We recently reported heteroleptic complexes that can serve as precursor molecules for polynuclear compounds. Treatment of such a precursor molecule, [Co(bmsab)(dme)] (dme = dimethylether), with deprotonated 1,2,4,5-tetrakis(methanesulfonamido)benzene, followed by oxidation with ferrocenium, allowed the isolation of dinuclear 2 (see Scheme 1). After crystallization, phase-pure material was obtained in yields of up to 30 %, allowing the isolation of several hundreds of milligrams of 2. The chemical purity of the material was established by means of elemental analysis, UV/Vis/NIR spectroscopy (Fig. ) and powder X-ray diffractometry (Fig. ). The use of anhydrous KOH, and of 18-crown-6 as an encapsulating agent during deprotonation proved to be instrumental in isolating crystalline material in a reproducible manner. This observation will be explained below in terms of the crystal structure and packing.