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Three new heterometallic [Cr III  8 Ni II  6 ] coordination cubes of formulae [Cr III  8 Ni II  6 L 24 (H 2 O) 12 ](NO 3 ) 12 ( 1 ), [Cr III  8 Ni II  6 L 24 (MeCN) 7 (H 2 O) 5 ](ClO 4 ) 12 ( 2 ), and [Cr III  8 Ni II  6 L 24 Cl 12 ] ( 3 ) (where HL = 1-(4-pyridyl)butane-1,3-dione), were synthesised using the paramagnetic metalloligand [Cr III L 3 ] and the corresponding Ni II salt. The magnetic skeleton of each capsule describes a face-centred cube in which the eight Cr III and six Ni II ions occupy the eight vertices and six faces of the structure, respectively. Direct current magnetic susceptibility measurements on ( 1 ) reveal weak ferromagnetic interactions between the Cr III and Ni II ions, with J  Cr-Ni = + 0.045 cm -1 . EPR spectra are consistent with weak exchange, being dominated by the zero-field splitting of the Cr III ions. Excluding wheel-like structures, examples of large heterometallic clusters containing both Cr III and Ni II ions are rather rare, and we demonstrate that the use of metalloligands with predictable bonding modes allows for a modular approach to building families of related polymetallic complexes. Compounds ( 1 )-( 3 ) join the previously published, structurally related family of [M III  8 M II  6 ] cubes, where M III = Cr, Fe and M II = Cu, Co, Mn, Pd.

[CrIII8NiII6]n+ Heterometallic Coordination Cubes