Straightforward measurement of individual 1J(CH) and 2J(HH) in diastereotopic CH2 groups

Josep Saurí; Laura Castañar; Pau Nolis; Albert Virgili; Teodor Parella

doi:10.1016/j.jmr.2014.02.003

Straightforward measurement of individual ¹J(CH) and ²J(HH) in diastereotopic CH₂ groups

Josep Saurí
, Laura Castañar
, Pau Nolis
, Albert Virgili
, Teodor Parella^*

^*Corresponding author for this work

Research output: Indexed journal article › Article › peer-review

18 Citations (Scopus)

Abstract

The C-H_A cross-peak corresponding to a diastereotopic CH _AH_B methylene spin system exhibits a characteristic 1:0:1 multiplet pattern along the indirect dimension of a ω₁-coupled HSQC spectrum. It is shown here that the use of the initial ¹³C Boltzmann polarization instead of the regular INEPT-based ¹H Boltzmann polarization makes visible the central lines of this multiplet pattern. A spin-state-selective method is proposed for the efficient measurement of both ¹J(CH_A) and ¹J(CH_B) along the indirect dimension of a 2D spectrum as well as to the magnitude and the sign of the geminal ²J(H_AH_B) coupling constant from the straightforward analysis of a single four-component E.COSY cross-peak. Additionally, the extraction of ¹J(CH) values for CH and CH ₃ multiplicities can be also performed from the same spectrum. The success of the method is also illustrated for the determination of residual dipolar ¹D(CH) and ²D(HH) coupling constants in a small molecule weakly aligned in a PMMA swollen gel.

Original language	English
Pages (from-to)	33-40
Number of pages	8
Journal	Journal of Magnetic Resonance
Volume	242
DOIs	https://doi.org/10.1016/j.jmr.2014.02.003
Publication status	Published - May 2014
Externally published	Yes

Keywords

E.COSY
Inverse INEPT
Methylene spin systems
One-bond proton-carbon coupling constants
Residual dipolar couplings
Two-bond proton-proton coupling constants

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10.1016/j.jmr.2014.02.003

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title = "Straightforward measurement of individual 1J(CH) and 2J(HH) in diastereotopic CH2 groups",

abstract = "The C-HA cross-peak corresponding to a diastereotopic CH AHB methylene spin system exhibits a characteristic 1:0:1 multiplet pattern along the indirect dimension of a ω1-coupled HSQC spectrum. It is shown here that the use of the initial 13C Boltzmann polarization instead of the regular INEPT-based 1H Boltzmann polarization makes visible the central lines of this multiplet pattern. A spin-state-selective method is proposed for the efficient measurement of both 1J(CHA) and 1J(CHB) along the indirect dimension of a 2D spectrum as well as to the magnitude and the sign of the geminal 2J(HAHB) coupling constant from the straightforward analysis of a single four-component E.COSY cross-peak. Additionally, the extraction of 1J(CH) values for CH and CH 3 multiplicities can be also performed from the same spectrum. The success of the method is also illustrated for the determination of residual dipolar 1D(CH) and 2D(HH) coupling constants in a small molecule weakly aligned in a PMMA swollen gel.",

keywords = "E.COSY, Inverse INEPT, Methylene spin systems, One-bond proton-carbon coupling constants, Residual dipolar couplings, Two-bond proton-proton coupling constants",

author = "Josep Saur{\'i} and Laura Casta{\~n}ar and Pau Nolis and Albert Virgili and Teodor Parella",

year = "2014",

month = may,

doi = "10.1016/j.jmr.2014.02.003",

language = "English",

volume = "242",

pages = "33--40",

journal = "Journal of Magnetic Resonance",

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T1 - Straightforward measurement of individual 1J(CH) and 2J(HH) in diastereotopic CH2 groups

AU - Saurí, Josep

AU - Castañar, Laura

AU - Nolis, Pau

AU - Virgili, Albert

AU - Parella, Teodor

PY - 2014/5

Y1 - 2014/5

N2 - The C-HA cross-peak corresponding to a diastereotopic CH AHB methylene spin system exhibits a characteristic 1:0:1 multiplet pattern along the indirect dimension of a ω1-coupled HSQC spectrum. It is shown here that the use of the initial 13C Boltzmann polarization instead of the regular INEPT-based 1H Boltzmann polarization makes visible the central lines of this multiplet pattern. A spin-state-selective method is proposed for the efficient measurement of both 1J(CHA) and 1J(CHB) along the indirect dimension of a 2D spectrum as well as to the magnitude and the sign of the geminal 2J(HAHB) coupling constant from the straightforward analysis of a single four-component E.COSY cross-peak. Additionally, the extraction of 1J(CH) values for CH and CH 3 multiplicities can be also performed from the same spectrum. The success of the method is also illustrated for the determination of residual dipolar 1D(CH) and 2D(HH) coupling constants in a small molecule weakly aligned in a PMMA swollen gel.

AB - The C-HA cross-peak corresponding to a diastereotopic CH AHB methylene spin system exhibits a characteristic 1:0:1 multiplet pattern along the indirect dimension of a ω1-coupled HSQC spectrum. It is shown here that the use of the initial 13C Boltzmann polarization instead of the regular INEPT-based 1H Boltzmann polarization makes visible the central lines of this multiplet pattern. A spin-state-selective method is proposed for the efficient measurement of both 1J(CHA) and 1J(CHB) along the indirect dimension of a 2D spectrum as well as to the magnitude and the sign of the geminal 2J(HAHB) coupling constant from the straightforward analysis of a single four-component E.COSY cross-peak. Additionally, the extraction of 1J(CH) values for CH and CH 3 multiplicities can be also performed from the same spectrum. The success of the method is also illustrated for the determination of residual dipolar 1D(CH) and 2D(HH) coupling constants in a small molecule weakly aligned in a PMMA swollen gel.

KW - E.COSY

KW - Inverse INEPT

KW - Methylene spin systems

KW - One-bond proton-carbon coupling constants

KW - Residual dipolar couplings

KW - Two-bond proton-proton coupling constants

UR - https://www.scopus.com/pages/publications/84897713343

U2 - 10.1016/j.jmr.2014.02.003

DO - 10.1016/j.jmr.2014.02.003

M3 - Article

AN - SCOPUS:84897713343

SN - 1090-7807

VL - 242

SP - 33

EP - 40

JO - Journal of Magnetic Resonance

JF - Journal of Magnetic Resonance

ER -

Straightforward measurement of individual ¹J(CH) and ²J(HH) in diastereotopic CH₂ groups

Abstract

Keywords

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