International. This e-offprint isLattice deformation and extended defects such as grain boundaries and dislocations affect the crystalline quality of films and can dramatically change material's properties. In particular, magnetic and optoelectronic properties depend strongly on these structural and substructural characteristics. In this paper, a combined methodology based on SEM, HRTEM, XRD, and HRXRD measurements is used to determine and assess the structural and substructural characteristics of films. This combined methodology has been applied to Zn 1Àx Mn x Te films grown on glass substrates by close-spaced vacuum sublimation. Nevertheless the methodology can be applied to a wide variety of materials and could become a useful characterization method which would be particularly valuable in semiconductor growth field. The knowledge of the structural and substructural characteristics can allow not only the optimization of growth parameters, but also the selection of specific samples having the desired characteristics (crystallite size, minimum dislocation content, etc.) for high-quality technological devices.