Two new ferrocene-porphyrin derivatives, namely 5,15-bis(ferrocenyl)-10,20-bis(4-nitrophenyl)porphyrin (1) and its nickel congener 5,15-bis(ferrocenyl)-10,20-bis(4-nitrophenyl)porphyrinatonickel (2) have been designed, synthesized, and characterized. Their self-assembly properties have been comparatively studied by electronic absorption and FTIR spectroscopy, TEM, SEM, XRD, and X-ray photoelectron spectroscopy (XPS). Metal-free 1 self-assembles into nanospheres with diameters in the range of 30-50 nm, de-