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α, β, γ, δ—Copper(II) tetraphenylporphyrinate (CuTPP) has been investigated as an active material in composites for optoelectronic devices, such as organic light-emitting diodes (OLEDs). This study focused on the spectroscopic, structural, and morphological analysis of CuTPP thin films obtained using layer-by-layer deposition. The infrared spectra of the films, deposited both on ceramic glass and indium tin oxide-coated glass, revealed that the substrate interacts with CuTPP, inducing the formation of aliphatic CH2 or CH3 and a general rearrangement of the bands related to the bending of phenyl groups. UV–vis spectroscopy indicated the presence of two bands at 350 and 472 nm in the films, instead of the intense band in the region between 380 and 500 nm corresponding to the Soret band. The structure of the complex was elucidated by single-crystal X-ray diffraction. X-ray powder diffraction analysis showed that films exhibited two peaks associated with the 101 and 103 planes, which noticeably increased after heating at 200 °C. Scanning electron microscopy images confirmed that the annealing favored the growth of two-dimensional square-shaped aggregates on the surface of the substrate.