Of note is the observation that no free ligand (L) was detected in the volatile byproducts, with the exception of reactions 1-3 where the ligands and AlCl 3 were supplied separately and deliberately with a slight excess of the ligand. This indicates that L/Al = 1 is maintained. In the case of precursors L-AlX3 (X = Me, Et, Cl) (reactions 1-15), the gravimetric Similarly, evidence that more SnMe4 is generated in THF could be found in the contrast between reactions 2, 7 (in THF) and reaction 4 (in toluene). Finally, reaction 6, which was conducted at an increased temperature (100 °C), produced roughly twice as much SnMe4 as the corresponding reaction at 60 °C (5), leading to the highest overall average connectivity (3.59 on Al / 3.54 on CUBE) at the formation of a porous gel structure (BET 126 m 2 g -1 ).