To improve confidence in the peak assignments two-dimensional 1 H- C HETCOR experiments at short contact times were performed, allowing for the investigation of 1 H nuclei located near the 13 CO2 adsorption product. The 1 H-13 C HETCOR experiment for (e-2)2-Mg2(dobpdc) (Figure ) shows a strong correlation of the chemisorbed CO2 to a 1 H environment at d = 4.3 ppm. This 1 H signal can be assigned to HNCOO -, confirming the reaction of the CO2 to the e-2 primary amine species. A weaker correlation can also be seen with a 1 H signal at d = 13.2 ppm, arising from hydrogen bonding between the adsorption product and the secondary ammonium on an adjacent metal site. As such, these correlations provide greater evidence for ammonium carbamate chain formation. Conversely, in the