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The ammonothermal synthesis of three ammoniates of indium, namely InAlF6(NH3)2, [In(NH3)6][AlF6], and [In2F(NH3)10]2[SiF6]5 ∙ 2 NH3 was successful from near-ammononeutral conditions in the presence of fluoride ions. Initially, all these compounds were obtained upon corrosion of the applied liner and crucible material Si3N4, which also contains small amounts of aluminum. The syntheses were performed in supercritical ammonia (T = 753 K, p up to 307 MPa). The crystal structures were solved and refined from single crystal X-ray diffraction intensity data. InAlF6(NH3)2 crystallizes as a typical layer-type structure with corner-sharing [InF4(NH3)2]– and [AlF6]3− octahedra. [In(NH3)6][AlF6] features isolated [In(NH3)6]3+ and [AlF6]3− octahedra. The crystal structure of [In2F(NH3)10]2[SiF6]5 ∙ 2 NH3 contains [(NH3)5In–F–In(NH3)5]5+ octahedra doubles next to [SiF6]2− octahedra and ammonia molecules. All intermediates have strong hydrogen bonding systems. The results from vibrational spectroscopy are reported.

Indium Ammoniates from Ammonothermal Synthesis: InAlF6(NH3)2, [In(NH3)6][AlF6], and [In2F(NH3)10]2[SiF6]5 ∙ 2 NH3