Man erhält (NH4)2[Nb3O5Cl7] in kristalliner Form in Quarzglasampullen aus NbCl5, NH4Cl und As2O3 bei 1050 K. Die Kristalle sind farblos manchmal blaßblau. (NH4)2[Nb3O5Cl7] kristallisiert bei 293 K monoklin in der Raumgruppe C2/c mit Z = 4 und den Gitterkonstanten a = 1680,6(8) pm, b = 886,6(1) pm, c = 1104,3(5) pm und β = 111,35(2)° Die Struktur besteht aus [(Nb3O5Cl7)2−] ∞2‐Schichten in denen die Oktaederbasisflächen über Ecken verknüpft sind. Die Struktur des Polyanions zeigt eine neuartige Oktaederverknüpfung für eine MX4‐Schichtstruktur. Zwischen diesen Schichten befinden sich die Ammoniumionen.
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