Dynamic nuclear polarisation of 1H in Gd-doped In(OH)3

Dynamic nuclear polarisation (DNP) of solids doped with high-spin metal ions, such as Gd3+, is a useful strategy to enhance the nuclear magnetic resonance (NMR) sensitivity for these samples. Spin diffusion can relay polarisation throughout a sample, which is most effective for dense 1H networks, while the efficiency of DNP using Gd3+ depends on the symmetry of the metal site. Here, we investigate cubic In(OH)3 as a high-symmetry, proton-containing material for endogenous Gd DNP. A 1H enhancement of up to 9 is demonstrated and harnessed to measure the 17O spectrum at natural abundance. The enhancement is interpreted in terms of clustering of the Gd3+ dopants and the local reduction in symmetry of the metal site induced by proton disorder, as demonstrated by quadrupolar 115In NMR. This is the first example of 1H DNP using Gd3+ dopants in an inorganic solid.& COPY; 2023 The Authors. Published by Elsevier Inc. This is an open access article under the CC BY license (http:// creativecommons.org/licenses/by/4.0/).

Automated summary

Dynamic nuclear polarisation (DNP) using high-spin metal ions, such as Gd3+, can enhance nuclear magnetic resonance (NMR) sensitivity. Spin diffusion and metal site symmetry are factors affecting DNP efficiency. In this study, cubic In(OH)3 was investigated as a high-symmetry proton-containing material for DNP using endogenous Gd3+. A 1H enhancement of up to 9 was achieved, and the clustering of Gd3+ dopants and the local reduction in symmetry of the metal site induced by proton disorder were identified as the reasons for the enhancement. This is the first example of 1H DNP using Gd3+ dopants in an inorganic solid.