A new type of mesoscale material composed of anionically charged clusters of hexarhenium selenocyanide [Re6Se8(CN)6] 4-, linked by various divalent transition metals, in presence of cetylpyridinium bromide (CTPB) template in formamide solution, was described. The cubic mesostructures of hexarhenium selenocyanide clusters were prepared by choosing CTPB-formamide (FM) system as a template. It is found that the broad width of CN band in the mesostructured phase implies different bonding environments for cyanide ligands. A highly relative concentration of divalent metal ions strongly inhibit the self-assembly procedure mediated by positively charged CTP+ micelles through a competitive process, producing dense microcrystalline materials. The successful incorporation of the template CTPB in the mesostructured phase is confirmed by Fourier-transform infrared spectroscopy.