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GeNi5.45Se2, tetragonal, I4/mmm (no. 139), a = 3.6117(4) Å, c = 18.281(3) Å, V = 238.5 Å, Z = 2, Rgt(F) = 0.051, wRref(F) = 0.078, T = 293 K. GeNi5.45Te2, tetragonal, I4/mmm (no. 139), a = 3.6858(3) Å, c = 19.072(3) Å, V = 259.1 Å, Z = 2, Rgt(F) = 0.043, wRref(F) = 0.082, T = 293 K. Source of material Ni5.45GeSe2 andNi5.45GeTe2were prepared in a solid-state reaction starting froman intimatemixture of pure elements, in themolar ratio 5:1:2 and iodine as a transport agent, which was filled into a dry quartz glass ampule (l = 20 cm,. = 1.8 cm) evacuated and sealed.The ampule was placedwith one end in the center of a tube furnace at 1073 K for 5 days. The educt consists of black square-shaped crystals which form preferably at the cold end of the ampule at an estimated temperature of 873K.Ni5.45GeSe2 and Ni5.45GeTe2 can be handled in air. Discussion In the course of attempts to synthesize new mixed-valence compounds with transition metals, several new solids were prepared [1]. Fe5GeTe2 [2] whichwas recently investigated in our research group, is another air-stable, black-metallic solid, whose crystals show significant flexibility and a pronounced hexagonal morphology. In contrast to Fe5GeTe2 the two title compounds Ni5.45GeQ2 (Q = Se, Te) show tetragonal prismatic morphology. The Ni5.45GeQ2 family (Q = Se, Te) is closely related to another group of phases which consists of Ni5.72SbSe2, Ni5.66SbTe2 [3], Ni5.98SnS2, Ni8.93Sn2S2 [4], Ni5.62SnSe2, Ni5.78SnTe2 [5] and Pd6.21SnTe2 [6]. In the crystal structure of the title compounds there are three crystallographically independent Ni sites. Ni3 is only partially occupied forNi5GeTe2 (s.o.f.(Ni3) = 0.22(1)).A similar situation also exists in theSn andSb analogues inwhichNi3 has an s.o.f. of 0.309(7) and 0.36(2), respectively. All Ni—Ni distances are found to be slightly longer than those inNi metal (2.49Å) [7].As one can see from the figure the structure is built of layer packages, which alternate perpendicular to [001]. Each layer package consists of five alternating layers (1.: Ni/Se, 2.: Ni, 3.: Ni/Ge, 4.: Ni, 5.: Ni/Se). The layers are repeated in a staggered fashion. Although for Ni5.78SnTe2 [8] a modulated crystal structure was reported, our X-ray single crystal structure investigations did not show satellite reflections. Z. Kristallogr. NCS 222 (2007) 171-172 / DOI 10.1524/ncrs.2007.0071 171 © by OldenbourgWissenschaftsverlag,München

Crystal structures of nickel germanium selenide, Ni 5.45 GeSe 2 , and nickel germanium telluride, Ni 5.45 GeTe 2