This study presents a general method which can be used for the synthesis of mononuclear complexes with europium(III) and organic ligands with carboxylic groups. It describes the procedure for preparing a new mononuclear coordination complex with europium(III) and carboxylate ligands sourced from benzoic acid. The construction of mononuclear complexes with a coordination sphere saturated in carboxylic ligands must go through the preparation and purification of a europium(III) intermediate complex that presents a coordination sphere with anions that will be later exchanged for carboxylic groups and finally precipitated as a solvent-free or anion-free complex within the coordination sphere. The detailed synthesis procedure for powders of a new complex, as well as studies of its structural composition at each phase and luminescent properties, are detailed in this study. Analytical and spectroscopic data reveal the formation of a new mononuclear complex of the general formula [Eu(OOCC6H5)3·(HOOCC6H5)2]. The crystal structure of the Eu(III) complex was solved using X-ray powder diffraction data and EXPO2014 software, and the crystal structure result was deposited in the CCDC service with number 19771999.