Structurally authenticated complexes of the cone-shaped p-sulfonatocalixarene and conformationally flexible p-sulfonatocalixarene devoid of co-ligands/ancillary molecules are limited. Early and late members of the lanthanide series as their trivalent ions, La3+, Er3+, and Yb3+, form complexes from aqueous media under these conditions. For La3+ and Er3+, distinct hydrophobic and hydrophilic bilayers are formed with p-sulfonatocalixarene, whereas for Yb3+, two complexes form that deviate from the well-known bilayer arrangement of calixarenes. Replacing the calixarene with p-sulfonatocalixarene results in a hydrogen-bonded network with alternating hydrophobic-hydrophilic layers associated with primary coordination of Yb3+, with the larger macrocyclic calixarene in a partial cone conformation.
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