Synthese und Kristallstruktur von Tetramethylammonium-Sodalith

Tetramethylammonium sodalite, a synthetic species of composition (CH₃)₄NAlSi₅O₁₂, has been obtained in good yield under hydrothermal conditions in the absence of metal cations. Its crystal structure has been determined using accurate powder data since single crystals could not be grown. The structure seems to be body-centered cubic with a = 8.975 Å but the true symmetry is non-cubic (probable space group I4 ). Each cage of the aluminosilicate framework contains one tetramethylammonium ion. The organic cation does not conform to the cubic symmetry of the ideal framework. The methyl groups point to oxygen atoms of the framework, and the short methyl-oxygen distances of 3.06 Å indicate strong C? H … O interaction. The present results indicate beyond doubt that C? H … O hydrogen bonding involving methyl groups can occur in silicates. This is of particular significance in zeolite chemistry and in the interpretation of interlayer distances in organic clay complexes.     

Synthese und Kristallstruktur von Tetramethylammonium-Gismondin

A new synthetic zeolite, (CH₃)₄NA1Si₃O₈, H₂O, has been synthesized and shown to be an isotype of the mineral gismondine, CaAl₂Si₂O₈,4H₂O. Sodium and other cations can be introduced by ion exchange after thermal decomposition of the organic cation. A continuous structural change to «cubic» NaP has thereby been recorded, which indicates that the latter is also based on a gismondine-type aluminosilicate framework. The crystal structure of tetramethylammonium-gismondine has been determined using X-ray powder data supplemented by electron diffraction. The crystals are tetragonal, a = 9.84 and c = 10.02 Å, with 4 formula units per unit cell. The apparent symmetry of the framework structure is I4₁/amd, however, this is violated by the organic cation. Two of the methyl groups are pointing to oxygen atoms of the framework and the short methyl-oxygen distances indicate C? H ? O interaction.     

Synthese und Kristallstruktur von N-Formylformamidinium-hexachloroantimonat

Synthesis and X-Ray Structure Determination of N-Formylformamidinium Hexachloroantimonate The title compound is formed in high yields by the interaction of [Cl₂CH? NH? CH?NH₂][SbCl₆] with SO₂ in CH₂Cl₂ solution. According to the spectra (i.r. and ¹H-n.m.r.) the cation [O?CH? NH? CH?NH₂]⁺ exists in an almost planar, all-cisoide conformation. The hexachloroantimonate crystallizes in the orthorhombic space group Pna2₁ with 4 formula units per cell. The anion-cation cross-linkage by relative short NH…?Cl(Sb) bridges is remarkable. The structure was refined to an R value of 0.027.     

Synthese und Kristallstruktur von CaBiVO5

Synthesis and Crystal Structure of CaBiVO₅ Single crystals of the hitherto unknown compound CaBiVO₅ were prepared and investigated by X-ray work. It crystallizes with orthorhombic symmetry, space group D? Pbca, a = 11.2022, b = 5.4283, c = 15.5605 Å, Z = 8. The crystal structure is characterized by layers of the edge-linked CaO₇ polyhedra, isolated VO₄ tetrahedra and an asymmetric surrounding of Bi³⁺ by oxygen.     

Synthese und Kristallstruktur von KTeOF3

Synthesis and Crystal Structure of KTeOF₃ KTeOF₃ has been synthesized by solid state reaction of KF, TeO₂ and KTeF₅ in equimolar amounts. Its crystal structure has been solved by single crystal structure analysis (P4₂/n, a = 1007.96(3), c = 789.58(3) pm, Z = 8, R₁ = 0.0311). As a characteristic feature, the compound contains unprecedented dimeric anions Te₂O₂F₆^2– formed by two edge‐sharing pseudo‐octahedral units. IR and Raman data are given.     

