Structure D 2000 Crystal Structure of Potassium Samarium Octacyanomolybdate(IV) Decahydrate. -Orange single crystals of the title compound are prepared by reaction of K2CO3 and Sm2(CO3)3 in 0.1M H4[Mo(CN)8]·2H2O in the dark (room temp., several months). KSm[Mo(CN)8]·10H2O crystallizes in the orthorhombic space group Pbcm with Z = 4. The structure contains [SmN4(H2O)5] 3+ and [Mo(CN)8] 4units, K + cations, and additional water molecules. -(TYPILO, I.; SEREDA, O.; SEMENYSHYN*, D.; STOECKLI-EVANS, H.; GLADYSHEVSKII, R.; Pol. J. Chem. 83 (2009) 2, 339-344; Inst. Chem. Chem. Eng., Lviv Polytech. Natl. Univ., Lviv 79013, Ukraine; Eng.) -Schramke 18-009
A review of the crystal structures of octacyanomolybdates(IV) and octacyanotungstates(IV) of {[K(H 2 O)][Ln(H 2 O) 4 ][M(CN) 8 ]·2H 2 O} n ( M 4+ = Mo and Ln 3 + = Y, La, Sm, Gd, Yb, M 4+ = W and Ln 3+ = Tb, Dy, Ho, Er, Lu) composition has been done. These compounds have 3D-structures and contain infinite chains -C≡N-M-N≡C-Ln-, which extend in three dimensions, unlike CeH 3 O[W(CN) 8 ]·6H 2 O, which has 2D-structure. The coordination polyhedra [ M (CN) 8 ] 4-(M 4+ = Mo, W) is different (dodecahedron, square antiprism, bicapped trigonal prism), depending on the nature of the rare-earth elements. The composition and form of the coordination polyhedra of the atoms of rareearth elements (square antiprism, monocapped tetragonal antiprism, tricapped trigonal prism) are also different. All complexes are polymeric compounds and differ in structure from octacyanometallates(IV) d-elements and octacyanometallates(V) f-elements.
X-ray diffraction on single crystal was used to refine the crystal structure of K 4 [Mo(CN) 8 ]⋅ ⋅ ⋅ ⋅2H 2 O. For the first time the positions of all hydrogen atoms in the complex were localized, the crystal structure being determined at temperature 173 K. The compound crystallizes in the orthorhombic system, space group Pnma, cell parameters a = 16.6959(10), b = 11.6090(6) and c = 8.6796(6) Å, V = 1682.30(18) Å 3 , Z = 4, D X = 1.961 g•cm-3 , number of independent reflections 2365, reliability factors R = 0.0329, wR = 0.0590. The coordination polyhedron of the molybdenum atoms is a dodecahedron [Mo(CN) 8 ]. The potassium atoms have three different deformed polyhedra: trigonal bipyramid [K1N 4 OH 2 ], tetragonal pyramid [K2N 5 ] and trigonal prism with one additional atom [K3N 5 (OH 2) 2 ]. All cyanogroups in the complex are terminal.
The crystal structure of distrontium octacyanotungstate decahydrate, Sr 2 [W(CN) 8 ]·10H 2 O, was solved using X-ray single crystal diffraction. The tungsten atom lies on a two fold axis. Eight cyanide anions create tetragonal antiprismatic coordination sphere of tungsten atom. The two edge-sharing tetragonal antiprisms of [Sr(NC) 3 (OH 2 ) 5 ], create a dimer, [Sr 2 (CN) 6 (H 2 O) 6 (μ-H 2 O) 2 ], which lies on the inversion * Dr. M. Daszkiewicz Fax: +71-34-410-29 E-Mail: m.daszkiewicz@int.pan.wroc.pl [a] W.
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