to an intramolecular close (2.5 degrees) H-H proximity. Differences in the initial CHHC buildup are observed between the one in 10 dilute and 100% samples for cases where there is a close intermolecular H-H proximity in addition to a close intramolecular H-H proximity. For the dilute sample, CHHC cross-peak intensities tended to significantly lower values for long mixing times (500 mu s) as compared to the 100% sample. This difference is explained as being due to the dependence of the limiting total magnetization on the ratio N-obs/N-tot between the number of protons that are directly attached to a C-13 nucleus and hence contribute significantly to the observed C-13 CHHC NMR signal, and the total number of H-1 spins into the system. H-1-H-1 magnetization exchange Curves extracted from CHHC spectra for the 100% L-tyrosine HCI sample exhibit a clear sensitivity to the root sum squared dipolar coupling, with fast buildup being observed for the shortest intramolecular distances (2.5 angstrom) and slower, yet observable buildup for the longer intermolecular distances (up to 5 angstrom). (C) 2009 Elsevier Inc. All rights reserved.

AB - A protocol is presented for correcting the effect of non-specific cross-polarization in CHHC solid-state MAS NMR experiments, thus allowing the recovery of the H-1-H-1 magnetization exchange functions front the mixing-time dependent buildup of experimental CHHC peak intensity. The presented protocol also incorporates a Scaling Procedure to take into account the effect Of multiplicity of a CH2 or CH3 moiety. Experimental CHHC buildup Curves are presented for L-tyrosine center dot HCl samples where either all OF only one in 10 molecules are U-C-13 labeled. Good agreement between experiment and 11-spin SPINEVOLUTION simulation (including only isotropic H-1 chemical shifts) is demonstrated for the initial buildup (t(mix) <100 mu s) of CHHC peak intensity corresponding to an intramolecular close (2.5 degrees) H-H proximity. Differences in the initial CHHC buildup are observed between the one in 10 dilute and 100% samples for cases where there is a close intermolecular H-H proximity in addition to a close intramolecular H-H proximity. For the dilute sample, CHHC cross-peak intensities tended to significantly lower values for long mixing times (500 mu s) as compared to the 100% sample. This difference is explained as being due to the dependence of the limiting total magnetization on the ratio N-obs/N-tot between the number of protons that are directly attached to a C-13 nucleus and hence contribute significantly to the observed C-13 CHHC NMR signal, and the total number of H-1 spins into the system. H-1-H-1 magnetization exchange Curves extracted from CHHC spectra for the 100% L-tyrosine HCI sample exhibit a clear sensitivity to the root sum squared dipolar coupling, with fast buildup being observed for the shortest intramolecular distances (2.5 angstrom) and slower, yet observable buildup for the longer intermolecular distances (up to 5 angstrom). (C) 2009 Elsevier Inc. All rights reserved.

KW - Solid-state NMR

KW - MAS

KW - CHHC

KW - H-1-H-1 dipolar coupling

KW - Distance constraints

KW - ANGLE-SPINNING NMR

KW - SPECTRIN SH3 DOMAIN

KW - ECHO PULSE-TRAIN

KW - CORRELATION SPECTROSCOPY

KW - ROTATING SOLIDS

KW - MAS NMR

KW - 3D STRUCTURE

KW - INTERNUCLEAR DISTANCES

KW - STRUCTURAL CONSTRAINTS

KW - RESONANCE ASSIGNMENT

U2 - 10.1016/j.jmr.2009.04.013

DO - 10.1016/j.jmr.2009.04.013

M3 - Journal article

VL - 199

SP - 173

EP - 187

JO - Journal of Magnetic Resonance

JF - Journal of Magnetic Resonance

SN - 1090-7807

IS - 2

ER -