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Improved Magnetization Transfers among Quadrupolar Nuclei in Two-Dimensional Homonuclear Correlation NMR Experiments Applied to Inorganic Network Structures
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).ORCID iD: 0000-0003-3242-0205
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).ORCID iD: 0000-0001-9409-2601
Number of Authors: 42020 (English)In: Molecules, ISSN 1431-5157, E-ISSN 1420-3049, Vol. 225, no 2, article id 337Article in journal (Refereed) Published
Abstract [en]

We demonstrate that supercycles of previously introduced two-fold symmetry dipolar recoupling schemes may be utilized successfully in homonuclear correlation nuclear magnetic resonance (NMR) spectroscopy for probing proximities among half-integer spin quadrupolar nuclei in network materials undergoing magic-angle-spinning (MAS). These (SR212)M, (SR214) M, and (SR218)M recoupling sequences with M = 3 and M = 4 offer comparably efficient magnetization transfers in single-quantum-single-quantum (1Q-1Q) correlation NMR experiments under moderately fast MAS conditions, as demonstrated at 14.1 T and 24 kHz MAS in the contexts of 11B NMR on a Na2O-CaO-B2O3-SiO2 glass and 27Al NMR on the open framework aluminophosphate AlPO-CJ19 [(NH4)2Al4(PO4)4HPO4 H2O]. Numerically simulated magnetization transfers in spin-3/2 pairs revealed a progressively enhanced tolerance to resonance offsets and rf-amplitude errors of the recoupling pulses along the series (SR212) M < (SR214)M < (SR218)M for increasing differences in chemical shifts between the two nuclei. Nonetheless, for scenarios of a relatively minor chemical-shift dispersions (. 3 kHz), the (SR212) M supercycles perform best both experimentally and in simulations.

Place, publisher, year, edition, pages
2020. Vol. 225, no 2, article id 337
Keywords [en]
interatomic connectivities, quadrupolar nuclei, half-integer spins, dipolar recoupling, B-11 NMR, Al-27 NMR, microporous aluminophosphate, borosilicate glass, glass structure
National Category
Chemical Sciences Biological Sciences
Identifiers
URN: urn:nbn:se:su:diva-181120DOI: 10.3390/molecules25020337ISI: 000515381800099PubMedID: 31947638OAI: oai:DiVA.org:su-181120DiVA, id: diva2:1426656
Available from: 2020-04-27 Created: 2020-04-27 Last updated: 2023-08-28Bibliographically approved

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Yu, YangKeil, PhilippHansen, Michael RyanEdén, Mattias

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