Die Kristallstruktur von H3Co(CN)6

The crystal structure of the hexagonal H₃Co(CN)₆ (a = 6.43 Å, c = 5.70 Å, Z = 1) has been determined by X-ray powder methods. The space group is D (at least pseudo), the cobalt atoms being in (0, 0, 0). Structure factor calculations lead to a final R-value of 13.2%, based on F²-sums of coinciding reflections. The carbon and nitrogen atoms are located at the vertices of a slightly distorted octahedron around the cobalt atom; the angle Co? C? N is 177°. The interatomic distances are: Co? C = 1.89 Å, Co? N = 2,98 Å, C? N = 1.09 Å. The pseudo-octahedral units of Co(CN)₆ are linked together by N? H? N bridges. Infrared spectra show that the most probable linkage is the one with a N? H? N-bond length of 2.7 Å.     

Zur Struktur von H3Co(CN)6 und Ag3Co(CN)6

The X-ray powder patterns of H₃Co(CN)₆ and Ag₃Co(CN)₆ have been indexed on the basis of a hexagonal unit cell: The length of the N? X? N-bond along the c-axis is 3.29 Å for X ? H and 4.24 Å for X ? Ag. These distances are in agreement with data obtained from infrared spectra and with structural properties of similar compounds.     

Die Struktur der Hydrate von Co3[Co(CN)6]2 und Cd3[Co(CN)6]2

The crystal structures of Co₃[Co(CN)₆]₂, 12 H₂O (a, = 10.210 ± 0.005 Å) and Cd₃[Co(CN)₆]₂, 12 H₂O (a = 10.590 ± 0.005 Å) have been determined by X-ray powder methods. According to the measured density the unit cell contains 1 1/3 formula units with 4 Co²⁺ (Cd²⁺) in 4a, 2 2/3 Co³⁺ in 4b, 16 C and 16 N in 24e, 8 H₂O_I near 24e, (96k) and 8 H₂O_II near 8 _c (192 l). Structure factor calculations based on the space group O_h⁵ - F m 3 m lead to the following final values of the reliability index R: 0.038 (Co₃[Co(CN)₆]₂, 12 H₂O) and 0.037 (Cd₃[Co(CN)₆]₂, 12 H₂O). The interatomic distances for the cobaltous compound (in parentheses for the cadmium compound) are: Co³⁺-C: 1.88 Å (1.89); C-N: 1.15 Å (1.17); Co²⁺-N: 2.08 Å (2.24); Co²⁺-O_I: 2.10 Å (2.27); shortest O_I-H-O_II-bonds: 2.89 Å (2.82). Co³⁺ is octahedrally coordinated by six carbon atoms, the divalent metal ion by four nitrogen atoms and two water molecules. The two different metal ions are connected by M²⁺-N-C-Co³-bonds to a threedimensional network. The infrared and electronic spectra are shown to be in agreement with the results of the structure analyses of these compounds. The observed positions of the OH-stretching vibrations lead to a hydrogenbond-length of 2.8–2.95 Å.     

Kristallstruktur von Tl4Fe(CN)6

Crystal Structure of Tl₄Fe(CN)₆ Single crystals of Tl₄Fe(CN)₆ have been prepared for the first time and its crystal structure was determined. The pale yellow compound crystallizes in the triclinic space group P1 (No. 2) with the lattice parameters a = 726.6(1) pm, b = 797.4(8) pm, c = 1 336.0(1) pm, α = 104.7(9)°, β = 90.0(8)°, γ = 97.6(7)°, Z = 2 in a new structure type.     

