| ¹²⁷I NQR (298 ± 2 K) | DIB-BiPy: ν₁ = 287.98 ± 0.02 MHz and ν₂ = 573.0 ± 0.4 MHz; pristine DIB: ν₁ = 276.68 ± 0.03 MHz and ν₂ = 552.1 ± 0.3 MHz |
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| Operando ¹²⁷I NQR, ball milling at 40 Hz | Rapid emergence of the DIB-BiPy NQR signal at 572.98 MHz within 10 minutes of milling, alongside attenuation of the DIB reactant signal at 552.09 MHz. Full conversion was not achieved after 2 hours; a residual DIB signal persisted in the final NQR spectrum |
| Ex situ powder X-ray diffraction | Residual DIB was present at the end of the milling |
César Leroy, Danielle Laurencin, Daniel Valenza, Patrice Montels, Philippe Gaveau. “A novel operando tool for mechanochemistry: NQR spectroscopy.” ChemRxiv (). https://doi.org/10.26434/chemrxiv.15003997/v2
NQR temperature-calibration, milling-setup-heating, and Raman method-comparison results were not retained. No separate supporting information file was available on the ChemRxiv article page
| Operando ¹²⁷I NQR, ball milling at 50 Hz | A sharp ¹²⁷I NQR signal emerged within 180 minutes at 164.11 MHz and grew in intensity over time |
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