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Lustrous needle shaped prismatic single crystals of the new compound Ca 10 V 5.2 Fe 0.8 O 24  were obtained out of a sample with nominal composition Ca 2 Fe 1.6 V 0.4 O 5  prepared at 1400 °C. The crystals are opaque and stable to humid air. Ca 10 V 5.2 Fe 0.8 O 24  crystallizes with a new structure type, space group Pnma with a = 6.803(3), b = 16.015(8), c = 10.418(7)Å , Z = 2, R = 0.041. The crystal structure is characterized by two mononuclear tetrahedral species, MO 4 , which differ significantly from each other with respect to their M-O bond lengths. One with an average bond distance of 1.709(8)Å represents an orthovanadate ion. The other with a significantly larger value d(M-O) = 1.744(6) Å corresponds to a mixed occupation of its centre according to [V 0.8 Fe 0.2 O 4 ] 3.5− . In the crystal structure the complex anions are arranged in separate sheets parallel to the (010) plane. They are separated from each other by three crystallographically independent Ca 2+  ions which are each coordinated by 7 oxygen atoms in distorted pentagonal bipyramidal and trigonal prismatic configurations, respectively.

Ca 10 V 5.2 Fe 0.8 O 24 , a Novel Oxometalate with Discrete Complex Anions