In this paper we report the study of metallo-organic polymer gels of [Fe(II) (4-octadecyl-1,2,4-triazole)3(ClO4)2]n in toluene. A thorough investigation of the molecular structure and the viscoelastic properties of the metallo-organic polymer gels in toluene has been carried out by small angle neutron scattering and controlled stress oscillatory rheology as a function of temperature and concentration in order to understand the self-assembly process leading to the gel formation. The results obtained point out a side-by-side aggregation of the individual metallo-organic polymer chains, behaving as “living” polymers, into fibres of different cross-sections as responsible for the gelation of these systems.