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Abstract

Se 7 (III) wurden durch Hydrothermalsynthese aus den Elementen unter Verwendung eines Amins hergestellt. I kristallisiert in der monoklinen Raumgruppe P2 1 /n (a = 1262,9(3) pm, b = 1851,3(4) pm, c = 2305,2(4) pm, b = 104,13(3)°und Z = 4). Das [Sn 2 Se 6 ] 4± -Anion besteht aus zwei u È ber eine Kante verknu È pften Tetraedern. II kristallisiert in der orthorhombischen Raumgruppe Pna2 1 (a = 2080,3(4) pm, b = 1308,2(3) pm, c = 2263,5(5) pm und Z = 4). Das Anion ist aus vier SnSe 4 -Tetraedern aufgebaut, die u È ber Ecken zu einem adamantanartigen [Sn 4 Se 10 ] 4± -Geru È st verknu È pft sind. III kristallisiert in der orthorhombischen Raumgruppe Pbcn (a = 1371,1(3) pm, b = 2285,4(5) pm, c = 2194,7(4) pm und Z = 8). Das Anion ist aus [Sn 3 Se 5 Se 4/2 ] 2± Blo È cken aufgebaut: Zwei u È ber eine Ecke verknu È pfte Tetraeder sind u È ber eine Kante des einen und u È ber eine Ecke des anderen mit einer trigonalen Bipyramide verbunden. Diese Einheiten sind u È ber Kanten der trigonalen Bipyramide zu Ketten verknu È pft. Die Ergebnisse von TG/DSC-Messungen und temperaturabha È ngige Diffraktometeraufnahmen zeigen, daû I und II zuna È chst unter Abgabe geringer Mengen von Triethylammonium in eine Schichtstruktur mit gro È ûeren Zelldimensionen u È bergehen. Danach bildet sich unter Abgabe von restlichen Triethylammonium und H 2 Se, SnSe 2 und Se. SnSe 2 wird bei noch ho È heren Temperaturen teilweise in SnSe u È berfu È hrt. Bei III konnte die komplexe Zwischenstufe nicht erfaût werden, es bildet sich direkt SnSe 2 . About Selenidostannates. I Synthesis, Structure, and Properties of [Sn 2 Se 6 ] 4± , [Sn 4 Se 10 ] 4± , and [Sn 3 Se 7 ] 2± Abstract. The selenidostannates [(C 4 H 9 ) 2 NH 2 ] 4 Sn 2 Se 6´H2 O (I), [(C 4 H 9 ) 2 NH 2 ] 4 Sn 4 Se 10´2 H 2 O (II) und [(C 3 H 7 ) 3 NH] 2 -Sn 3 Se 7 (III) were prepared by hydrothermal syntheses from the elements and the amines. I crystallizes in the monoclinic spacegroup P2 1 /n (a = 1262.9(3) pm, b = 1851.3(4) pm, c = 2305.2(4) pm, b = 104.13(3)°and Z = 4). The [Sn 2 Se 6 ] 4± anion consists of two edge-sharing tetrahedra. II crystallizes in the orthorhombic spacegroup Pna2 1 (a = 2080.3(4) pm, b = 1308.2(3) pm, c = 2263.5(5) pm and Z = 4). The anion is formed from four SnSe 4 tetrahedra which are joined by common corners to the adamantane cage [Sn 4 Se 10 ] 4± . III crystallizes in the orthorhombic spacegroup Pbcn (a = 1371.1(3) pm, b = 2285.4(5) pm, c = 2194.7(4) pm and Z = 8). The anion is a chain, built from edge-sharing [Sn 3 Se 5 Se 4/2 ] 2± units, in which two corner sharing tetrahedra are connected to a trigonal bipyramid by an edge of one and a corner of the other tetrahedron.The results of the TG/DSC measurements and of temperature dependent X-ray diffractograms reveal that I and II decompose at first by release of minor quantities of triethylammonium to compounds with layer structure and larger cell dimensions. At still higher temperature the rest of triethylammonium and H 2 Se is evolved, leaving SnSe 2 and Se in the bulk. The former decomposes partially at the h...

Solvothermal Synthesis and Characterization of Lanthanide Chalcogenidostannates [Ln2(en)6(μ2‐OH)2][Sn2S6] (Ln = Dy, Er) and [Dy2(en)6(μ2‐OH)2][Sn2Se6]

“…The structure of the coordination polyhedron LnN 6 O 2 can be described as a distorted bicapped trigonal prism. The OϪLnϪN and NϪLnϪN angles in 1 range from 73.73(9) to 152.90(9)°, and from 66.20 (10) (4)Ϫ2.570(4) Å for ErϪN, and are similar to those in other dysprosium(III) and erbium(III) complexes with amino ligands, respectively [17,18]. The LnϪO and LnϪN lengths decrease from Dy to Er, as expected from the lanthanide contraction.…”

“…Similar mild solvothermal method was employed by Bensch et al [8] to prepare compounds [Ni(dap) 3 [11]. The cations of these chalcogenidostannate compounds can be classified as alkali ions [1,9], organic ammonium ions [3Ϫ5, 10,11]…”

Solvothermal synthesis and characterization of tris(ethylenediamine)nickel(II) hexaselenodistannate(IV)

“…Low-temperature solvo(hydro)thermal reactions have produced a limited number of selenostannates (Loose & Sheldrick, 2001). Among these selenostannates, the counterions to the [Sn x Se y ] nÀ anions can be classified as metal cations (Zimmermann & Dehnen, 1999), organic amine cations (Fehlker & Blachnik, 2001) and transition metal complex cations. The study of selenostannates combining with transition metal complex cations as counter-ions is still a fairly unexplored area.…”

Varied forms of lamellar [Sn3Se7]n2n−anion: the competitive and synergistic structure-directing effects of metal–amine complex and imidazolium cations

“…31,41,52 By using these binary aggregates as secondary building units (SBUs), many chalcogenidostannates with varied structural dimensionalities have been obtained. Among these, it is interesting that [Sn 3 Q 10 ] units as SBUs can interlink with each other via sharing two μ 2 -Q bridging atoms, resulting in distinct structures of [Sn 3 Q 7 ] n 2n− ranging from single-chain, 40,47,53 double-chain, 47,48 and layer 11,36,40,42,43,45,[47][48][49]51 to coexisting single-chain and layer.…”