Complete H-1 resonance assignment of beta-maltose from H-1-H-1 DQ-SQ CRAMPS and H-1 (DQ-DUMBO)-C-13 SQ refocused INEPT 2D solid-state NMR spectra and first principles GIPAW calculations

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https://doi.org/10.1039/c001290d
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Keywords

POWDER DIFFRACTION DATA, QUANTUM-CHEMICAL CALCULATIONS, NUCLEAR-MAGNETIC-RESONANCE, PROTON-PROTON PROXIMITIES, DENSITY-FUNCTIONAL THEORY, PI-PI PACKING, CRYSTAL-STRUCTURE, O-17 NMR, 1ST-PRINCIPLES CALCULATION, CORRELATION SPECTROSCOPY

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Complete H-1 resonance assignment of beta-maltose from H-1-H-1 DQ-SQ CRAMPS and H-1 (DQ-DUMBO)-C-13 SQ refocused INEPT 2D solid-state NMR spectra and first principles GIPAW calculations. / Webber, Amy L.; Elena, Benedicte; Griffin, John M. et al.
In: Physical Chemistry Chemical Physics, Vol. 12, No. 26, 2010, p. 6970-6983.

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

Bibtex

@article{6afce910c336435db3c223b343b62687,

title = "Complete H-1 resonance assignment of beta-maltose from H-1-H-1 DQ-SQ CRAMPS and H-1 (DQ-DUMBO)-C-13 SQ refocused INEPT 2D solid-state NMR spectra and first principles GIPAW calculations",

abstract = "A disaccharide is a challenging case for high-resolution H-1 solid-state NMR because of the 24 distinct protons (14 aliphatic and 10 OH) having H-1 chemical shifts that all fall within a narrow range of approximately 3 to 7 ppm. High-resolution H-1 (500 MHz) double-quantum (DQ) combined rotation and multiple pulse sequence (CRAMPS) solid-state NMR spectra of beta-maltose monohydrate are presented. H-1-H-1 DQ-SQ CRAMPS spectra are presented together with H-1 (DQ)-C-13 correlation spectra obtained with a new pulse sequence that correlates a high-resolution H-1 DQ dimension with a C-13 single quantum (SQ) dimension using the refocused INEPT pulse-sequence element to transfer magnetization via one-bond C-13-H-1 J couplings. Compared to the observation of only a single broad peak in a H-1 DQ spectrum recorded at 30 kHz magic-angle spinning (MAS), the use of DUMBO H-1 homonuclear decoupling in the H-1 DQ CRAMPS experiment allows the resolution of distinct DQ correlation peaks which, in combination with first-principles chemical shift calculations based on the GIPAW (Gauge Including Projector Augmented Waves) plane-wave pseudopotential approach, enables the assignment of the H-1 resonances to the 24 distinct protons. We believe this to be the first experimental solid-state NMR determination of the hydroxyl OH H-1 chemical shifts for a simple sugar. Variable-temperature H-1-H-1 DQ CRAMPS spectra reveal small increases in the H-1 chemical shifts of the OH resonances upon decreasing the temperature from 348 K to 248 K.",

keywords = "POWDER DIFFRACTION DATA, QUANTUM-CHEMICAL CALCULATIONS, NUCLEAR-MAGNETIC-RESONANCE, PROTON-PROTON PROXIMITIES, DENSITY-FUNCTIONAL THEORY, PI-PI PACKING, CRYSTAL-STRUCTURE, O-17 NMR, 1ST-PRINCIPLES CALCULATION, CORRELATION SPECTROSCOPY",

author = "Webber, {Amy L.} and Benedicte Elena and Griffin, {John M.} and Yates, {Jonathan R.} and Pham, {Tran N.} and Francesco Mauri and Pickard, {Chris J.} and Gil, {Ana M.} and Robin Stein and Anne Lesage and Lyndon Emsley and Brown, {Steven P.}",

year = "2010",

doi = "10.1039/c001290d",

language = "English",

volume = "12",

pages = "6970--6983",

journal = "Physical Chemistry Chemical Physics",

issn = "1463-9076",

publisher = "Royal Society of Chemistry",

number = "26",

}

RIS

TY - JOUR

T1 - Complete H-1 resonance assignment of beta-maltose from H-1-H-1 DQ-SQ CRAMPS and H-1 (DQ-DUMBO)-C-13 SQ refocused INEPT 2D solid-state NMR spectra and first principles GIPAW calculations

AU - Webber, Amy L.

