Heating to 550 °C under a constant oxygen flow leads to the thermal decomposition and/or burn-off of any organic components in the V2O5 samples (caution: temperatures above ca. 600-650 °C should be avoided in these TGA experiments due to the low melting temperature of V2O5). The mass loss upon heating of the V2O5-alkyldiamine samples occurs mainly in two steps, as shown in Fig. . The mass loss below ca. 150 °C is attributed to the loss of surface water and/or crystal water in the interlayer space. This mass loss corresponded to ca. 5 wt.%, 3.5 wt.%, and 2 wt.% for V2O5-2C-DA, V2O5-6C-DA, and V2O5-12C-DA, respectively. The second step between ca. 200-400 °C, accounting for a subsequent mass loss of 8 wt.%, 9.7 wt.%, and 16.5 wt.% for V2O5-2C-DA, V2O5-6C-DA, and V2O5-12C-DA, respectively, is ascribed to the decomposition and/or burn-off of the alkyldiamine pillars. While the molar ratio of educts in the reactions is chosen as 1:1 for alkyldiamine to vanadium, the TGA experiments reveal a product composition with significantly less pillars. The ratio of alkyldiamine pillars in the products is comparable for all samples, with a slightly higher number for 2C-DA, which is explained by its small size and low boiling point that allows for higher mobility during the synthesis.