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In aqueous solutions, thiacalixarene (TCAS) and LnIII (= NdIII, YbIII) self‐assembled over a long period of time (1 d) to form 3:2 complexes LnIII3·TCAS2 in which the LnIII3 core is sandwiched between two TCAS ligands, which results in a high kinetic stability. This was not expected from the exo‐coordination fashion of TCAS with the O,S,O donors found in the 1:1 complex LnIII·TCAS, and thus this feature...
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