General solid-state NMR experimental details

Solid-state NMR experiments were carried out at the solid-state NMR Facility at the University of St Andrews using Bruker Avance III 400 and 600 MHz NMR spectrometers, equipped with wide-bore superconducting 9.4 and 14.1 T magnets. Samples were packed into conventional 4.0, 3.2, 2.5, 1.9 and 1.3 mm ZrO2 rotors and rotated at rates between 1 and 60 kHz. 89

Y-containing powdered samples were packed into 4.0 mm Si3N4 rotors to

prevent the background signal appearing in the NMR spectrum. Solid- state NMR experiments were carried out using commercially available double- or triple-resonance probes. For low-γ nuclei, such as 67

Zn or 89

Y, a commercial low-γ double-resonance 4.0 mm HX probe was used. Higher- field solid-state NMR experiments were carried out at the UK 850 MHz Solid-State NMR Facility, held at the University of Warwick, using a Bruker Avance III 850 MHz NMR spectrometer equipped with a wide- bore superconducting 20.0 T magnet. This facility was funded by the EPSRC and BBSRC, as well as the University of Warwick including via part funding through Birmingham Science City Advanced Materials Projects 1 and 2, supported by Advantage West Midlands (AWM) and the European Regional Development Fund (ERDF). For specific details relating to each experiment, see the relevant figure captions.

2.7

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