Low-temperature dynamic nuclear polarization with helium-cooled samples and nitrogen-driven magic-angle spinning

		BioNMR > Educational resources > Journal club
Low-temperature dynamic nuclear polarization with helium-cooled samples and nitrogen-driven magic-angle spinning

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

02-24-2016, 01:30 AM

nmrlearner

Senior Member

Join Date: Jan 2005

Posts: 23,777

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

Low-temperature dynamic nuclear polarization with helium-cooled samples and nitrogen-driven magic-angle spinning

Low-temperature dynamic nuclear polarization with helium-cooled samples and nitrogen-driven magic-angle spinning

Publication date: March 2016
Source:Journal of Magnetic Resonance, Volume 264

Author(s): Kent Thurber, Robert Tycko

We describe novel instrumentation for low-temperature solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS), focusing on aspects of this instrumentation that have not been described in detail in previous publications. We characterize the performance of an extended interaction oscillator (EIO) microwave source, operating near 264GHz with 1.5W output power, which we use in conjunction with a quasi-optical microwave polarizing system and a MAS NMR probe that employs liquid helium for sample cooling and nitrogen gas for sample spinning. Enhancement factors for cross-polarized 13C NMR signals in the 100–200 range are demonstrated with DNP at 25K. The dependences of signal amplitudes on sample temperature, as well as microwave power, polarization, and frequency, are presented. We show that sample temperatures below 30K can be achieved with helium consumption rates below 1.3l/h. To illustrate potential applications of this instrumentation in structural studies of biochemical systems, we compare results from low-temperature DNP experiments on a calmodulin-binding peptide in its free and bound states.
Graphical abstract

Source: Journal of Magnetic Resonance

Did you find this post helpful?

Similar Threads
Thread	Thread Starter	Forum	Replies	Last Post
Nuclear Depolarization and Absolute Sensitivity in Magic-Angle Spinning Cross-Effect Dynamic Nuclear Polarization From The DNP-NMR Blog: Nuclear Depolarization and Absolute Sensitivity in Magic-Angle Spinning Cross-Effect Dynamic Nuclear Polarization Mentink-Vigier, F., et al., Nuclear Depolarization and Absolute Sensitivity in Magic-Angle Spinning Cross-Effect Dynamic Nuclear Polarization. Phys. Chem. Chem. Phys., 2015. http://dx.doi.org/10.1039/C5CP03457D	nmrlearner	News from NMR blogs	0	07-30-2015 12:01 AM
Theoretical Aspects of Magic Angle Spinning - Dynamic Nuclear Polarization From The DNP-NMR Blog: Theoretical Aspects of Magic Angle Spinning - Dynamic Nuclear Polarization Mentink-Vigier, F., et al., Theoretical Aspects of Magic Angle Spinning - Dynamic Nuclear Polarization. J. Magn. Reson., 2015. http://www.sciencedirect.com/science/article/pii/S1090780715001500	nmrlearner	News from NMR blogs	0	07-27-2015 10:41 PM
Magic Angle Spinning NMR of Proteins: High-Frequency Dynamic Nuclear Polarization and H Detection From The DNP-NMR Blog: Magic Angle Spinning NMR of Proteins: High-Frequency Dynamic Nuclear Polarization and H Detection Su, Y., L. Andreas, and R.G. Griffin, Magic Angle Spinning NMR of Proteins: High-Frequency Dynamic Nuclear Polarization and H Detection. Annu Rev Biochem, 2015. http://www.ncbi.nlm.nih.gov/pubmed/25839340	nmrlearner	News from NMR blogs	0	04-17-2015 08:49 PM
[NMR paper] Magic Angle Spinning NMR of Proteins: High-Frequency Dynamic Nuclear Polarization and (1)H Detection. Magic Angle Spinning NMR of Proteins: High-Frequency Dynamic Nuclear Polarization and (1)H Detection. Magic Angle Spinning NMR of Proteins: High-Frequency Dynamic Nuclear Polarization and (1)H Detection. Annu Rev Biochem. 2015 Mar 30; Authors: Su Y, Andreas L, Griffin RG Abstract Magic angle spinning (MAS) NMR studies of amyloid and membrane proteins and large macromolecular complexes are an important new approach to structural biology. However, the applicability of these experiments, which are based on (13)C- and...	nmrlearner	Journal club	0	04-04-2015 05:31 PM
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</br> </br> We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20–25K 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 , but also includes a corrugated waveguide for transmission of microwaves from...	nmrlearner	Journal club	0	12-15-2012 09:51 AM
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
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

« 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