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Solid State NMR News
Peter Gierth, Bruker UK / Sebastian Wegner, Bruker BioSpin GmbH Bruker UK Users’ Meeting
Innovation with Integrity
Solid State NMR News
• Solid State DNP NMR
• 111 kHz MAS NMR
• Adaptor kit for Varian and Chemagnetics probes
• MAS III firmware upgrades
• Application notes
• Training courses
Innovation with Integrity
Solid State DNP NMR
• Many applications in solid state NMR suffer from insufficient sensitivity
• Solid state DNP NMR today is the method of choice to solve this
– Biological systems (membrane proteins, fibrils etc.)
– Pharmaceuticals (13C and 15N 2D correlations at natural abundance
– Materials (frameworks, MOFs)
Innovation with Integrity
DNP of MOFs
• DNP-enhanced 15N{1H} CPMAS NMR spectra of UiO-66-NH2 (a), UiO-66-NH2 exposed to KCl (b), and Pt2+-loaded samples
• The –NH2 Pt peak grows linearlywith Pt loading of the MOF. Estimates of the ratio of free NH2 vs. –NH2 Pt can be made based on the relative peak intensities in the NMR spectra.
Innovation with Integrity
Solid-State DNP NMR Spectrometer Gyrotron and Klystron Options
Work in Progress: 263 GHz Klystron
• Offer a lower-price more compact
microwave source at 263 GHz
• Design compatible with possible upgrade later to gyrotron for full power performance
• Power output ~ 5 W • Available 2017
DNP with Gyrotron
DNP with Klystron (EIK)
Innovation with Integrity
111kHz - 0.7mm MAS Probe
• Highest available MAS rate
• High RF excitation in the 0.5MHz regime
• MAS stability of better than 0.25 ‰ at 111kHz (±28Hz max)
• 500nl Volume (350nl active volume)
• Available for SB/WB in HX / HXY / HCN configuration
• MAS 3 is mandatory !
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MAS 3 – High Accuracy MAS regulation for 0.7 mm
• Standard deviation less than 4Hz
• Long term stability for more than 7 hours tested
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Tools
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Solution State / Solid State MAS NMR
Innovation with Integrity
BL 0.7 mm – first results hNH 2D correlation@ 111kHz
Coherence Lifetimes & Linewidths (Gb1)
Data courtesy of
Guido Pintacuda, ENS Lyon
Innovation with Integrity
• GB1 proved possibilities
• In 2016 unknown structures are targeted
• Picture shows a e.g.capsid
Data on the following slides courtesy of Guido Pintacuda, ENS Lyon
Structure Elucidation of a capsid protein
PNAS 2016 113 (33) E4757-E4758
Innovation with Integrity
1. Backbone Resonance Assignment
Innovation with Integrity
2. Elucidating Ha @ >100kHz MAS
15N-Linked Ha Detected Walk 13CO Linked Ha Detected Walk -> linking over prolines
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15N-Linked Ha Detected Walk
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3. Rapid Side Chain Assignment
Innovation with Integrity
4. Proximities Between Protons in Side-Chain
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5. Automatic Structure Calculation with UNIO (T. Herrmann)
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Paramagnetic Metalloproteins: Metal Ion Coordination
Innovation with Integrity
Paramagnetic Solids Large Offsets and Large Shift Anisotropies
pNMR Network
Innovation with Integrity
Lanthanide luminescent complexes
Innovation with Integrity
Solid State NMR News
• Solid State DNP NMR
• 111 kHz MAS NMR
• Adaptor kit for Varian and Chemagnetics probes
• MAS III firmware upgrades
• Application notes
• Training courses
Innovation with Integrity
Support of Chemagnetics, Varian and Agilent MAS probes
• Bruker provides an adaptor kit for solid state NMR probes
from
• Easy integration of these probes into the Bruker workflow
• Full integration of the VT operation
• Full integration of the MAS operation
• Scope of the kit
• Probe adaptor plate
• VT adaptor for Johnston coupling
• Pneumatic adaptors and electrical interface for MAS
controller
Innovation with Integrity
Support of Chemagnetics, Varian and Agilent MAS probes
• Probe probe adaptor
plate for WB system
• Probe adaptor plate mounted
to the probe transport frame
Innovation with Integrity
Support of Chemagnetics, Varian and Agilent MAS probes
• Probe with adaptor plate mounted to the Bruker Shim coil
Innovation with Integrity
Support of Chemagnetics, Varian and Agilent MAS probes
• Top: VT stack of a WB system with a
Bruker Johnson VT adaptor for
experiments above room temperature
• Right: poking out VT stack of WB
magnet. Includes black adaptor flange
on top of Bruker shim stack
Innovation with Integrity
New MAS III Firmware
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Different to former MAS units, MAS III firmware updates are straightforward:
1. open the Swiss FTP server ‘ftp://ftp.bruker.ch’ in an internet browser
2. go to: ‘/NMR/download/servtools/firmware/mas/’
3. download the latest firmware (e.g. to your desktop or home directory)
Innovation with Integrity
New MAS III Firmware
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Different to former MAS units, MAS III firmware updates are straightforward:
4. open TopSpin and the MAS Display (‘masdisp’)
5. open the tab ‘Configuration’ in the MAS display
6. Click on ‘MAS firmware update’
Innovation with Integrity
New MAS III Firmware
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Different to former MAS units, MAS III firmware updates are straightforward:
7. in the MAS webpage browse to the just downloaded firmware file
8. click on ‘Update’
mas3_20151008_1638.bin
Innovation with Integrity
Application Notes – 1H-Detection for Protein Samples
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• full set of ten 1H-detected experiments combined with (ultra-) fast MAS
• for protein backbone & side chain assignment
• available with at least TopSpin 3.2.7/ 3.5.3 (or on demand)
• 3 Application Notes explain theoretical and practical aspects:
Introduction to 1H-detection
Experiments explained in more detail
Straightforward optimization protocol
Innovation with Integrity
Application Notes – BSH CP for Protein Samples
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• Band-Selective Homonuclear Cross Polarization
• homonuclear C-C transfer in NCαCx and NCOCx experiments is essential for protein backbone assignment
• BSH CP represents a highly robust & efficient dipolar-based transfer method
• efficiently suppresses:
• unwanted sequential & long-range C-C transfers by dipolar truncation
• undesirable transfer to Cβ resonances
• five different experiments implemented from 1D up to 4D
• tested for protonated & deuterated samples
• available with at least TopSpin 3.2.6 / 3.5.2 or on demand
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Application Notes – Where to find them? www.bruker.com
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Home . Products . Magnetic Resonance . NMR . Probes . Solids . Very Fast MAS . 0.7 mm . Learn More
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Application Notes – Where to find them? www.theresonance.com
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application note
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New TopSolids2 – Where to find Topsolids2
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Solid State NMR Training Courses – www.bruker.com
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Other courses available upon request:
• 13C-detected solid state NMR on protein samples
• 1H-detected solid state NMR on protein samples
• TopSolids
• CRAMPS
We are always open for further suggestions: [email protected]
Innovation with Integrity
Acknowledgements
• core application people solid-state NMR:
Gerhard Althoff (DE)
Venita Decker (DE)
Sebastian Wegner (DE)
Barbara Perrone (CH)
Jochem Struppe (US) Fabien Aussenac (F) for DNP
+ all the other application people world wide!
• important E-mails:
Innovation with Integrity © Copyright Bruker Corporation. All rights reserved.
Innovation with Integrity
Copyright © 2015 Bruker Corporation. All rights reserved. www.bruker.com