Die Kristallstruktur der Tieftemperaturmodifikation von Ag8GeS6

The low temperature form of Ag₈GeS₆ (synthetic argyrodite) is orthorhombic, space group Pna2₁, witha=15.149 (1),b=7.476 (2),c=10.589 (1), andZ=4. The crystal structure has been determined from 2-circle diffractometer data by means of direct methods and refined toR=0.081 for 3431 intensities. The structure consists of slightly distorted isolated GeS₄ tetrahedra (mean Ge–S bond length 2.212 Å) and two further sulphur atoms without bonds to the germanium atoms. The GeS₄ tetrahedra and the S atoms are connected by the Ag atoms to form a three-dimensional framework. Three types of Ag coordination by S atoms are encountered. Three Ag positions have a strongly distorted tetrahedral environment, four Ag positions an approximately planar threefold coordination, while one Ag atom is almost linearly coordinated by two S atoms. The Ag–S distances are 2.56–2.94 Å, 2.49–2.76 Å, and 2.42–2.44 Å, resp. All Ag atoms have at least one near Ag neighbour between 2.93 and 3.11 Å.

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Mit 3 Abbildungen     

Die Kristallstruktur von Ag2TeO2(OH)4

Zusammenfassung Die Kristallstruktur von Ag₂TeO₂(OH)₄ wurde mit Hilfe von Einkristallmethoden bestimmt und nach der Methode der kleinsten Quadrate verfeinert. Die Gitterparameter der Elementarzelle (Fdd 2–C _2v ¹⁹ ) betragen:a=18,72;b=6,48;c=8,94 Å. Mit allen beobachteten Reflexen wurde einR-Wert von 8,50%, unter Einschluß derHamilton-Reflexe einR-Wert von 9,41% erhalten. Die Telluratome sind oktaedrisch von 6 Sauerstoffen umgeben, während die Silberatome stark verzerrt tetraedrisch von 4 Sauerstoffen umgeben sind. Zwei dieser Tetraeder bilden mit einem dazwischenliegenden Oktaeder eine geometrische Einheit. Diese Einheiten sind über Sauerstoffe, die zu zwei verschiedenen Tetraedern gehören, und über Wasserstoffbrücken zu einem dreidimensionalen Gerüst verknüpft.

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The crystal structure of Ag₂TeO₂(OH)₄

The crystal structure of Ag₂TeO₂(OH)₄ has been determined by single crystal X-ray methods and refined by the least squares method. The lattice parameters of the cell (Fdd 2–C _2v ¹⁹ ) are:a=18.72;b=6.48;c=8.94 Å. With all observed reflections anR-Value of 8.50% was obtained; if allHamilton-reflections are includedR=9.41%. The Te atoms are surrounded octahedrally by 6 oxygens, the 4 oxygens around the silver atoms form a distorted tetrahedron. Two of these tetrahedra form with an intermediate octahedron a geometric unit. These units are linked together to a three-dimensional structure by oxygens belonging to two different tetrahedra and by hydrogen bondings.

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Mit 5 Abbildungen     

Die Kristallstruktur von Co4Hf2P3

Zusammenfassung Die Struktur einer ternären Phase mit der Idealzusammensetzung Co₄Hf₂P₃ wurde röntgenographisch mittels Einkristallmethoden bestimmt und verfeinert. Die Gitterparameter der hexagonalen Elementarzelle sinda=12,0559 undc=3,6249 Å, die Raumgruppe ist . Die Phase ist strukturell mit Fe₂P und Fe₁₂Zr₂P₇ verwandt.

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The structure of a ternary phase with the ideal composition Co₄Hf₂P₃ has been determined and refined by means of singlecrystal X-ray methods. The cell dimensions of the hexagonal unit cell are found to be:a=12,0559 andc=3,6249 Å, the space group is . The phase is structurally related to Fe₂P and Fe₁₂Zr₂P₇.

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Die Kristallstruktur von BaHg(CN)4 · 4 Pyridin

Crystal Structure of BaHg(CN)₄ · 4 Pyridine The structure of the tetragonal BaHg(CN)₄ · 4 Pyridine (space group I4 , a = 1119.4(7), c = 1 057.9(7) pm, Z = 2, d_c = 1.87 g · cm^?3) contains tetrahedral Hg(CN)₄ and bisdisphenoide Ba(NC)₄(py)₄ groups, which are linked together by Hg? CN? Ba bridges. The BaHg(CN)₄ framework consists of a 3-dimensional network of all round edge-sharing tetrahedrons. The analogous strontium compound is isotype with a = 1 108.2(9) and c = 1 035.3(14) pm.     

