Precise Measurement of Long-Range Heteronuclear Coupling Constants by a Novel Broadband Proton-Proton-Decoupled CPMG-HSQMBC Method

István Timári; Tünde Z Illyés; Ralph W Adams; Mathias Nilsson; László Szilágyi; Gareth Morris; Katalin E Kövér

doi:10.1002/chem.201405535

Precise Measurement of Long-Range Heteronuclear Coupling Constants by a Novel Broadband Proton-Proton-Decoupled CPMG-HSQMBC Method

István Timári, Tünde Z Illyés, Ralph W Adams, Mathias Nilsson, László Szilágyi, Gareth Morris, Katalin E Kövér

Research output: Contribution to journal › Article › peer-review

Abstract

A broadband proton-proton-decoupled CPMG-HSQMBC method for the precise and direct measurement of long-range heteronuclear coupling constants is presented. The Zangger-Sterk-based homodecoupling scheme reported herein efficiently removes unwanted proton-proton splittings from the heteronuclear multiplets, so that the desired heteronuclear couplings can be determined simply by measuring frequency differences between singlet maxima in the resulting spectra. The proposed pseudo-1D/2D pulse sequences were tested on nucleotides, a metal complex incorporating P heterocycles, and diglycosyl (di)selenides, as well as on other carbohydrate derivatives, for the extraction of (n)J(H-1, P-31), (n)J(H-1, Se-77), and (n)J(H-1, C-13) values, respectively.

Original language	English
Pages (from-to)	3472-3479
Number of pages	8
Journal	Chemistry-A European Journal
Volume	21
Issue number	8
DOIs	https://doi.org/10.1002/chem.201405535
Publication status	Published - 2015

Keywords

hsqmbc
heteronuclear coupling constants
nmr spectroscopy
proton-proton decoupling
structure elucidation
bond correlation spectroscopy
correlation nmr-spectroscopy
hsqc-tocsy experiments
pure shift h-1-nmr
accurate measurement
natural-abundance
homonuclear
resolution
spectra
sensitivity

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10.1002/chem.201405535

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@article{4077cfaf4936409dabcb0dafb591ca98,

title = "Precise Measurement of Long-Range Heteronuclear Coupling Constants by a Novel Broadband Proton-Proton-Decoupled CPMG-HSQMBC Method",

abstract = "A broadband proton-proton-decoupled CPMG-HSQMBC method for the precise and direct measurement of long-range heteronuclear coupling constants is presented. The Zangger-Sterk-based homodecoupling scheme reported herein efficiently removes unwanted proton-proton splittings from the heteronuclear multiplets, so that the desired heteronuclear couplings can be determined simply by measuring frequency differences between singlet maxima in the resulting spectra. The proposed pseudo-1D/2D pulse sequences were tested on nucleotides, a metal complex incorporating P heterocycles, and diglycosyl (di)selenides, as well as on other carbohydrate derivatives, for the extraction of (n)J(H-1, P-31), (n)J(H-1, Se-77), and (n)J(H-1, C-13) values, respectively.",

keywords = "hsqmbc, heteronuclear coupling constants, nmr spectroscopy, proton-proton decoupling, structure elucidation, bond correlation spectroscopy, correlation nmr-spectroscopy, hsqc-tocsy experiments, pure shift h-1-nmr, accurate measurement, natural-abundance, homonuclear, resolution, spectra, sensitivity",

author = "Istv{\'a}n Tim{\'a}ri and Illy{\'e}s, {T{\"u}nde Z} and Adams, {Ralph W} and Mathias Nilsson and L{\'a}szl{\'o} Szil{\'a}gyi and Gareth Morris and K{\"o}v{\'e}r, {Katalin E}",

note = "Financial support from TMOP-4.2.2/A-11/1/KONV-2012-0025, OTKA K 105459, and OTKA NN 109671 (to K.E.K and L.Sz.), from Richter Gedeon Talentum Alaptvny (Ph.D. scholarship to I.T.), from the Engineering and Physical Sciences Research Council (grant numbers EP/I007989 and EP/L018500) (to R.W.A. , M.N., and G.A.M.) is gratefully acknowledged. The research of I.T. was supported by the European Union and the State of Hungary, co-financed by the European Social Fund in the framework of TMOP-4.2.4/A/2-11/1-2012-0001 “National Excellence Program”.Cb5jw Times Cited:1 Cited References Count:61",