Synthese und Kristallstruktur von LiHSO4

Synthesis and Crystal Structure of LiHSO₄ Single crystals of the new compound LiHSO₄ are synthezised from the system Lithiumsulfate/Sulfuric acid. The up to day not determined structure of the title compound is monoclinic, space group P2₁/c with the lattice constants a = 5.234(2), b = 7.322(1) and c = 8.363(1) Å, b? = 90.02(2)°. The volume of the unit cell has been determined to V = 320.5 ų, the number of formula units to Z = 4 and the density to D_x = 2.156 g cm^?3. There are crystallographically identical SO₃(OH)- and LiO₄-tetrahedra in the structure. Every tetraheda is linked to four different tetrahedra of the other sort. Two neighboured LiO4 terahedra form a common edge. In that way layers are formed running parallel the yz-plane. These layers are connected over hydrogen bonds.     

Synthese und Kristallstruktur von BaVo2,5

Single crystals of BaVO_2,5 were prepared by high temperature LASER-technique under a hydrogen atmosphere. The X-ray investigation leads to a trigonal symmetry (a=571.8;c=1161.3 pm, space group C _3v ¹ -P3m 1). BaVO_2,5 consists of a closest sphere packing of oxygen with a sequence of cubic and hexagonal layers of the type ... ccchh ... The consequences in respect to the coordination of Ba²⁺ and V³⁺ are discussed.

     

Synthese und Kristallstruktur von Rb3PbCl5

Synthesis and Crystal Structure of Rb₃PbCl₅ The synthesis of the hitherto unknown compound Rb₃PbCl₅ in the quasi-binary system RbCl/PbCl₂ and its structure determination is reported. This 3 : 1-phase decomposes peritectoidally at 305 °C and crystallizes in a so far unknown structure type in the orthorhombic space group Pnma (a = 863.498(5) pm, b = 1573.11(1) pm, c = 838.875(5) pm). It shows typical structural characteristics of ns²-configurated cations, although there are more noble gas-configurated cations than ns²-configurated cations in the structure.     

Synthese und Kristallstruktur von Cs3AuO2

Synthesis and Crystal Structure of Cs₃AuO₂ Bright orange single crystals of Cs₃AuO₂, sensitive to moisture and atmosphere, are obtained by reacting CsAu with a 1 : 1 molar mixture of Cs₂O and CsO₂ (CsAu : Cs₂O : CsO₂ = 3 : 2 : 2) in sealed silver crucibles under argon atmosphere at 380 °C for a period of 6 days. The crystal structure (Pearsoncode mP72, P2₁/n, a = 1019.6(3), b = 1984.3(7), c = 1028.5(4) pm, β = 93.96(1)°, Z = 12, 2562 reflections mit I_o > 2σ(I), R₁ = 0.0662, wR₂ = 0.1660) is characterized by the presence of dumb‐bell‐shaped [O–Au–O]‐moieties (d(Au–O) = 200,8(2) pm), a common feature of oxoaurates(I).     

Synthese und Kristallstruktur von Cu2PtIIPtS8

Synthesis and Crystal Structure of Cu₂Pt^IIPt S₈ (NH₄)₂PtCl₆ and Cu(CH₃COO)₂ were reacted at 380 K in a constant flow of H₂S in the molar ratio of 2:1. Subsequent annealing of the product in sealed quartz glass ampoules in the presence of CuS as a buffer for the sulfur activity (temperature range 770 to 870 K) yields Cu₂Pt₄S₈ as a polycrystalline, greyish black powder. Cu₂Pt₄S₈ crystallizes in the space group P2/n (No. 13) with the cell parameters a = 10.6478(2), b = 6.9350(1), c = 6.7411(1) Å, β = 91.942(1), Z = 2. The structure determination and refinement were performed by the means of x-ray powder diffraction data of this first copperthioplatinate. There are no isotypic compounds known, so far. According to the characteristic coordination of the metals by sulfur, the oxidation states are Cu^+I, Pt^+II and Pt^+IV, the compound may be formulated as Cu₂Pt^+IIPtS₈. Cu₂Pt₄S₈ exhibits diamagnetic and semiconducting properties.     

