Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K

		BioNMR > Educational resources > Journal club
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K

Webservers

NMR processing:

MDD

NMR assignment:

Backbone:

Side-chains:

NOEs:

Structure from NMR restraints:

Ab initio:

Fragment-based:

Rosetta-NMR (Robetta)

Template-based:

GeNMR

I-TASSER

Refinement:

Amber

Structure from chemical shifts:

Fragment-based:

Homology-based:

Torsion angles from chemical shifts:

Preditor

TALOS

Promega- Proline

Secondary structure from chemical shifts:

CSI (via RCI server)

TALOS

MICS caps, β-turns

d2D

PECAN

Flexibility from chemical shifts:

RCI

Interactions from chemical shifts:

HADDOCK

Chemical shifts re-referencing:

NMR model quality:

NOEs, other restraints:

Chemical shifts:

RDCs:

Pseudocontact shifts:

Protein geomtery:

SAVES2 or SAVES4

Quality Control Check

NMR spectrum prediction:

FANDAS

MestReS

V-NMR

Flexibility from structure:

Backbone S2

Methyl S2

B-factor

Molecular dynamics:

Gromacs

Amber

Antechamber

Chemical shifts prediction:

From structure:

Shiftx2

Sparta+

Camshift

CH3shift- Methyl

ArShift- Aromatic

ShiftS

Proshift

PPM

CheShift-2- Cα

From sequence:

Shifty

Camcoil

Poulsen_rc_CS

Disordered proteins:

MAXOCC

Format conversion & validation:

CCPN

From NMR-STAR 3.1

Validate NMR-STAR 3.1

NMR sample preparation:

Protein disorder:

DisMeta

Protein solubility:

Isotope labeling:

Solid-state NMR:

Thread Tools

Search this Thread

Rate Thread

Display Modes

12-15-2012, 09:51 AM

nmrlearner

Senior Member

Join Date: Jan 2005

Posts: 23,715

Points: 193,617, Level: 100

Level up: 0%, 0 Points needed

Activity: 50.7%

Last Achievements

Award-Showcase

NMR Credits: 0

NMR Points: 193,617

Downloads: 0

Uploads: 0

Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K

Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K

January 2013
Publication year: 2013
Source:Journal of Magnetic Resonance, Volume 226

We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20–25K and 9.4Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier [1], but also includes a corrugated waveguide for transmission of microwaves from below the probe to the sample. With a 30mW circularly polarized microwave source at 264GHz, MAS at 6.8kHz, and 21K sample temperature, greater than 25-fold enhancements of cross-polarized 13C NMR signals are observed in spectra of frozen glycerol/water solutions containing the triradical dopant DOTOPA-TEMPO when microwaves are applied. As demonstrations, we present DNP-enhanced one-dimensional and two-dimensional 13C MAS NMR spectra of frozen solutions of uniformly 13C-labeled l-alanine and melittin, a 26-residue helical peptide that we have synthesized with four uniformly 13C-labeled amino acids.
Graphical abstract

Highlights

? Probe for solid state NMR with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20K and 9.4Tesla. ? Signal enhancement greater than 25-fold (microwaves on versus microwaves off) using 30mW of microwaves. ? 2D 13C–13C spectra for 160nmol of the 26 residue peptide melittin in frozen solution, taken in ~2½h.

Source: Journal of Magnetic Resonance

Did you find this post helpful?

