Lower rim 1,3-disubstituted p-tert-butylcalix[4]arene is studied here in its deprotonated form as complexing ligand for iron and chromium chloride. Crystallization of the two complexes from dry THF gives two different stoichiometries and structures, a trinuclear iron compound and a second, mononuclear structure with chromium. In both cases, the ligand adopts an elliptical shape and the metal...