Crystals of Na5Cu 3 (P0 4 ) 2 (P04HP04) were synthesized under hydrothermal conditions. The crystal structure was solved by Patterson methods and was refined to R w = 0.045 (a = 5.106(2) Ä, b = 8.409(3) Ä, t· = 9.052(3) Ä, α = 115.76(3)°, β = 90.09(3)°, y = 106.01(3)°, space group Pi, Ζ = 1). The two crystallographically different Cu atoms display "square planar" coordination; one of them has a fifth Ο atom neighbour with Cu -Ο at 2.183 Ä. Two of the four phosphate groups per formula unit are connected by an extreme short (symmetry restricted) hydrogen bond with O. . .O at 2.388 Ä.
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