This study performs a sono-photochemical method to get more effective therapeutic outcomes for cancer treatment. Additionally, sonochemical and sono-photochemical properties of lutetium phthalocyanines have been presented in this study for the first time. Although it aims to synthesize a series of new peripherally/nonperipherally mono lutetium (III) phthalocyanines (1-3Lu), the related double-decker lutetium (III) phthalocyanines (1?-3?Lu) were simultaneously synthesized. Characterization of the resulting macromolecules was carried out using diverse spectroscopic approaches including NMR (1H and 13C NMR; for 1-3Lu), UV?Vis, FT-IR, and Mass spectroscopy. The double-decker lutetium (III) phthalocyanines (1?-3?Lu) were also characterized by performing electron spin resonance (ESR) measurements. The solubility of all the new macromolecules was studied using different polar and non-polar organic solvents. The photophysicochemical properties of the resulting mono lutetium (III) complexes were analyzed and photochemical, sonochemical, and sono-photochemical properties were investigated to determine the efficiencies of singlet oxygen. When the data were compared, the highest singlet oxygen quantum yields (?? = 0.86 for 1-Lu, 0.96 for 2-Lu, 0.83 for 3-Lu) were obtained for the sonophotochemical studies. The results prove that sono-photochemical properties improve the therapeutic effects compared to photochemical ones.