Die Kristallstruktur von Kalium-trithiowolframat-chlorid K3(WOS3)Cl

A recently prepared new thiotungstate has been characterized by three-dimensional X-ray structure analysis, to be a double salt, containing K₂WOS₃ and KCl in equimolar proportions: potassium trithiotungstate chloride, K₃(WOS₃)Cl. Space group: Pca2₁ with a = 12.507, b = 6.317, c = 12,371 Å, Z = 4. The compound represents a new structure type with stoichiometry M^I₂XY₄ · M^IZ. Besides isolated tetrahedral WOS₃^2- ions (bond lengths W–O 1.760 Å, W–S 2.208, 2.197, 2.196 Å) the structure contains Cl^? ions octahedrally co-ordinated by K⁺, the K⁺ ions having 5S + 10 + 2Cl as neighbours. The dimensions of the WOS₃^2? ions in this compound show that, as in other transition metal oxo-, thio- and selenoanions, strong π bonding is present, the W–S bonds taking part in the π bond system.     

Die Kristallstruktur von In(CH2Ph)3

Crystal Structure of In(CH₂Ph)₃ The reaction of InCl₃ with PhCH₂MgCl forms tribenzylindane 1 , precipitating from toluene as pale yellow crystals. The crystal structure shows one dimensional chains of 1 in a zigzag arrangement. The synthesis and characterization of (PhCH₂)₂InCl 2 and PhCH₂InCl₂ 3 is reported.     

Die Kristallstruktur von BaTeO3

Crystal Structure of BaTeO₃ Crystals of BaTeO₃ were prepared from melts. BaTeO₃ is isotropic with KClO₃ and crystallizes in the monoclinic system, space group P2₁/m. The lattice parameters are a = 4.63₃, b = 5.95₂, c = 7.30₈ Å, β = 111.2°. The formula unit is 2. The crystal structure was determined by Patterson synthesis, refined by least squares and confirmed by (F_o — F_c) synthesis. Using isotropic temperature corrections the R-value of 1072 observed reflections calculated as 0.748, and anisotropic the R-value as 0.702. In BaTeO₃ tellurium forms with three oxygen atoms pyramidal TeO₃-groups, barium has to oxygen atoms the coordination 7+2. The TeO₃ groups are not linked one with another, but with the BaO₉ polyhedrons by common corners and edges, the latter are linked one with another only by common edges.     

Die Kristallstruktur von Cu7(OH)6(TeO3)2(SO4)2

The crystal structure of the new phase Cu₇(OH)₆(TeO₃)₂(SO₄)₂ [a=7.389 (1),b=7.638 (1),c=7.662 (2) Å, =75.17 (1), =75.90 (1), =84.19 (1)°;Z=1] was determined by direct methods andFourier summations from X-ray intensities, and was refined in space group P -C _i ¹ toR=0.039. As usual, the Cu(II) atoms are coordinated to four O atoms forming approximately a square with average Cu-O=1.96 (3) Å; one or two more distant O neighbours complete the coordination. The shape of the TeO₃ group is a rather clear-cut trigonal pyramid. A disorder was found for the SO₄ tetrahedra. The compound was synthesized under hydrothermal conditions [500 (10) K, saturation vapour pressure].

Herrn Prof. Dr.K. Komarek zum 60. Geburtstag gewidmet.     

Die Kristallstruktur von Cs5Eu(N3)8

Summary The crystal structure of pentacesium octaazidoeuropiate(III), Cs₅Eu(N₃)₈, was determined by single crystal X-ray diffraction: orthorhombic,a=16.811(4),b=16.860(5),c=16.964(3)Å, space group Pbca,Z=8, 2 310 observed reflections,R=0.048. Europium atoms are coordinated to eight azide groups, the coordination polyhedra have no azide groups in common. Four cesium atoms are surrounded by eight, one by seven azide groups. The azide groups are symmetric with mean N-N-distances of 1.17(1)Å.

