In Figure , samples Br-170 and I-110 show a well-defined stacking pattern, while Br-110 shows a multiple-phase profile. Sample I-170 does not show any evidence of an organized superlattice due to its large variation in size in all dimensions. To extract the parameters from these scattering curves, we fitted the peaks with Lorentzian functions, and, for the background (i.e., scattering from solvents, capillary, etc.), we used a sum of different spheric populations only to match the curve (no physical meaning). An example of the fitting is shown in Figure , and the parameters extracted from all samples are summarized in Table . The family of peaks enumerated from 1 to 3 is consistent with Bragg reflections from a lamellar crystal structure resulting from the stacking of the PNPls. Sample Br-170 shows an additional scattering feature between 0.03 and 0.06 Å -1 that corresponds to the space between columns of stacks (average of 14 nm), in agreement with the FFT of the STEM image in Figure . The scattering signal is broad because this distance varies with the lateral size of the Br-170 PNPls. Sample I-110 does not show the same broad feature in low-Q values, which suggests that the stacks of these PNPls are randomly oriented and not laterally aligned. This observation also agrees with what we observed in its STEM image in Figure . The reason for this lack of column alignment might be the higher variability of the B-and C-side in this sample compared to its Br-170 analogue. Sample Br-110 shows different features in addition to the diffractions from the lamellar phases observed in its counterparts. First, we can distinguish two different lamellar structures in this sample with slightly different particle distances: d1 = 5.15 and d1' = 4.81 nm (Table ). The peaks of the second lamellar phase are marked with a prime for clarity (1' and 2'). The distinction of the peak 1 is challenging due to the convolution of 3 diffractions in this region (Figure ). The existence of two lamellar phases is somewhat consistent with the difference between the thickness (A-side) and the B-side in this sample (Table ). Coexisting with the two lamellar phases, we can also assign an extra crystalline phase of the NWs. The peaks at 0.113 Å -1 (√1) and 0.198 Å -1 (√3) present relative positions with the ratio √1:√3, which can be related to an hexagonal phase. Lastly, sample Br-110 presents a gravitational effect, causing the NWs to orient vertically relative to the X-ray beam. This effect generates higher-intensity signals along the Qy axis of the diffraction discs, as depicted in Figure .