The structure of a La 2 CuO 4+ y single crystal with the excess oxygen content y =0.03 has been studied by means of neutron diffraction at T =13 K. Although the extra oxygen content of y =0.03 is inside the miscibility gap of La 2 CuO 4+ y (0.01 y Cmca symmetry. It was confirmed that the extra oxygen, O4, is located close to the site (1/4, 1/4, 1/4). The structural parameters for all atoms lay between those previously determined for the oxygen-poor and oxygen-rich phases representing the edges of the miscibility gap, y =0.01 and 0.06, respectively. Our data allow us to conclude that (1) the phase-separated and non-phase-separated La 2 CuO 4+ y compounds are structurally identical, and (2) the crystal structure of La 2 CuO 4+ y changes monotonically when the extra oxygen content changes from 0 to 0.05.
