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Phosphide-based materials have been investigated as promising candidates for solid electrolytes, among which the recently reported Li 9 AlP 4 displays an ionic conductivity of 3 mS cm -1 . While the phases Li-Al-P and Li-Ga-P have already been investigated, no ternary indium-based phosphide has been reported up to now. Here, we describe the synthesis and characterization of the first lithium phosphidoindate Li 3 InP 2 , which is easily accessible via ball milling of the elements and subsequent annealing. Li 3 InP 2 crystallizes in the tetragonal space group I 4 1 / acd with lattice parameters of a = 12.0007(2) and c = 23.917(5) Å, featuring a supertetrahedral polyanionic framework of interconnected InP 4 tetrahedra. All lithium atoms occupy tetrahedral voids with no partial occupation. Remarkably, Li 3 InP 2 is not isotypic to the previously reported homologues Li 3 AlP 2 and Li 3 GaP 2 , which both crystallize in the space group Cmce and feature 2D layers of connected tetrahedra but no supertetrahedral framework. DFT computations support the observed stability of Li 3 InP 2 . A detailed geometrical analysis leads to a more general insight into the structural factors governing lithium ion mobility in phosphide-based materials: in the non-ionic conducting Li 3 InP 2 the Li ions exclusively occupy tetrahedral voids in the distorted close packing of P atoms, whereas partially filled octahedral voids are present in the moderate ionic conductors Li 2 SiP 2 and Li 2 GeP 2 .

chemical science

Supertetrahedral polyanionic network in the first lithium phosphidoindate Li3InP2 – structural similarity to Li2SiP2 and Li2GeP2 and dissimilarity to Li3AlP2 and Li3GaP2