Chemical shift referencing in MAS solid state NMR

Morcombe, Corey R.; Zilm, Kurt W.

doi:10.1016/s1090-7807(03)00082-x

Cited by 782 publications

(732 citation statements)

References 20 publications

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“…The 15 N chemical shifts were referenced to liquid 15 NH 3 at 0 p.p.m. using the indirect referencing of a 13 C signal for adamantane 40,41 . In all the experiments, the external air temperature was set to − 10 °C using a Varian VT controller, and the MAS spinning speed was 20,000 ± 10 Hz.…”

Section: Methodsmentioning

confidence: 99%

Chemical structures of hydrazine-treated graphene oxide and generation of aromatic nitrogen doping

et al. 2012

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Chemically modified graphene platelets, produced via graphene oxide, show great promise in a variety of applications due to their electrical, thermal, barrier and mechanical properties. understanding the chemical structures of chemically modified graphene platelets will aid in the understanding of their physical properties and facilitate development of chemically modified graphene platelet chemistry. Here we use 13 C and 15 n solid-state nuclear magnetic resonance spectroscopy and X-ray photoelectron spectroscopy to study the chemical structure of 15 nlabelled hydrazine-treated 13 C-labelled graphite oxide and unlabelled hydrazine-treated graphene oxide, respectively. These experiments suggest that hydrazine treatment of graphene oxide causes insertion of an aromatic n 2 moiety in a five-membered ring at the platelet edges and also restores graphitic networks on the basal planes. Furthermore, density-functional theory calculations support the formation of such n 2 structures at the edges and help to elucidate the influence of the aromatic n 2 moieties on the electronic structure of chemically modified graphene platelets.

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Section: Methodsmentioning

confidence: 99%

Chemical structures of hydrazine-treated graphene oxide and generation of aromatic nitrogen doping

et al. 2012

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“…The sample was cooled with nitrogen gas at −10°C to counteract radiofrequency heating. Spectra were externally referenced to the methylene carbon of adamantane at 40.5 ppm, which corresponds to the 13 C referencing used in liquidstate NMR of soluble proteins [21,26].…”

Section: Solid-state Nmr Spectroscopymentioning

confidence: 99%

Isotopically labeled expression in E. coli, purification, and refolding of the full ectodomain of the influenza virus membrane fusion protein

Curtis-Fisk

Spencer

Weliky

2008

Protein Expression and Purification

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This paper describes methods to produce an isotopically labeled 23 kDa viral membrane protein with purified yield of 20 mg/L of E. coli shake flask culture. This yield is sufficient for NMR structural studies and the protein production methods are simple, straightforward, and rapid and likely applicable to other recombinant membrane proteins expressed in E. coli. The target FHA2 protein is the full ectodomain construct of the influenza virus hemagglutinin protein which catalyzes fusion between the viral and the cellular endosomal membranes during infection. The high yield of FHA2 was achieved by: (1) initial growth in rich medium to A 600 ~ 8 followed by a switch to minimal medium and induction of protein expression; and (2) obtaining protein both from purification of the detergent-soluble lysate and from solubilization, purification, and refolding of inclusion bodies. The high cell density was achieved after optimization of pH, oxygenation, and carbon source and concentration, and the refolding protocol was optimized using circular dichroism spectroscopy. For a single residue of membrane-associated FHA2 that was obtained from purification and refolding of inclusion bodies, native conformation was verified by the 13 CO chemical shift measured using solidstate nuclear magnetic resonance spectroscopy.

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“…1 H chemical shifts were referenced to the single resonance observed for protons in adamantane at 1.87 ppm with respect to the signal for neat TMS. 13 C chemical shifts were referenced to the CH 2 resonance observed for adamantane at 38.48 ppm with respect to the signal for neat TMS 14 .…”

Section: Nmr Experimentsmentioning

confidence: 99%

De Novo Determination of the Crystal Structure of a Large Drug Molecule by Crystal Structure Prediction-Based Powder NMR Crystallography

et al. 2013

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ABSTRACT:The crystal structure of Form 4 of the drug (4-[4-(2-adamantylcarbamoyl)-5-ter-butyl-pyrazol-1-yl] benzoic acid) is determined using a protocol for NMR powder crystallography at natural isotopic abundance combining solid-state 1 H NMR spectroscopy, crystal structure prediction, and DFT chemical shift calculations. This is the first example of NMR structure determination for a molecular compound of previously unknown structure, and at 422 g/mol this is the largest compound to which this method has been applied so far.

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Chemical shift referencing in MAS solid state NMR

Cited by 782 publications

References 20 publications

Chemical structures of hydrazine-treated graphene oxide and generation of aromatic nitrogen doping

Chemical structures of hydrazine-treated graphene oxide and generation of aromatic nitrogen doping

Isotopically labeled expression in E. coli, purification, and refolding of the full ectodomain of the influenza virus membrane fusion protein

De Novo Determination of the Crystal Structure of a Large Drug Molecule by Crystal Structure Prediction-Based Powder NMR Crystallography

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