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Na 3 B 2 PO 5 F 4  has been synthesized by an allsolid- state reaction between Na 3 PO 4  and NaBF 4  and, alternatively by solid-gas reaction between Na 3 PO 4  and BF 3 . The new fluoridoboratophosphate is dimorphic. Monoclinic Na 3 B 2 PO 5 F 4 -II (P2 1 /n, a = 6.5230(6), b = 12.174(1), c = 8.8279(8) Å, β= 102.322(5)º) and orthorhombic Na 3 B 2 PO 5 F 4 -II (Cmcm, a = 12.175(2), b = 6.719(1), c = 9.077(1) Å) were obtained at 623 and 673 K, respectively. The latter is a dynamically or statically disordered polymorph of the former. Both modifications contain a cyclic six membered anion build up by three interconnected tetrahedra, i.e. one PO 4  and two BF 2 O 2  units. These complex cyclo-anions feature the same number of valence electrons as cyclo-triphosphate [P 3 O 9 ] 3-  and fluoridooxidoborate [B 3 O 3 F 6 ] 3- .

Novel Fluorido-Oxoanions via Lewis Acid-Base Reactions – Synthesis and Crystal Structure Determination of Na 3 B 2 PO 5 F 4