Corrugation of triazine-based, 2D networks has been predicted computationally in the past, however, to this date there was no experimental evidence to support it. To corroborate that the removal of intercalated ions is indeed accompanied by corrugation and delamination, we compared the experimentally obtained diffractogram of PTI-IF with the simulated diffraction patterns of corrugated and non-corrugated PTI-structures in three different stacking arrangements: (i) alternating layers with a mirror plane through the triazine units (AA*), (ii) eclipsed orientation (AA), and (iii) staggered orientation (AB). Simulated diffraction patterns based on the corrugated structures match the experimental data better (δRwp = 2-7%), and they correctly describe the peak at 18° 2Θ (assigned as -111) than the non-corrugated ones. The best Pawley fit was obtained for the corrugated PTI-IF structure in AA* stacking mode (Figure , a-b, Table , Figure ). Further evidence for the corrugation of PTI-IF comes from CBED (Figure , Figure ). In the case of a perfectly planar, intercalated PTI-LiBr structure, we observe no discrepancies between observed and predicted patterns (Figure ). For PTI-IF, once again the corrugated structure reproduces the experimental pattern better. In particular, simulated ED patterns based on the corrugated PTI-IF structure account correctly for the missing systematic absences in the 100 zone axis pattern (Figure , d, Figure ). We note however, that an AB flat structure also shows a loss of the systematic absences. This means a clear assignment of the effect to corrugation or the presence of other stacking modes is still not possible from the ED patterns.