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A family of five [MIII2MII3]  n + trigonal bipyramidal cages (M III = Fe, Cr and Al; M II = Co, Zn and Pd; n = 0 for 1-3 and n = 6 for 4-5 ) of formulae [Fe 2 Co 3 L 6 Cl 6 ] ( 1 ), [Fe 2 Zn 3 L 6 Br 6 ] ( 2 ), [Cr 2 Zn 3 L 6 Br 6 ] ( 3 ), [Cr 2 Pd 3 L 6 (dppp) 3 ](OTf) 6 ( 4 ) and [Al 2 Pd 3 L 6 (dppp) 3 ](OTf) 6 ( 5 ) (where HL is 1-(4-pyridyl)butane-1,3-dione and dppp is 1,3-bis(diphenylphosphino)propane) are reported. Neutral cages 1-3 were synthesised using the tritopic [M III L 3 ] metalloligand in combination with the salts Co II Cl 2 and Zn II Br 2 , which both act as tetrahedral linkers. The assembly of the cis -protected [Pd II (dppp)(OTf) 2 ] with [M III L 3 ] afforded the anionic cages 4-5 of general formula [MIII2PdII3](OTf) 6 . The metallic skeleton of all cages describes a trigonal bipyramid with the M III ions occupying the two axial sites and the M II ions sitting in the three equatorial positions. Direct current (DC) magnetic susceptibility, magnetisation and heat capacity measurements on 1 reveal weak antiferromagnetic exchange between the Fe III and Co II ions. EPR spectroscopy demonstrates that the distortion imposed on the {MO 6 } coordination sphere of [M III L 3 ] by complexation in the {MIII2MII3} supramolecules results in a small, but measurable, increase of the zero field splitting at M III . Complete active space self-consistent field (CASSCF) calculations on the three unique Co II sites of 1 suggest D  Co ≈ -14 cm -1 and E / D ≈ 0.1, consistent with the magnetothermal and spectroscopic data.

[MIII2MII3]n+ trigonal bipyramidal cages based on diamagnetic and paramagnetic metalloligands

[MIII2MII3]ⁿ⁺ trigonal bipyramidal cages based on diamagnetic and paramagnetic metalloligands