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ClN3Pr6S4, orthorhombic, Pnma (No. 62), a = 11.3987(8) Â, b = 4.0235(3) k,c = 26.999(1) À, V= 1238.3 Â 3 ,Z = 4, Rè{F) = 0.037, RUF) = 0.079, T= 293 Κ. Source of material Pr6N3S4Cl was prepared from PrCb, praseodymium powder, sulfur, and sodium azide (NaN3) as nitrogen source (molar ratio 2:16:12:3) with small amounts of NaCl or a slight excess of PrCb as fluxing agents [1, 2], The mixture was heated in a sealed evacuated silica vessel at 1123 Κ (7 d) and subsequently cooled down (25 K/d) at ambient temperature. Discussion Pr6N3S4Cl belongs to the Nd&N3S4Cl-typc of structure [1], The orthorhombic unit cell contains two different types of chains built 3— "*3+ up by edgeand vertex-sharing Ν -centred (Pr )4 tetrahedra ~[(Nl)(Prl)3/3(Pr2)i/i] and ~[(Pr5)2/2(N2XPr3)(i+i)/(i+i)(Pr4)(1+i)/(i+i)(N3)(Pr6)2/2], both commensurate in translation along [010], which are depicted in the figure (Pr: black, N: small, S and CI: large circles) by closed polyhedra [3-7]. Table 1. Data collection and handling. Crystal: reddish brown, transparent, lath-shaped needles, size 0.03 χ 0.08 χ 0.15 mm Wavelength: Mo Ka radiation (0.7107 Â) μ: 239.9 cm"' Diffractometer, scan mode: Siemens-Stoe, profile fitted ω-20-scan [11] 29max64.4° N(hkl)measured, N(hkl)u„ique: 4648, 2350 Criterion for Fobs, N(hkl)¡t: Fobs > 3 o(F0bs), 1665 N(param) refined: 86 Programs: SHELXS-86 [8], SHELXL-93 [9], DIAMOND [10] Table 2. Atomic coordinates and displacement parameters (in À). Atom Site X y ζ Un Un ί/33 Un ί/13 Un Pr(l) 4c 0.40104(5) 1/4 0.46236(2) 0.0116(2) 0.0132(3) 0.0138(2) 0 -0.0012(2) 0 Pr(2) 4c 0.24374(6) 1/4 0.06443(2) 0.0138(3) 0.0140(3) 0.0158(2) 0 -0.0023(2) 0 Pr(3) Ac 0.43801(5) 1/4 0.19285(2) 0.0124(3) 0.0146(3) 0.0151(2) 0 -0.0008(2) 0 Pr(4) Ac 0.24533(6) 1/4 0.32661(2) 0.0130(3) 0.0134(3) 0.0138(2) 0 -0.0004(2) 0 Pr(5) Ac 0.44107(6) 1/4 0.92262(2) 0.0126(3) 0.0181(4) 0.0158(2) 0 -0.0010(2) 0 Pr(6) Ac 0.38142(6) 1/4 0.71331(2) 0.0135(3) 0.0142(3) 0.0149(2) 0 -0.0012(2) 0 N(l) Ac 0.0980(8) 1/4 0.0133(3) 0.009(4) 0.017(5) 0.012(3) 0 0.000(3) 0 N(2) Ac 0.0621(9) 1/4 0.3747(3) 0.020(5) 0.004(4) 0.017(4) 0 -0.004(3) 0 N(3) Ac 0.1111(9) 1/4 0.2606(3) 0.018(5) 0.016(5) 0.016(4) 0 -0.004(3) 0 S(l) Ac 0.2041(3) 1/4 0.89640(9) 0.014(1) 0.013(1) 0.016(1) 0 0.0017(9) 0 Bereitgestellt von | Technische Informationsbibliothek Hannover Angemeldet Heruntergeladen am | 06.11.18 12:36 24 Hexapraseodymium(III) trinitride tetrasulfide chloride T a b l e 2 . Continued. Atom Site χ y Ζ Un U22 UÌÌ Un t/13 UÎÎ S(2) Ac 0.0431(3) 1/4 0.13630(9) 0.015(1) 0.022(2) 0.016(1) 0 -0 .0018(9) 0 S(3) 4c 0.1449(3) 1/4 0.50411(9) 0.013(1) 0.018(2) 0.019(1) 0 0.0001(9) 0 S(4) 4c 0.1900(3) 1/4 0.63676(9) 0.016(1) 0.017(2) 0.014(1) 0 0.0035(9) 0 CI 4c 0.1374(3) 1/4 0.76448(9) 0.017(1) 0.018(1) 0.017(1) 0 -0 .0007(9) 0

Crystal structure of hexapraseodymium(III) trinitride tetrasulfide chloride, Pr 6 N 3 S 4 Cl