With the opportunity to study this MOF-electrolyte anion interaction, we further employed NMR to study a system previously reported to have negligible ion uptake (at null potential), by soaking Ni3(HITP)2 with 1 M sodium triflate in dimethyl formamide (NaSO3CF3/DMF) electrolyte (Figure ). The resulting spectrum closely resembles those of the other organic electrolyte systems, with two peaks which we assign to in-pore and ex-pore environments, and a F Δδ of +1.6 ppm. The charge density on the fluorine atoms in the SO3CF3 -anion from DFT calculations is similar to the TFSI -anion, supporting a similarly weak interaction with the MOF compared to BF4 -(Figure ) and thus a smaller Δδ (SI Figure ). The larger Δδ relative to TFSI -(Figure ) is likely a result of the smaller anion size of SO3CF3 - allowing on average a closer approach of the anion to the MOF than TFSI -. As before, note that significant spinning sidebands are present only for the more anisotropic in-pore environment in this system, supporting our assignments (SI Figure , SI Table ). Overall, our results suggest that there is in fact a significant in-pore anion population even without charging, in contrast with the negligible ion uptake previously reported by He et al. These findings highlight the significant power of F NMR to probe ion adsorption and specific MOF-electrolyte interactions.