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New paracelsian-like beryllophosphates M4LiBe4P7O24 and their tetrahedra-substituted phases M4Li(Li3P)P7O24 (MLiP2O6, M = Cs, Rb) were designed and synthesized. Interestingly, two types of phases undergo a structural transformation, resulting from the radius and valence charge number of tetrahedral cations. Four crystals demonstrate potential deep-UV NLO properties such as short absorption edges (<190 nm) and phase-matching SHG response.

Graphical abstract: M4LiBe4P7O24 and M4Li(Li3P)P7O24 (M = Cs, Rb): deep-ultraviolet nonlinear-optical phosphates with a tetrahedra-substituted paracelsian-like framework

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