year = "2015",

doi = "10.1002/chem.201405535",

language = "English",

volume = "21",

pages = "3472--3479",

journal = "Chemistry-A European Journal",

issn = "0947-6539",

publisher = "John Wiley & Sons Ltd",

number = "8",

}

TY - JOUR

T1 - Precise Measurement of Long-Range Heteronuclear Coupling Constants by a Novel Broadband Proton-Proton-Decoupled CPMG-HSQMBC Method

AU - Timári, István

AU - Illyés, Tünde Z

AU - Adams, Ralph W

AU - Nilsson, Mathias

AU - Szilágyi, László

AU - Morris, Gareth

AU - Kövér, Katalin E

N1 - Financial support from TMOP-4.2.2/A-11/1/KONV-2012-0025, OTKA K 105459, and OTKA NN 109671 (to K.E.K and L.Sz.), from Richter Gedeon Talentum Alaptvny (Ph.D. scholarship to I.T.), from the Engineering and Physical Sciences Research Council (grant numbers EP/I007989 and EP/L018500) (to R.W.A. , M.N., and G.A.M.) is gratefully acknowledged. The research of I.T. was supported by the European Union and the State of Hungary, co-financed by the European Social Fund in the framework of TMOP-4.2.4/A/2-11/1-2012-0001 “National Excellence Program”.Cb5jw Times Cited:1 Cited References Count:61

PY - 2015

Y1 - 2015

N2 - A broadband proton-proton-decoupled CPMG-HSQMBC method for the precise and direct measurement of long-range heteronuclear coupling constants is presented. The Zangger-Sterk-based homodecoupling scheme reported herein efficiently removes unwanted proton-proton splittings from the heteronuclear multiplets, so that the desired heteronuclear couplings can be determined simply by measuring frequency differences between singlet maxima in the resulting spectra. The proposed pseudo-1D/2D pulse sequences were tested on nucleotides, a metal complex incorporating P heterocycles, and diglycosyl (di)selenides, as well as on other carbohydrate derivatives, for the extraction of (n)J(H-1, P-31), (n)J(H-1, Se-77), and (n)J(H-1, C-13) values, respectively.

AB - A broadband proton-proton-decoupled CPMG-HSQMBC method for the precise and direct measurement of long-range heteronuclear coupling constants is presented. The Zangger-Sterk-based homodecoupling scheme reported herein efficiently removes unwanted proton-proton splittings from the heteronuclear multiplets, so that the desired heteronuclear couplings can be determined simply by measuring frequency differences between singlet maxima in the resulting spectra. The proposed pseudo-1D/2D pulse sequences were tested on nucleotides, a metal complex incorporating P heterocycles, and diglycosyl (di)selenides, as well as on other carbohydrate derivatives, for the extraction of (n)J(H-1, P-31), (n)J(H-1, Se-77), and (n)J(H-1, C-13) values, respectively.

KW - hsqmbc

KW - heteronuclear coupling constants

KW - nmr spectroscopy

KW - proton-proton decoupling

KW - structure elucidation

KW - bond correlation spectroscopy

KW - correlation nmr-spectroscopy

KW - hsqc-tocsy experiments

KW - pure shift h-1-nmr

KW - accurate measurement

KW - natural-abundance

KW - homonuclear

KW - resolution

KW - spectra

KW - sensitivity

U2 - 10.1002/chem.201405535

DO - 10.1002/chem.201405535

M3 - Article

SN - 0947-6539

VL - 21

SP - 3472

EP - 3479

JO - Chemistry-A European Journal

JF - Chemistry-A European Journal

IS - 8

ER -

Precise Measurement of Long-Range Heteronuclear Coupling Constants by a Novel Broadband Proton-Proton-Decoupled CPMG-HSQMBC Method

Abstract

Keywords

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