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Single crystals of the mixed valency phase Zn 2 (Zn 1-x Fe x )Fe III (PO 4 ) 3  · 2 H 2 O were grown by hydrothermal treatment of phosphophyllite (Zn 2 Fe(PO 4 ) 2  · 4 H 2 O) at 160 °C in 1 M H 3 PO 4 . The crystal structure (tricl., P 1̅; a = 641.5(4) pm, b = 914.4(4) pm, c = 983.4(4) pm, α = 70.79(5)°, β = 78.32(5)°, γ = 73.69(5)°; Ζ = 2) contains PO 4  tetrahedra, connected via vertices shared with coordination polyhedra of the metal ions. Cation coordination polyhedra (Fe III (O p ) 5 O w  octahedra, (Zn 1  -x Fe x )(O p ) 5 O w  octahedra and Zn(O p ) 5  trigonal bipyramids) are connected to centrosymmetrical six-membered chains by sharing common Op-edges. These short chains are interconnected by common vertices of Zn(O p ) 4  tetrahedra to form infinitive ribbons of cation coordination polyhedra. The x-values observed for the substitutional position (Zn 1  -x Fe x ) varied from x = 0.5 (single crystal determination) to x = 1 (Mössbauer investigation). The Mössbauer parameters are consistent with high-spin iron in a slightly distorted octahedral environment and valence states (II) and (III).

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Zn 2 (Zn 1-x Fe x )Fe III (PO 4 ) 3  · 2 H 2 O: Darstellung, Kristallstruktur und Mößbauer-Untersuchung / Zn 2 (Zn 1-x Fe x )Fe III (PO 4 ) 3  · 2 H 2 O: Preparation, Crystal Structure and Mössbauer Investigation