Acceleration of indirect detection 195 Pt solid-state NMR experiments by sideband selective excitation or alternative indirect sampling schemes

• Published in: Journal of magnetic resonance (1997) 2023-07, Vol.352, p.107457
• Main Authors: Atterberry, Benjamin A, Wimmer, Erik, Estes, Deven P, Rossini, Aaron J
• Format: Article
• Language: English
• Subjects: Acceleration; Anisotropy; Isotopes; Magnetic Resonance Imaging; Magnetic Resonance Spectroscopy - methods
• ISSN: 1096-0856

The measurement of the of chemical shift (CS) tensors via solid-state NMR (ssNMR) spectroscopy has proven to be a powerful probe of structure for organic molecules, biomolecules, and inorganic materials. However, when measuring the NMR spectra of heavy spin-1/2 isotopes the chemical shift anisotropy (CSA) is commonly on the order of thousands of parts per million, which makes acquisition of NMR spectra difficult due to the low NMR sensitivity imposed by the breadth of the signals and challenges in uniformly exciting the NMR spectrum. We have recently shown that complete Pt NMR spectra could be rapidly measured by using Pt saturation or excitation selective long pulses (SLP) with multiple rotor-cycle durations and RF fields less than 50 kHz into H{ Pt} or H- P{ Pt} PE S-RESPDOR, TONE D-HMQC-4, J-resolved, and J-HMQC pulse sequences. The SLP only provide signal or dephasing when they are applied on resonance with a spinning sideband. The magic angle spinning Pt NMR spectrum is reconstructed in the sideband selective NMR experiments by acquiring 1D NMR spectra at variable Pt pulse offsets. In this work, we present a detailed investigation of the specific pulse conditions required for the ideal performance of sideband selective experiments. Sideband selective experiments are shown to be able to accurately reproduce MAS NMR spectra with minimal distortions of relative sideband intensities. It is also demonstrated that a Pt NMR spectrum indirectly detected with HMQC can be rapidly obtained by acquiring a single rotor cycle of indirect dimension evolution points. We dub this method One Rotor Cycle of Acquisition (ORCA) HMQC. Sideband selective experiments and ORCA HMQC experiments are shown to provide a one order of magnitude improvement in experiment times as compared to conventional wideline HMQC experiments.