Solid State NMR News Sebastian Wegner, Bruker BioSpin GmbH, Rheinstetten, Germany 40. Deutsches NMR Meeting
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
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 ( 13 C and 15 N 2D correlations at natural abundance Materials (frameworks, MOFs)
DNP of MOFs DNP-enhanced 15 N{ 1 H} CPMAS NMR spectra of UiO-66-NH 2 (a), UiO-66- NH 2 exposed to KCl (b), and Pt 2+ - loaded samples The NH 2 Pt peak grows linearlywith Pt loading of the MOF. Estimates of the ratio of free NH 2 vs. NH 2 Pt can be made based on the relative peak intensities in the NMR spectra.
Solid-State DNP NMR Spectrometer Gyrotron and Klystron Options DNP with Gyrotron 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 DNP with Klystron (EIK) Available 2017
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!
MAS 3 High Accuracy MAS regulation for 0.7 mm Standard deviation less than 4Hz Long term stability for more than 7 hours tested
Tools
Solution State / Solid State MAS NMR
BL 0.7 mm first results hnh 2D correlation@ 111kHz Coherence Lifetimes & Linewidths (Gb1) Data courtesy of Guido Pintacuda, ENS Lyon
Structure Elucidation of a capsid protein 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 PNAS 2016 113 (33) E4757-E4758
1. Backbone Resonance Assignment
2. Elucidating Hα @ >100kHz MAS 15 N-Linked Hα Detected Walk 13 CO Linked Hα Detected Walk -> linking over prolines
15 N-Linked Hα Detected Walk
3. Rapid Side Chain Assignment
4. Proximities Between Protons in Side-Chain
5. Automatic Structure Calculation with UNIO (T. Herrmann)
Paramagnetic Metalloproteins: Metal Ion Coordination
Paramagnetic Solids Large Offsets and Large Shift Anisotropies pnmr Network
Lanthanide luminescent complexes
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
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
Support of Chemagnetics, Varian and Agilent MAS probes Probe probe adaptor plate for WB system Probe adaptor plate mounted to the probe transport frame
Support of Chemagnetics, Varian and Agilent MAS probes Probe with adaptor plate mounted to the Bruker Shim coil
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
New MAS III Firmware 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) 28
New MAS III Firmware 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 29
New MAS III Firmware 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 30
Application Notes 1 H-Detection for Protein Samples full set of ten 1 H-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 1 H-detection Experiments explained in more detail Straightforward optimization protocol 31
Application Notes BSH CP for Protein Samples 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 32
Application Notes Where to find them? www.bruker.com Home. Products. Magnetic Resonance. NMR. Probes. Solids. Very Fast MAS. 0.7 mm. Learn More 33
Application Notes Where to find them? www.theresonance.com application note 34
New TopSolids2 Where to find Topsolids2
Solid State NMR Training Courses www.bruker.com Other courses available upon request: 13 C-detected solid state NMR on protein samples 1 H-detected solid state NMR on protein samples TopSolids CRAMPS We are always open for further suggestions: solids@bruker.com 36
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: solids@bruker.com
Copyright Innovation 2015 Bruker Bruker with Corporation. Integrity Corporation. All rights reserved. www.bruker.com All rights reserved.