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Complete 1H resonance assignment of β-maltose from 1H–1H DQ-SQ CRAMPS and 1H (DQ-DUMBO)–13C SQ refocused INEPT 2D solid-state NMR spectra and first principles GIPAW calculations
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Webber, Amy L., Elena, Benedicte, Griffin, John M., Yates, Jonathan R., Pham, Tran N., Mauri, Francesco, Pickard, Chris J., Gil, Ana M., Stein, Robin, Lesage, Anne, Emsley, Lyndon and Brown, Steven P. (2010) Complete 1H resonance assignment of β-maltose from 1H–1H DQ-SQ CRAMPS and 1H (DQ-DUMBO)–13C SQ refocused INEPT 2D solid-state NMR spectra and first principles GIPAW calculations. Physical Chemistry Chemical Physics, Vol.12 (Vol.26). pp. 6970-6983. doi:10.1039/c001290d ISSN 1463-9076.
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Official URL: http://dx.doi.org/10.1039/c001290d
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.
| Item Type: | Journal Article | ||||
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| Alternative Title: | |||||
| Subjects: | Q Science > QD Chemistry Q Science > QC Physics |
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| Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | ||||
| Journal or Publication Title: | Physical Chemistry Chemical Physics | ||||
| Publisher: | Royal Society of Chemistry | ||||
| ISSN: | 1463-9076 | ||||
| Official Date: | 2010 | ||||
| Dates: |
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| Volume: | Vol.12 | ||||
| Number: | Vol.26 | ||||
| Number of Pages: | 14 | ||||
| Page Range: | pp. 6970-6983 | ||||
| DOI: | 10.1039/c001290d | ||||
| Status: | Peer Reviewed | ||||
| Publication Status: | Published | ||||
| Access rights to Published version: | Restricted or Subscription Access | ||||
| Funder: | Engineering and Physical Sciences Research Council (EPSRC), Fundacao para a Ciencia e a Tecnologia, Portugal, Advantage West Midlands (AWM), EC | ||||
| Grant number: | POCTI/33075/QUI/2000, RII3-026145 |
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