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The environmental aspects of ore processing and waste treatment call for an optimization of applied technologies. There, understanding of the structure and complexation mechanism on a molecular scale is indispensable. Here, the complexation of U VI  with a calix[4]arene‐based 8‐hydroxyquinoline ligand was investigated by applying a wide range of complementary methods. In solution, the formation of two complex species was proven with stability constants of log  ß  1:1 =5.94±0.02 and log  ß  2:1 =6.33±0.01, respectively. The formation of the 1:1 complex was found to be enthalpy driven [Δ H  1:1 =(−71.5±10.0) kJ mol −1 ;  T Δ S  1:1 =(−37.57±10.0) kJ mol −1 ], whereas the second complexation step was found to be endothermic and entropy driven [Δ H  2:1 =(32.8±4.0) kJ mol −1 ;  T Δ S  2:1 =(68.97±4.0) kJ mol −1 ]. Moreover, the molecular structure of [UO 2 (H 6 L)(NO 3 )](NO 3 ) ( 1 ) was determined by single‐crystal X‐ray diffraction. Concluding, radiotoxic U VI  was separated from a Eu III ‐containing solution by the calix[4]arene‐based ligand in solvent extractions.

chemistryopen

Uranium(VI) Complexes with a Calix[4]arene‐Based 8‐Hydroxyquinoline Ligand: Thermodynamic and Structural Characterization Based on Calorimetry, Spectroscopy, and Liquid–Liquid Extraction