     

Synthese,Kristallstruktur und Festkörper-NMR-spektroskopische Untersuchungen von K5H(CN2)3

Synthesis, Crystal Structure, and Solid State MAS-NMR Spectroscopic Investigation of K₅H(CN₂)₃ Single phase K₅H(CN₂)₃ was synthesized by reaction of KHCN₂ with metallic potassium in liquid ammonia or by reaction of KNH₂ with melamine C₃N₃(NH₂)₃ at 320 °C, respectively. The crystal structure was determined from X-ray powder and single crystal data: K₅H(CN)₃, space group Im3m, a = 795.68(7) pm, Z = 2, R1 = 0.025, wR2 = 0.0438. In the solid K₅H(CN₂)₃ contains K⁺ and CN₂^2–, the anions exhibit D_∞h symmetry. According to ¹H and ¹³C solid state MAS-NMR investigations, temperature dependent impedance spectroscopy, and FTIR spectroscopy the protons are only loosely bound to the CN₂^2– ions. The proton conductivity shows a sharp increase above 70 °C.     

Die Kristallstruktur von Cs2NaInF6

Using single crystal data the occurence of the K₂NaCrF₆ type of structure for Cs₂NaInF₆ (a = 8.905 Å) has been confirmed and x_F determined to be x_F = 0.229; in consequence: In–F = 2.03₉ Å [430 (hkl) with h + k = 2n and h = 0 to 7; R = 11.1%; Mo? K_α.]. The Madelung Part of Lattice Energy is calculated and discussed in detail.     

Die Kristallstruktur von Li8PbO6

Crystal Structure of Li₈PbO₆ The crystal structure of Li₈PbO₆ (Li₈TbO₆ structure, space group R3 ? C, hexagonal lattice constants a = 554.3, c = 1 563 pm) has been refined by profile analysis of a neutron diffraction pattern. Deviations from ideal tetrahedral and octahedral coordination of lithium atoms are similar to those described for Li₈SnO₆.     

Die Kristallstruktur von [TeCl3(15-Krone-5)]SbCl6

The Crystal Structure of [TeCl₃(15-crown-5)]SbCl₆ The title compound is synthesized by the reaction of tellur tetrachloride, 15-crown-5 and antimony pentachloride in acetonitrile solution, forming colourless crystals, which were characterized by IR spectroscopy and an X-ray structure determination. Space group Pnma, Z = 4, 1966 observed unique reflections, R = 0.072, R_w = 0.052. The compound forms ions [TeCl₃(15-crown-5)]⁺ and SbCl₆^?; in the cation the tellurium atom is eightfold coordinated by the three chlorine atoms and the five oxygen atoms of the crownether molecule (Te? O bond lengths 266 and 279 pm).     

Die Kristallstruktur von TlFe3Te3

TlFe₃Te₃ is hexagonal, space groupP6₃/m–C _2h ⁶ ,a=9.350(2) Å,c=4.2230 (7) Å,Z=2. Iron and tellurium atoms occupy the positions 6 (h) withx=0.170,y=0.149 andx=0.046,y=0.357 respectively. Thallium atoms are situated in 2 (d). The structure was determined on the basis of single crystal data obtained form a four circle diffractometer. Refinement yielded andR-value of 4.8% for an asymmetric set of 267 reflections. TlFe₃Te₃ is a new structure type. The structure and its relations to the Mn₅Si_3–, the Nb₃Te₄-and the Tl _x V₆S₈-type are discussed.

     

Die Kristallstruktur von Cr3GeN

The crystal structure of Cr₃GeN has been determined by single crystal methods: $$\begin{gathered} Space group P \bar 42_1 m - D_{2d}^3 ; \hfill \\ a = 5.375{\AA}; c = 4.012 {\AA}; c/a = 0.7465 \hfill \\ \end{gathered} $$ The close relationship of Cr₃GeN with the phases having filled U₃Si-type and the perowskite carbides and-nitrides will be discussed.