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Structures of partially and completely protonated Ruddlesden–Popper phases, H0.7Na0.3NdTiO4·0.3H2O and HNdTiO4, have been established by means of neutron and X-ray diffraction analysis and compared among themselves as well as with that of the initial titanate NaNdTiO4. It was shown that while interlayer sodium cations in the partially protonated form are coordinated by nine oxygen atoms, including one related to intercalated water, in the fully protonated compound the ninth oxygen proves to be an axial anion belonging to the opposite slab of titanium-oxygen octahedra. Moreover, the partially protonated titanate was found to significantly differ from the other two in the octahedron distortion pattern. It is characterized by a weakly pronounced elongation of the octahedra towards the Nd-containing interlayer space making Ti4+ cations practically equidistant from both axial oxygen atoms, which is accompanied by a low-frequency shift of the bands relating to the asymmetric stretching mode of axial Ti–O bonds observed in the Raman spectra.

Protonated Forms of Layered Perovskite-Like Titanate NaNdTiO4: Neutron and X-ray Diffraction Structural Analysis