Contributions on thermal behaviour and crystal chemistry of anhydrous phosphates. XXXXIII [1] – Rhenium(VI) Oxidephosphate: Chemical Vapour Transport, Crystal Structure, Spectroscopic Characterisation and Magnetic Behaviour [2]

Re 2 O 3 (PO 4 ) 2 was obtained as microcrystalline, dark‐red powder at 450 °C by reaction of ReO 3 with P 4 O 10 . Crystallisation was achieved through chemical vapour transport in a temperature gradient 600 → 500 °C using iodine as transport agent. Re 2 O 3 (PO 4 ) 2 ( Pmcn , Z = 4, a = 6.2986(6) Å, b = 7.79654(5) Å, c = 15.2714(12) Å], 86 parameters, 1185 independent reflections, R 1 = 0.027, wR 2 = 0.066) adopts its own structure type. The crystal structure consists of isolated double‐octahedra [Re VI 2 O 11 ] and [PO 4 ] tetrahedra. Re 2 O 3 (PO 4 ) 2 shows a weak temperature dependent magnetic moment (0.05 ≤ μ exp / μ B ≤ 0.27; 3 K ≤ T ≤ 300 K). Its single‐crystal electronic absorption spectrum exhibits a weak band around $\tilde{\nu}$ =ν = 12000 cm –1 , above $\tilde{\nu}$ =ν = 16000 cm –1 the UV/Vis spectrum is completely dark.