A novel metallo-organic ligand [RuL2] with four uncomplexed coordination sites was created, and upon treatment with Zn2+ generated a dimetallic 3D metallosupramolecule in nearly quantitative yield. This self-assembly process gave stable intermediates, opening the pathway to the first 3D metallo-assembly possessing two Ru2+, two Fe2+, and two Zn2+ ions precisely located in the different edges. This strategy opens the door to novel designer 3D polymetallic constructs capable of diverse applications.