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XRD results are not the only reason why we eliminate the possibility of dimer formation. It is important to note that dimer formation does not ensure π stacking and in that case the two events (hydrogen bonding and π stacking) are decoupled. However, we saw clear evidence of π stacking in spectroscopic experiments. That is the reason we believe the mode of hydrogen bonding must account for synergistic π-stacking interaction and that can be explained with the proposed syn-syn catemer formation. This was our hypothesis based on the above mentioned logic which we supported by XRD. However, it may be argued that interdigitations among the alkyl chains may also lead to shortening of interlayer spacing compared to the theoretically calculated length of fully extended NDI-1 dimer. However, in AFM images (Figure 4), we observed the height of the aggregates nearly matched to the estimated length of the two hydrogen-bonded NDI chromophores in the syn-syn catemer motif. It is difficult to imagine in that case how interdigitations of the alkyl chains can happen, because in a hydrophobic solvent like MCH, it is more likely that the hydrophilic carboxylic acid will be inside the aggregated fiber. Having argued this, it is also important to note that these are still indirect forms of evidence and at this moment we do not have any conclusive direct evidence to suggest that the proposed mode of assembly is the only possibility.
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