Zur Synthese und Kristallstruktur von LiPdAlF6 und PdZrF6

Synthesis and Crystal Structure of LiPdAlF₆ and PdZrF₆ . For the first time single crystals of the new compounds LiPdAlF₆ and PdZrF₆ have been obtained. LiPdAlF₆ (blue) crystallizes trigonal, space group P3 1c—D (No. 163; LiCaAlF₆-type [2]), in an ordered structure variant of the Li₂[ZrF₆]-structure [3], with a=497.21(9) pm, c=914.0(9) pm and Z=2. PdZrF₆ (also blue) is isotypic with LiSbF₆ [4] and crystallizes trigonal-rhomboedric with a=552,3(1) pm, c=1 447,5(4) pm, space group R 3 —C (No. 148) and Z=3.     

Die Synthese und Kristallstruktur von K2UTe3

The Synthesis and Crystal Structure of K₂UTe₃ Syntheses of K₂UTe₃ were performed via polytelluride fluxes from K₂Te₃ and metallic uranium in the molar ratio 2 : 1 at 600 to 800 °C. Well-formed crystals were isolated by washing the reguli with liquid ammonia. One-phase powder samples of K₂UTe₃ are also available by reactions of stoichiometric mixtures of K₂Te₃ and uranium. K₂Te₃ was prepared in liquid ammonia from the elements using a glass apparatus specially designed for the synthesis of alkali metal chalcogenides. By x-ray structure analyses of single crystals we found K₂UTe₃ to crystallize monoclinic (space group C2/m, Z = 4) with the lattice parameters a = 800.41(3) pm, b = 1387.67(5) pm, c = 851.63(4) pm and β = 108.495(3)°. The crystal structure of the compound may be regarded as a stuffed AlCl₃-type structure. The existence of an analogous compound Rb₂UTe₃ crystallizing isotypically to K₂UTe₃ has been shown by x-ray powder investigations.     

Synthese und Kristallstruktur von Bi2ErO4I

Synthesis and Crystal Structure of Bi₂ErO₄I Bi₂ErO₄I was prepared by solid‐state reaction of stoichiometric mixture of BiOI, Bi₂O₃ and Er₂O₃. Bi₂ErO₄I is a new compound and the first bismuth rare earth oxide iodide. The crystal structure was determined by the Rietveldmethod (P4/mmm, a = 3,8896(6) Å, c = 9,554(2) Å, Z = 1). In this structure [M₃O₄]⁺‐layers are interleaved by single I^–‐layers. Er and Bi atoms of Bi₂ErO₄I are 8‐coordinated. The structure can be derived from the LiBi₃O₄Cl₂‐structure type.     

Synthese und Kristallstruktur von Calcium-Kupfer-Diarsenat CaCuAs2O7

Synthesis and Crystal Structure of the Calcium Copper Diarsenate CaCuAs₂O₇ Solid state reactions led to single crystals of CaCuAs₂O₇. X-ray investigations revealed monoclinic symmetry, space group C⁵_2h-P2₁/c, lattice constants a = 7.272(1); b = 8.946(2); c = 9.307(2) Å; β = 109.48(2)°; Z = 4. CaCuAs₂O₇ is characterized by ¹_∞[CaO₆] chains, connected by As₂O₇ double tetrahedra and elongated square CuO₅ pyramids. The hitherto unknown crystal structure shows relationships to CaCuP₂O₇ but not to CaCuV₂O₇.     

Synthese und Kristallstruktur von K2Mn3S4

Synthesis and Crystal Structure of K₂Mn₃S₄ Single crystals of K₂Mn₃S₄ have been prepared by a fusion reaction of potassium carbonate with manganese in a stream of hydrogen sulfide at 900 °C. K₂Mn₃S₄ crystallizes in a new monoclinic layered structure type (P2/c, a = 7.244(2) Å, b = 5.822(1) Å, c = 11.018(5) Å, β = 112.33(3)°, Z = 2) which can be described as a stacking variant of the orthorhombic Cs₂Mn₃S₄ structure type. Measurements of the magnetic susceptibilities show antiferro‐magnetic interactions.     

