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Ca5Co2N4, tetragonal, P4/ncc (no. 130), a = 8.0767(1) Å, c = 12.1401(2) Å, V = 791.9 Å, Z = 4, R(I) = 0.062, R(P) = 0.017, T = 295 K. Source of material Single phase black powder samples ofCa5[CoN2]2were obtained from the reaction of pellets ofCa3N2 (by reaction of calciummetal, Alfa, 99.9 % and nitrogen, Praxair, 99.999 % at 700 °C) and Co (Merck, 1 &m) in themolar ratio 2:1.The reactionwas carried out underN2 at ambient pressure inTa crucibles at 1150 °C for 100 h. Startingmaterials and products are sensitive tomoisture and air. Discussion Only few crystal structures of alkaline earth nitridocobaltates are known up to now: LiSr2[CoN2] [1], Sr39Co12N31 [2], and Ba[CoN] [3]. Predominant structural features of these compounds are isolated dumbbells [CoN2] and chains [CoN], respectively. The crystal structure of Ca5[CoN2]2 is isotypic to BaCa4[CuN2]2 [4] and BaCa4[CoN2]2 [5] and contains near-linear [CoN2] anions (d(Co—N) = 1.821(4)Å,/N–Co–N= 178.1(2)°).Charge compensation is accomplished by Ca. The isolated [CoN2] ions are arranged in layers running parallel (001). The dumbbells are tilted from [001] by 15.85(7)°. The calcium-nitrogen substructure is made up by double layers of edge-sharingN-centered Ca5 tetragonal pyramids running parallel (001). These layers are linked via common cobalt atoms along [001], thereby completing the octahedral coordination of N (Ca5Co). Both Ca1 and Ca2 sites (d(Ca—Co) = 2.400(3)Å – 2.646(3)Å, average 2.55Å) are fourfold coordinated by N. The interatomic distances are in good agreement with respective values in related compounds (d(Co—N): 1.810 Å [1], 1.813 Å [2], 1.816 Å [3]; d(Ca—N): 2.460 Å [4], 2.488 Å [5], 2.503 Å (Ca2[FeN2], [6]), 2.505 Å (Ca[NiN], [7])). In 1993X-ray powder pattern and lattice parameters of an alleged compound -Ca3CoN3were presented [8]. It should be emphasized that the publishedX-ray powder pattern of -Ca3CoN3fits well to the pattern of Ca5[CoN2]2 by assigning the remaining peaks in the pattern to CaO [9]. Z. Kristallogr. NCS 222 (2007) 165-166 / DOI 10.1524/ncrs.2007.0068 165 © by OldenbourgWissenschaftsverlag,München Powder: black, size 5 – 20 &m Wavelength: Co K20 radiation (1.78897 Å) &: 73.5 cm−1 Diffractometer: Stoe STADI P 2'max, stepwidth: 84.915, 0.005° N(points)measured: 16384 N(hkl)measured: 98 N(param)refined: 27 Programs: FULLPROF [10], DIAMOND [11], STRUCTURE TIDY [12] Table 1. Data collection and handling.

Crystal structure of pentacalcium bis(dinitridocobaltate(I)), Ca 5 [CoN 2 ] 2 , and a note on “Ca 3 CoN 3 “