The title compounds were synthesized via click reaction. They were characterized by IR, H-1-NMR, elemental analysis, UV, fluorescence in solution were also applied to characterise their photophysical characterization and single-crystal X-ray diffraction analysis. 1,1-Ferrocene-dicarboxyl-{[(3-methylphenyl)-imino]di-2,1-ethanediyl} 1 (C23H23FeNO4) crystallizes in the monoclinic system, with a = 7.4261(13), b = 29.911(5), c = 9.8426(13) angstrom, = 90 degrees, = 118.251(10)degrees, = 90 degrees, V = 1925.8(5) angstrom(3,) 1,1-Ferrocene-dicarboxyl-{[(2-methylphenyl)-imino]di-2,1-ethanediyl} 2 (C23H23FeNO4) crystallizes in the monoclinic system, with a = 15.4000 (15) , b =7.9007 (8) , c = 16.0776 (15) angstrom, = 90 degrees, = 94.266 (2)degrees, = 90 degrees, V = 1950.8 (3)angstrom (3), Both 1 and 2 form 3D net structures, which are further linked to form 3D supramolecular net structures via intermolecular CHO, CH and CHC stacking interactions, respectively. Fluorescent and UV-vis absorption spectra were also investigated.