Synthese,Kristallstruktur und Eigenschaften von Na2RbAuO2

Synthesis, Crystal Structure, and Properties of Na₂RbAuO₂ Single phase samples of Na₂RbAuO₂ were prepared by reacting RbAu with Na₂O₂ in an equimolar ratio in sealed silver cylinders (placed under argon in glas tubes) at 400 °C for two weeks. The colourless single crystals of needle shaped habitus decompose immediately when exposed to air. Na₂RbAuO₂ (Pearsoncode oP12, Pnnm, a = 992.76(6), b = 559.03(3), c = 408.64(3) pm, Z = 2, 414 reflections with I_o > 2σ(I), R₁ = 0.0363, wR₂ = 0.1057) crystallizes isotypic with Na₂KAuO₂. Besides linear [O–Au–O] units, which are characteristic for oxoaurates(I), the structure reveals uncommon low coordination numbers for the alkali metal cations.     

Synthese und Kristallstruktur von Cu6Mo5O18

Synthesis and Crystal Structure of Cu₆Mo₅O₁₈ Single crystals of the hitherto unknown compound Cu₆Mo₅O₁₈ were prepared and investigated by X-ray methods (a = 18.884(19), b = 6.273(7), c = 15.259(23) Å, β = 130.40(5)°, space group C–C2/c, Z = 4). The typical features of the structure are described and compared with the crystal chemistry of oxocuprates(I). Observed and calculated powder patterns show that the correct composition of the earlier described compound Cu₆Mo₄O₁₅ is Cu₆Mo₅O₁₈.     

Synthese und Kristallstruktur von Cs3Y7Se12

Synthesis and Crystal Structure of Cs₃Y₇Se₁₂ The oxidation of yttrium metal with selenium in the presence of CsCl (7 d, 700°C, evacuated silicia tubes) results in the formation of pale yellow, lath-shaped single crystals of Cs₃Y₇Se₁₂. The crystal structure (orthorhombic, Pnnm, Z = 2, a = 1272.8(3), b = 2627.7(5), c = 413.32(8) pm) consists of edge- and vertex-connected [YSe₆] octahedra forming a rocksalt-related network [Y₇Se₁₂]^3?. One-dimensional infinite channels along [001], apt to take up extra cations, provide coordination numbers of 6 and 7 + 1, respectively, for two crystallographically different Cs⁺.     

Synthese und Kristallstruktur von Ba6ZnIn2Cl20

Synthesis and Crystal Structure of Ba₆ZnIn₂Cl₂₀ Colourless single crystals of Ba₆ZnIn₂Cl₂₀ are obtained from a 6 : 3 : 2 molar mixture of BaCl₂, ZnCl₂ and InCl₃ at 420 °C in a Pyrex ampoule. It crystallizes with the monoclinic space group P2₁/c (Z = 4) with a = 1957.8(2), b = 1014.69(8), c = 1778.7(2) pm, β = 110.94(1)°, in a new structure. Zn²⁺ is surrounded tetrahedrally and In³⁺ octahedrally by chloride ions. Half of the [InCl₆] octahedra are isolated from each other, the other half shares common edges to form [In₂Cl₁₀] double octahedra. Ba²⁺ has coordination numbers of eight and nine. There are chloride ions that do not belong to Zn²⁺ or In³⁺ so that the formula may be written as Ba₁₂Cl₁₀[ZnCl₄]₂[InCl₆]₂[In₂Cl₁₀].     

Synthese und Kristallstruktur von Sr2Rh7P6

Synthesis and Crystal Structure of Sr₂Rh₇P₆ Single crystals of Sr₂Rh₇P₆ were obtained by reaction of the elements in molten lead at 1100 °C and investigated by X-ray methods. The compound crystallizes tetragonally (a = 11.080(2), c = 4.098(1) Å) and forms a crystal structure (P 4 2₁m; Z = 2) with ThCr₂Si₂ analogous units, which are linked with each other in a new way. Therefore the RhP₄ tetrahedra form bands of edge sharing chains parallel to [001] anstead of layers as in the ThCr₂Si₂ type structure. The arrangement enables a part of the P atoms to form short P–P distances of 2,26 Å and space for additional Rh atoms with a likewise distorted tetrahedral coordination of P atoms is obtained.