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The oxidation of the light lanthanides (M = La - Nd) with sulfur and NaN 3  in the presence of the tribromides MBr 3  yields bromine-poor nitride sulfide bromides with the composition M 6 N 3 S 4 Br when appropriate molar ratios of the reactants are used. Additional NaBr as a flux secures complete and fast reactions (7 d) at 850 °C in evacuated silica tubes as well as singlecrystals of the pure phase (brownish needles). The orthorhombic crystal structure (Pnma, Z = 4) was determined from single crystal X-ray data for La 6 N 3 S 4 Br (a = 1159.23(9), b = 410.85(3), c = 2765.6(2) pm), Ce 6 N 3 S 4 Br (a = 1152.31(9), b = 407.52(3), c = 2747.4(2) pm), Pr 6 N 3 S 4 Br (a = 1145.42(9), b = 404.21(3), c = 2729.3(2) pm), and Nd 6 N 3 S 4 Br (a = 1138.59(9), b = 400.94(3), c = 2711.3(2) pm). Six crystallographically different M 3+  cations are present, two of them (M1 and M2) build up chain I ( 1  ∝  {[NM2] 3+ }) by cis-edge connection of [NM 4 ] tetrahedra. The four remainders (M3 - M6) arrange as pairs [N 2 M 6 ] of edge-shared [NM 4 ] units which are further connected via four vertices to form a double chain (chain II =  1  ∝  {[N 2 M 4 ] 6+ }). Bundled along [010] like a closest packing of rods, both types of chains are commensurate in translation and held together by one Br -  and four S 2-  anions which, in contrast to an earlier work on the pseudo-isotypic chloride analogues M 6 N 3 S 4 Cl (M = La - Nd), are perfectly ordered.

zeitschrift für naturforschung b

Nitridsulfidhalogenide der leichten Lanthanide vom Typ M6N3S4X (M = La - Nd; X = Cl, Br) mit ausgeordneten Sulfid- und Halogenid-Lagen / Nitride Sulfide Halides of the Light Lanthanides with the Formula Type M6N3S4X (M = La - Nd; X = Cl, Br) with Ordered Sulfide and Halide Positions