title: Straightforward, effective calibration of SPINAL-64 decoupling results in the enhancement of sensitivity and resolution of biomolecular solid-state NMR.
abstract: We describe a simple yet highly effective optimization strategy for SPINAL-64 ¹H decoupling conditions for magic-angle spinning solid-state NMR. With adjustment of the phase angles in a coupled manner, the optimal conditions resulting from three parameter optimizations can be determined with adjustment of a single phase. Notably, echo T₂ relaxation times for ¹³C and ¹⁵N show significant enhancement (up to 64%), relative to the previous described SPINAL-64 conditions, under the moderate ¹H decoupling levels (60-100 kHz) and MAS rate (13.3 kHz) commonly employed for high-resolution SSNMR spectroscopy of proteins. Additionally, we also investigated the effect at higher spinning rate (33.3 kHz) and compared the results with other ¹H decoupling schemes (TPPM, XiX), as well as SPINAL-64 with the originally reported optimal values.
authors.affiliation: Center for Biophysics and Computational Biology, University of Illinois at Urbana-Champaign, Urbana, IL 61801, USA.
authors.forename: Gemma
authors.initials: G
authors.lastname: Comellas
authors.forename: Jakob J
authors.initials: JJ
authors.lastname: Lopez
authors.forename: Andrew J
authors.initials: AJ
authors.lastname: Nieuwkoop
authors.forename: Luisel R
authors.initials: LR
authors.lastname: Lemkau
authors.forename: Chad M
authors.initials: CM
authors.lastname: Rienstra
mesh_terms: D002138:Calibration; D002250:Carbon Radioisotopes / Q000737:chemistry; D017352:Echo-Planar Imaging; D004574:Electromagnetic Fields; D009590:Nitrogen Radioisotopes / Q000737:chemistry; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000295:instrumentation / Q000379:methods*; D011522:Protons
chemical_list: D002250:Carbon Radioisotopes; D009590:Nitrogen Radioisotopes; D011522:Protons