By mixing ferrocenecarboxylic acid with 4,4’-azopyridine in methanol, in a basic medium created by adding 2,6-lutidine, a supramolecular structure has been formed as can be seen in Figure 1. Figure 1 Both FTIR spectrum and single crystal X-ray diffraction revealed association through hydrogen bonds. The main packing unit represents a centrosymmetric associate stabilized via strong intermolecular O-H···N hydrogen bonding, were carboxylic group acts as donor while pyridine nitrogen as acceptor: O−H···N [O−H 0.82 Å, H···N 1.89 Å, O1···N 2.679(3) Å, O1−H···N1 179.8°]. The spin state of the iron nucleus was verified by Mössbauer spectroscopy while the redox behavior was studied by cyclic voltammetry.