This dataset contains supplementary materials related to the publication “Sustainable and eco-friendly single- and multilayer polyester foils from polylactide (PLA) and poly(ethylene 2,5-furandicarboxylate) (PEF)” published in Molecules 2025, 30(1), 178; https://doi.org/10.3390/molecules30010178 . The uploaded files include experimental data, processing parameters, and additional characterization results supporting the preparation and evaluation of single-layer and multilayer polyester films based on PLA and PEF. The materials provide detailed information on film fabrication, material compositions, and physicochemical characterization, including mechanical, thermal, and structural properties. These data complement the results presented in the publication and are intended to ensure transparency, reproducibility, and further research on sustainable bio-based polyester materials and their potential applications in environmentally friendly packaging systems.