Irrespective of increasing the number of AlCl3 equivalents unreacted dipyrrin remained after complexation but could be recovered via column chromatography. The majority of these complexes adopt a symmetrical octahedral geometry with clear signals in the proton and carbon NMR spectra testifying the expected symmetry. As mentioned, α-pyrrole protons of the dipyrrin precursors appear at a lower field ~7.5-7.6 ppm, whilst in the octahedral complex configuration they appear at higher field ~6.7-7.0 ppm. This stems from the increasing shielding effect (double) by the two adjacent dipyrrinato moieties. Moreover, mass spectrometry was employed and their exact mass was confirmed by APCI method. Additionally, the octahedral aluminum coordination center was confirmed via Al NMR with a signal/resonance in the range of 6.5-7.15 ppm which is characteristic of the octahedral coordination (between -46 and 40 ppm). The insufficient solubility of AL(DIPY)3 13g resulted in practical issues, thereby it was difficult to proceed with the complete photophysical characterization, but it was characterized by UV-Vis, NMR and MS.