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Red crystals of Na 4 TiSe 4  were obtained by reacting an intimate mixture of Na 2 Se, Ti and Se at 750°C. Na 4 TiSe 4  is monoclinic, space group I2/a with a = 24.027(6), b = 7.346(4), c = 21.572(6) Å, (β = 104.52(2)°, Z = 16. Its crystal structure was determined from diffractometer data (AgK α-radiation) and refined to a conventional R of 0.036 for 2673 F 0′ s and 158 variables. The crystal structure is of a new type, characterized by the presence of discrete tetrahedral complex anions, [TiSe 4 ] 4-  , which are arranged in slabs parallel to (100). The average Ti-Se bond length is 2.385(1) Å. The Na +  cations are in different chalcogen environments with distorted octahedral, square pyramidal or planar configurations, respectively

Preparation and Crystal Structure of Na 4 TiSe 4 . A Selenotitanate with Discrete Tetrahedral Anions