Poly(GVGVP) is the head of a novel group of biopolymers showing exceptional potential for future applications in different fields such as biomedical, environmental, energy or industrial. Taking into account their future development, further knowledge is needed to understand the molecular basis of their remarkable behaviour and other structural and technical parameters. This paper is devoted to a particular task of this challenge: the structural study of its solid state, which is approached for the first time in this work. Thermal, wide-angle X-ray diffraction and vibrational Raman analysis were used. On the whole, all the observations are consistent with the existence of a metastable amorphous phase composed by polymer chains without apparent conformational order. The main structural property is the existence of an extensive and dense net of hydrogen bonds, which seemed to comprise the majority of the amide groups present. Thermal treatment induces structural changes on this polymer. Part of the hydrogen bonds broke and the polymer chains reorganise to achieve a stable state. This state in non-crystalline in the classical sense and irreversible. Thus, due to the thermal input, the polymer chains had gained enough mobility to optimise their inter and intramolecular interactions and to fulfil their entropic requirements.
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