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Cr 7 (PO 4 ) 6  [Cr 3  2+  Cr 4  3+ (PO 4 ) 6 ] can be obtained reducing a mixture of Cr 2 O 3  and CrPO 4  by CrP (950°C, 48h, 100 mg iodine as mineralizer). By means of chemical transport reactions (transport agent iodine; 1050 → 950°C) the compound has been separated from its neighbour phases and crystallized (dark brown, transparent crystals; pinacoidal, edge length up to 0.5 mm). Cr 7 (PO 4 ) 6  [ P  [unk];  Z  = 1;  a  = 9.3184(19) Å,  b  = 8.0044(18) Å,  c  = 6.2532(14) Å,  α  = 100.982(9)°,  β  = 107.954(11)°,  γ  = 107.144(10)°] is isotypic to Fe 7 (PO 4 ) 6 . The crystal structure refinement from single single crystal data led to a conventional residual  R  = 0.032 (3016 independent  F  0 , 170 parameters). For M = Cr 2+  two different M–O-coordination polyhedra were observed; a  compressed  octahedron and a strongly distorted trigonal bipyramide. The influence of the Jahn-Teller effect on the coordination geometry of Cr 2+  will be discussed. The Cr 3+  ions (2 sites) are surrounded octahedrally by oxygen (1,884 Å ≤  d  Cr–O  ≤ 2,071 Å). Zn 3 Cr 4 (PO 4 ) 6  also isotypic to Fe 7 (PO 4 ) 6  has been synthesized and characterized by its Guinier powder pattern [ a  = 9.248(4) Å,  b  = 7.835(3) Å,  c  = 6.277(2) Å,  α  = 101.59(4)°,  β  = 108.10(3)°,  γ  = 105.34(4)°].

zeitschrift für kristallographie - crystalline materials

Beiträge zum thermischen Verhalten wasserfreier Phosphate VIII.* Darstellung und Kristallstruktur von Cr 7 (PO 4 ) 6 . Das erste gemischtvalente Phosphat mit Cr(II) und Cr(III)