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In this work, we studied the structural features of La_1.9Ca_0.1NiO_4.11, which is considered a promising cathode material for intermediate temperature solid-oxide fuel cells (IT-SOFC). The effect of different pretreatments on the structural characteristics of the sample was studied using X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) in order to elucidate the origin of a peculiar change of lattice parameters observed earlier during in situ XRD studies. The XRD studies have shown that anisotropic broadening for reflections with a high Miller index <i>l</i> appears after tempering of a quenched (from 1100 °C) sample at 250 °C. This temperature is too low for the release/incorporation of oxygen into the structure but is sufficient for oxygen migration inside the structure. The HRTEM assisted us in revealing differences in the defect structure after different pretreatments. Based on obtained results, the following possible explanation was proposed. Observed additional microstrains and non-oriented planar defects as well as a decrease in the coherent scattering region size in the [00l] direction are caused by the non-homogeneous redistribution of interstitial oxygen in the structure during tempering.