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The synthesis and single crystal structure of Na 3/4 (NH 4 ) 1/4 ZnPO 4 , a new sodium-ammonium zinc phosphate, are reported. This phase adopts a previously unseen tetrahedral topology and is built up from a three-dimensional network of ZnO 4  [d av (Zn-O) = 1.952 (2) Å] and PO 4  [d av (P-O) = 1.538 (2) Å] units, fused together via Zn-O-P links [θav = 125.1 (1)°]. Extra-framework Na+ and NH 4  +  cations complete the crystal structure. The tetrahedral topology of this phase may be described as being built up from 63 hexagonal sheets containing two types (SSCSSC and SSSCSC) of six-rings arrayed normal to [100]. The crystal structures of related MZnPO 4  type phases (M = univalent cation) are reviewed. Crystal data: Na 3/4 (NH 4 ) 1/4 ZnPO 4 , Mr = 364.23, orthorhombic, space group Pbcn (No. 60), a = 8.251 (2) Å, b = 10.371 (3) Å, c = 17.430 (4) Å, V = 1491.4 (6) Å 3 , Z = 16, R = 2.71%, Rw = 2.56% [133 parameters, 1585 observed reflections with I &gt; 3σ(I)].

Na 3/4 (NH 4 ) 1/4 ZnPO 4 , a new framework zincophosphate. Survey of MZnPO 4 tetrahedral topologies