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The mixed ligand coordination compounds containing acesulfamato and N,N -diethylnicotinamide biomolecules of some rare earth metal cations (Eu 3+ , Tb 3+ , Ho 3+ , Er 3+ and Yb 3+ ) were synthesized, and their structural properties were investigated. Possible structural formulas have been proposed by determining the chemical composition of molecules (elemental analysis), binding properties (infrared spectroscopy, mass analysis, solid-state UV-vis spectroscopy), thermal degradation properties (TGA / DTA curves). Based on the data collected, it is suggested that rare earth metal cations with a 3+ oxidation state have sextet coordination. The geometries of the structures were thought to be distorted octahedral. The charge balance of the coordination sphere is balanced by a monoanionic acesulfamato located outside the coordination sphere. When the thermal behaviours of the complexes were examined, it was determined that the compounds with Eu 3+ , Tb 3+ , and Yb 3+ metal cations contained one hydrate water outside the coordination sphere. Hydrate waters do not exist in the Ho 3+ and Er 3+ metal cation-centred complexes. At the end of the thermal decomposition analysis of all complex structures, it was determined that they leave the relevant metal oxides in the reaction vessels as final decomposition products.