Similar Threads
Thread	Thread Starter	Forum	Replies	Last Post
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K Available online 20 November 2012 Publication year: 2012 Source:Journal of Magnetic Resonance</br> </br> We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20-25 K and 9.4 Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier (Thurber et al., J. Magn. Reson. 2008) , but also includes a...	nmrlearner	Journal club	0	12-01-2012 06:10 PM
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K Publication year: 2012 Source:Journal of Magnetic Resonance</br> Kent R. Thurber, Alexey Potapov, Wai-Ming Yau, Robert Tycko</br> We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20-25 K and 9.4 Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier (Thurber et al., J. Magn. Reson. 2008) ,...	nmrlearner	Journal club	0	11-21-2012 04:33 AM
Spectral editing of two-dimensional magic-angle-spinning solid-state NMR spectra for protein resonance assignment and structure determination Spectral editing of two-dimensional magic-angle-spinning solid-state NMR spectra for protein resonance assignment and structure determination Abstract Several techniques for spectral editing of 2D 13Câ??13C correlation NMR of proteins are introduced. They greatly reduce the spectral overlap for five common amino acid types, thus simplifying spectral assignment and conformational analysis. The carboxyl (COO) signals of glutamate and aspartate are selected by suppressing the overlapping amide Nâ??CO peaks through 13Câ??15N dipolar dephasing. The sidechain methine (CH) signals of valine,...	nmrlearner	Journal club	0	10-13-2012 04:42 AM
Intermolecular Structure Determination of Amyloid Fibrils with Magic-Angle Spinning and Dynamic Nuclear Polarization NMR Intermolecular Structure Determination of Amyloid Fibrils with Magic-Angle Spinning and Dynamic Nuclear Polarization NMR Marvin J. Bayro, Galia T. Debelouchina, Matthew T. Eddy, Neil R. Birkett, Catherine E. MacPhee, Melanie Rosay, Werner E. Maas, Christopher M. Dobson and Robert G. Griffin http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja203756x/aop/images/medium/ja-2011-03756x_0002.gif Journal of the American Chemical Society DOI: 10.1021/ja203756x http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA...	nmrlearner	Journal club	0	08-13-2011 02:47 AM
Intermolecular structure determination of amyloid fibrils with magic-angle spinning and dynamic nuclear polarization NMR. Intermolecular structure determination of amyloid fibrils with magic-angle spinning and dynamic nuclear polarization NMR. Intermolecular structure determination of amyloid fibrils with magic-angle spinning and dynamic nuclear polarization NMR. J Am Chem Soc. 2011 Jul 21; Authors: Bayro MJ, Debelouchina GT, Eddy MT, Birkett NR, Macphee CE, Rosay MM, Maas WE, Dobson CM, Griffin RG We describe magic-angle spinning NMR experiments designed to elucidate the interstrand architecture of amyloid fibrils. Three methods are introduced for this purpose, two...	nmrlearner	Journal club	0	07-23-2011 08:54 AM
[NMR paper] Resonance assignments and secondary structure analysis of E. coli thioredoxin by magic angle spinning solid-state NMR spectroscopy. Resonance assignments and secondary structure analysis of E. coli thioredoxin by magic angle spinning solid-state NMR spectroscopy. Related Articles Resonance assignments and secondary structure analysis of E. coli thioredoxin by magic angle spinning solid-state NMR spectroscopy. J Phys Chem B. 2005 Sep 29;109(38):18135-45 Authors: Marulanda D, Tasayco ML, Cataldi M, Arriaran V, Polenova T De novo site-specific 13C and 15N backbone and sidechain resonance assignments are presented for uniformly enriched E. coli thioredoxin, established using...	nmrlearner	Journal club	0	12-01-2010 06:56 PM
Automated protein resonance assignments of magic angle spinning solid-state NMR spect Automated protein resonance assignments of magic angle spinning solid-state NMR spectra of Î²1 immunoglobulin binding domain of protein G (GB1) Abstract Magic-angle spinning solid-state NMR (MAS SSNMR) represents a fast developing experimental technique with great potential to provide structural and dynamics information for proteins not amenable to other methods. However, few automated analysis tools are currently available for MAS SSNMR. We present a methodology for automating protein resonance assignments of MAS SSNMR spectral data and its application to experimental peak lists of the...	nmrlearner	Journal club	0	10-15-2010 05:16 PM
Automated protein resonance assignments of magic angle spinning solid-state NMR spect Automated protein resonance assignments of magic angle spinning solid-state NMR spectra of ?1 immunoglobulin binding domain of protein G (GB1). Related Articles Automated protein resonance assignments of magic angle spinning solid-state NMR spectra of ?1 immunoglobulin binding domain of protein G (GB1). J Biomol NMR. 2010 Oct 8; Authors: Moseley HN, Sperling LJ, Rienstra CM Magic-angle spinning solid-state NMR (MAS SSNMR) represents a fast developing experimental technique with great potential to provide structural and dynamics information for...	nmrlearner	Journal club	0	10-12-2010 02:52 PM

« Previous Thread | Next Thread »

Posting Rules
You may not post new threads You may not post replies You may not post attachments You may not edit your posts BB code is On Smilies are On [IMG] code is On HTML code is On Trackbacks are Off Pingbacks are Off Refbacks are Off