To validate that the obtained aggregates correspond to COF-300, we conducted synchrotron Xray diffraction measurements on both yellow powders (Figure ). The acquired diffraction data were subjected to fitting using the Pawley refinement method, employing the reported structural model as a reference. While the observed diffraction pattern of the nanoparticles with peaks at 2θ ( λ = 0.827 Å) = 3.52º (200), 4.96º (220), 7.05º (400), 9.67º (411), 10.57º (600) and 10.87º (501) can be assigned to the well-defined COF-300 structure, which crystallizes in the I41/a space group, the nanorods exhibit a distinct diffraction pattern that cannot be assigned to any reported structure despite their evident crystalline nature with observable peaks at 2θ ( λ = 0.827 Å) = 3.69º, 7.41º, 8.30º, 9.10º, 9.82º, and 11.13º. In addition, the refinement of COF-300 nanoparticles yielded a unit cell parameter of a = b = 26.89877 Å, c = 7.43909 Å and a unit-cell volume of 5382.5 Å 3 (see Table ). Accordingly, and considering the diamond topology associated to COF-300 and the aforementioned body-centered tetragonal space group, we observed that the obtained parameters for the nanoparticles closely correspond to a diamond net with 7-fold interpenetration (dia-c7), in which the degree of interpenetration (N) was determined with the unit cell parameters (see Equation S1 in the SI). The analysis using powder X-ray diffraction (PXRD) further confirmed the successful generation of COF-300 using the micellar approach at lower catalyst concentration (Figure ), despite the lower resolution of the XRD diffraction patterns. In contrast, when using the higher catalyst concentration (Figure ), the XRD pattern acquired from the resulting yellow powder did not correspond to the crystalline structure of COF-300, providing additional support to the synchrotron XRD measurements.