AU - Elena, Benedicte

AU - Griffin, John M.

AU - Yates, Jonathan R.

AU - Pham, Tran N.

AU - Mauri, Francesco

AU - Pickard, Chris J.

AU - Gil, Ana M.

AU - Stein, Robin

AU - Lesage, Anne

AU - Emsley, Lyndon

AU - Brown, Steven P.

PY - 2010

Y1 - 2010

N2 - A disaccharide is a challenging case for high-resolution H-1 solid-state NMR because of the 24 distinct protons (14 aliphatic and 10 OH) having H-1 chemical shifts that all fall within a narrow range of approximately 3 to 7 ppm. High-resolution H-1 (500 MHz) double-quantum (DQ) combined rotation and multiple pulse sequence (CRAMPS) solid-state NMR spectra of beta-maltose monohydrate are presented. H-1-H-1 DQ-SQ CRAMPS spectra are presented together with H-1 (DQ)-C-13 correlation spectra obtained with a new pulse sequence that correlates a high-resolution H-1 DQ dimension with a C-13 single quantum (SQ) dimension using the refocused INEPT pulse-sequence element to transfer magnetization via one-bond C-13-H-1 J couplings. Compared to the observation of only a single broad peak in a H-1 DQ spectrum recorded at 30 kHz magic-angle spinning (MAS), the use of DUMBO H-1 homonuclear decoupling in the H-1 DQ CRAMPS experiment allows the resolution of distinct DQ correlation peaks which, in combination with first-principles chemical shift calculations based on the GIPAW (Gauge Including Projector Augmented Waves) plane-wave pseudopotential approach, enables the assignment of the H-1 resonances to the 24 distinct protons. We believe this to be the first experimental solid-state NMR determination of the hydroxyl OH H-1 chemical shifts for a simple sugar. Variable-temperature H-1-H-1 DQ CRAMPS spectra reveal small increases in the H-1 chemical shifts of the OH resonances upon decreasing the temperature from 348 K to 248 K.

AB - A disaccharide is a challenging case for high-resolution H-1 solid-state NMR because of the 24 distinct protons (14 aliphatic and 10 OH) having H-1 chemical shifts that all fall within a narrow range of approximately 3 to 7 ppm. High-resolution H-1 (500 MHz) double-quantum (DQ) combined rotation and multiple pulse sequence (CRAMPS) solid-state NMR spectra of beta-maltose monohydrate are presented. H-1-H-1 DQ-SQ CRAMPS spectra are presented together with H-1 (DQ)-C-13 correlation spectra obtained with a new pulse sequence that correlates a high-resolution H-1 DQ dimension with a C-13 single quantum (SQ) dimension using the refocused INEPT pulse-sequence element to transfer magnetization via one-bond C-13-H-1 J couplings. Compared to the observation of only a single broad peak in a H-1 DQ spectrum recorded at 30 kHz magic-angle spinning (MAS), the use of DUMBO H-1 homonuclear decoupling in the H-1 DQ CRAMPS experiment allows the resolution of distinct DQ correlation peaks which, in combination with first-principles chemical shift calculations based on the GIPAW (Gauge Including Projector Augmented Waves) plane-wave pseudopotential approach, enables the assignment of the H-1 resonances to the 24 distinct protons. We believe this to be the first experimental solid-state NMR determination of the hydroxyl OH H-1 chemical shifts for a simple sugar. Variable-temperature H-1-H-1 DQ CRAMPS spectra reveal small increases in the H-1 chemical shifts of the OH resonances upon decreasing the temperature from 348 K to 248 K.

KW - POWDER DIFFRACTION DATA

KW - QUANTUM-CHEMICAL CALCULATIONS

KW - NUCLEAR-MAGNETIC-RESONANCE

KW - PROTON-PROTON PROXIMITIES

KW - DENSITY-FUNCTIONAL THEORY

KW - PI-PI PACKING

KW - CRYSTAL-STRUCTURE

KW - O-17 NMR

KW - 1ST-PRINCIPLES CALCULATION

KW - CORRELATION SPECTROSCOPY

U2 - 10.1039/c001290d

DO - 10.1039/c001290d

M3 - Journal article

VL - 12

SP - 6970

EP - 6983

JO - Physical Chemistry Chemical Physics

JF - Physical Chemistry Chemical Physics

SN - 1463-9076

IS - 26

ER -

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