✨ New paper out in #JACS! We looked at the intrinsically disordered CTD tail of #Hsp90 often seen as a passive linker. Turns out, it’s not.
#StructuralBiology #Biophysics #EPR #NMR
pubs.acs.org/doi/10.1021/...

Crystallographic and EPR-based characterisation of Cu2+-binding to serum albumin: ATCUN coordination and additional sites Copper homeostasis is essential for mammalian physiology. Serum albumin plays an important role in plasma copper transport and buffering, yet its Cu2+ binding sites have remained incompletely characte...

Just published: copper(II) binding to Human Serum Albumin. 1st structure including the ATCUN site that is square planar as expected. There are multiple copper(II) sites and EPR (including hyperfine and pulse dipolar) reveals occupation of multiple sites at low loading. doi.org/10.1039/D6QI...

Work just published in @natcomms.nature.com rdcu.be/e9ieD demonstrating how pulse dipolar EPR can resolve different states of a human transporter in native membranes. EPR contributions by @ackermannkatrin.bsky.social @st-andrewschem.bsky.social

Structural characterization and the role of EPR spectroscopy for protein–polymer conjugates Protein-polymer conjugates (PPCs) are an important class of therapeutic macromolecules offering improvements in protein stability, circulation time, a…

Protein–polymer conjugates: how do we understand their structure & dynamics? 🔬Our new review highlights EPR spectroscopy+complementary techniques for insights in vitro & in cells.
Read more 👇
www.sciencedirect.com/science/arti...
#ProteinPolymerConjugates #EPR #Biomaterials #PolymerScience

C-terminal domain dimerization in yeast Hsp90 is moderately modulated by the other domains Heat shock protein 90 (Hsp90) serves as a crucial regulator of cellular proteostasis by stabilizing and regulating the activity of numerous substrates, many of which are oncogenic proteins. Therefore,...

With growing interest in Hsp90 CTD inhibitors here's a reminder of our CTD study on yeast Hsp90. We showed the NTD and MD to modulate CTD dimerization and shape allostery; super relevant for CTD-targeted drug design #Hsp90 #allostery #DugDesign #Biophysics
www.cell.com/biophysj/ful...

Chiral molecular 4f qubits by post functionalization We herein demonstrate the synthesis of a pair of enantiomerically pure YbIII complexes by post-functionalisation of the parent YbIII complex via condensation with an enantiomerically pure chiral amine...

A new paper 📜 with the Piligkos Lab at DTUpublished in ‪@inorgchemfront.rsc.org‬ We show that Chiral molecular 4f qubits retain properties suitable for quantum information processing. Thanks to all involved. ⚛️ 🧪 doi.org/10.1039/D5QI...

The Radical S-Adenosyl-l-methionine Enzyme HydE Forms an Fe(I)Fe(I) Dimer En Route to the [FeFe] Hydrogenase H-Cluster [FeFe] hydrogenases are highly efficient metalloenzymes that catalyze hydrogen conversion via a sophisticated active site cofactor known as the H-cluster. Biosynthesis of its [2Fe]H subcluster, which ...

is the dimer core of the H-cluster of FeFe hydrogenase formed by rSAM chemistry in HydE?

pubs.acs.org/doi/full/10....

Cryogenic and Dissolution DNP NMR on γ-Irradiated Organic Molecules Nuclear magnetic resonance (NMR) plays a central role in the elucidation of chemical structures but is often limited by low sensitivity. Dissolution dynamic nuclear polarization (dDNP) emerges as a transformative methodology for both solution-state NMR and metabolic NMR imaging, which could overcome this limitation. Typically, dDNP relies on combining a stable radical with the analyte within a uniform glass under cryogenic conditions. The electron polarization is then transferred through microwave irradiation to the nuclei. The present study explores the use of radicals introduced via γ-irradiation, as bearers of the electron spins that will enhance 1H or 13C nuclides. 1H solid-state NMR spectra of γ-irradiated powders at 1–5 K revealed, upon microwave irradiation, signal enhancements that, in general, were higher than those achieved through conventional glass-based DNP. Transfer of these samples to a solution-state NMR spectrometer via a rapid dissolution driven by a superheated water provided significant enhancements of solution-state 1H NMR signals. Enhancements of 13C signals in the γ-irradiated solids were more modest, as a combined consequence of a low radical concentration and of the dilute concentration of 13C in the natural abundant samples examined. Nevertheless, ca. 700–800-fold enhancements in 13C solution NMR spectra of certain sites recorded at 11.7 T could still be achieved. A total disappearance of the radicals upon performing a dDNP-like aqueous dissolution and a high stability of the samples were found. Overall, the study showcases the advantages and limitations of γ-irradiated radicals as candidates for advancing spectroscopic dDNP-enhanced NMR.

One more DNP paper in JACS:
Cryogenic and Dissolution DNP NMR on γ-Irradiated Organic Molecules. We introduced γ-irradiation–generated radicals to enhance ¹H and ¹³C signals via DNP under cryogenic and dissolution conditions.
🔗 pubs.acs.org/doi/full/10....

#NMR #DNP #Hyperpolarization

Toward Generalized Solution-State 1H DNP NMR via Particle-Mediated Cross-Relaxation This study discusses a potential route for enhancing 1H NMR signals in the liquid phase at high magnetic fields for samples on the 100 μL volume scale using dynamic nuclear polarization (DNP). The approach involves dispersing an inert powder that is both rich in protons and capable of undergoing DNP with good efficiency at noncryogenic temperatures, and letting the solid 1H polarization thus enhanced pass from the dispersed particles onto the surrounding liquid via spontaneous cross relaxation effects. To this end, BDPA-doped polystyrene (PS) particles in the μm range were suspended in 30 μL of heptane, loaded into 3.2 mm sapphire rotors, and spun at ≈500 Hz for homogeneity purposes in a 14.1 T magnet. Irradiation with ≈13 W at 395 GHz while maintaining temperature in the 185–220 K range thus enhanced the PS proton polarization ≈12-fold within ≈2 s; after ca. 6 s of irradiation, this resulted in ca. 3-fold enhancements of the heptane proton resonances, while preserving their ≤2 Hz line widths. The conditions over which such particle-mediated transfer occurs were explored over a range of sample composition, deuteration and molecular weight; best results were obtained when polarizing a ball-milled powder made of deuterated-PS/PS/BDPA = 86.4/9.6/4.0 suspended on perdeuterated heptane-d16. While the solution-state enhancements provided by this approach are still relatively modest, its generality could open new avenues in DNP-enhanced 1H NMR that do not sacrifice on the volumes, on the high-resolution conditions, or on the multiscan averaging that is customary in contemporary applications.

New paper out in J. Phys. Chem. Lett.: Toward Generalized Solution-State ¹H DNP NMR.
BDPA-polystyrene boosts ¹H ~12× in 2s, transfers ~3× to liquids in 6s
🔗 pubs.acs.org/doi/full/10....
#NMR #DNP #Hyperpolarization