Zur Reaktion von Thionylchlorid mit Polysulfanen: Darstellung und Eigenschaften von S8O

On the Reaction of Thionyl Chloride with Polysulfanes: Preparation and Properties of S₈O The reactions of H₂S₂, H₂S₅, and crude sulfane with thionyl chloride at low temperatures are reported. S₈O can be prepared from SOCl₂ and H₂S_x at ?40°C in CS₂/(CH₃)₂O. Solubility, density, stability, mass spectrum, and some simple reactions of S₈O are reported and discussed.     

Darstellung und Charakterisierung von P4O7S

Syntheses and Characterization of P₄O₇S P₄O₇S was synthesized for the first time and characterized by X-ray structure determination (single-crystal methods) and ³¹P-n.m.r. (solution and MAS-solid) (P1 ; a = 687.2(1); b = 718.2(1); c = 809.1(1) pm; α = 92.58(1)°; β = 104.43(1)°; γ = 94.82(2)°; 2 907 diffractometer data; R₁ = 0.030; wR² = 0.102). The different influences of terminally bound oxygen and sulfur on the geometry of the P₄O₆ cage are discussed.     

Darstellung und Kristallstruktur von Cs8P8O24 · 8H2O

Synthesis and Crystal Structure of Cs₈P₈O₂₄ · 8H₂O Cs₈P₈O₂₄ · 8H₂O was obtained from Na₈P₈O₂₄ · 6H₂O by cation exchange. Crystal growth was achieved by applying gel techniques (agar agar). The crystal structure (P1 ; a = 766.6(8); b = 1 156.9(9); c = 1 163.4(9) pm; α = 100,2(1)°; β = 106.5(2)°; γ = 92.2(1)°; Z = 1; 4 099 unique diffractometer data; R = 0.051; R(w) = 0.037) contains cyclo-octaphosphate anions with point symmetry C_2h. The cesium atoms are coordinated irregularily by eight and ten oxygen atoms, respectively. The threedimensional linkage of the P₈O₂₄^8?-rings is established via bonds to cesium atoms and hydrogen bonds Provided by H₂O molecules.     

Verbesserte Darstellung,Kristallzüchtung und Strukturanalyse von P4O6S2 und P4O6S3

Improved Syntheses, Crystal Growth, and Crystal Structure Determination of P₄O₆S₂ and P₄O₆S₃ Syntheses and single crystal growths of the title compounds are described. Both compounds crystallize in the space group P2₁/c (P₄O₆S₂: a = 11.293(4); b = 6.457(3); c = 11.588(4) Å; β = 90.29(2)°, 2 450 diffractometer data, R_w = 0.035/P₄O₆S₃: a = 15.611(5); b = 8,303(3); c = 9.697(4) Å; β = 127.12(2)°, 2 481 diffractometer data, R_w = 0.034). The structural data for the series P₄O₆S_n (n = 1 – 4) thus completed are compared to their oxide analogues P₄O₆O_n (n = 1 – 4). The changes in the geometry of the P₄O₆-cage in course of its successive oxidation are discussed.     

Darstellung und Kristallstruktur von Cyclooktadekaschwefel,S18, und Cycloikosaschwefel,S20

Preparation and Crystal Structure of Cyclooctadecasulphur, S₁₈, and Cycloikosasulphur, S₂₀ Starting with mixtures of sulfanes and chlorosulfanes new sulfur rings S₁₈ and S₂₀. are synthesized according to The new compounds are remarkable stable. Preparation of the starting materials as well as the structure determinations by X-rays are reported.     

Darstellung und Kristallstruktur von Ag2O3

Preparation and Crystal Structure of Ag₂O₃ The novel compound Ag₂O₃ was obtained by anodic oxidation of aqueous solutions of AgBF₄, AgClO₄, and AgPF₆. According to single crystal investigations Ag₂O₃ belongs to the orthorhombic crystal system (Fdd2; a = 1286.9(1), b = 1049.0(1), c = 366.38(5) pm; Z = 8; 309 independent diffractometer data; R = 1.2%). Ag₂O₃ is isostructural to Au₂O₃ and contains silver square-planarly coordinated by oxygen. The AgO₄ groups are connected via common vertices forming a 3-d framework.     

Zur Darstellung und Kristallstruktur von Tl2O

The preparation of Tl₂O and its crystal structure is discussed. By FOURIER methods for a monoclinic unit cell(a_M = 6.08₂, b_M = 3.52₀, c_M = 13.2₄ Å, β = 108.2°, Z = 4, space group C_2h³) the determined atomic parameters can be transformed into the trigonal system by the assumption of special oxygen positions (space group No. 166–R3 m). Correspondingly the Tl₂O crystal structure may be described as a threefold polytype form of the anti CdJ₂ type (a_H = 3,51₆ c_H = 37.8₄ Å; c/a = 10.76, Z = 6, mol. vol. = 40.7 cm³; d_x = 10.44, d_pyk = 10.4 g m^?).     

Darstellung,Eigenschaften und Phasenbeziehungen von Ru3Sn15O14

Preparation, Properties, and Phase Relations of Ru₃Sn₁₅O₁₄ Coexistence relations in the system Ru/Sn/O have been investigated by X‐ray measurements of powder mixtures annealed in the region of 1173–1273 K. Thermodynamic data of Ru₂Sn₃, Ru₃Sn₇, and Ru₃Sn₁₅O₁₄ were obtained by EMF measurements. Phase diagrams calculated with these data are in good agreement with experimental results. Only one phase, Ru₃Sn₁₅O₁₄, exists in the ternary system between 973 and 1273 K. Red translucend single crystals were obtained from a tin melt. Polycrystalline powder was prepared by solid state reaction of a mixture of Ru₃Sn₇, SnO₂, and Sn with molar ratio 1:7:1 at 1173 K. Ru₃Sn₁₅O₁₄ is a p‐type semiconductor, E_A = 0.50(5) eV, as conductivity and thermopower measurements show. Mössbauer investigations confirm the existence of three different tin surroundings.     

Zur Darstellung und Struktur von LaNb5O14

Preparation and Structure of LaNb₅O₁₄ Single crystals of LaNb₅O₁₄ could be prepared by chemical transport reactions (T₂ → T₁; T₂ = 1050°C; T₁ = 950°C) using chlorine as transport agent. LaNb₅O₁₄ crystallizes in the orthorhombic space group Pbem with cell dimensions a = 3.8749(2) Å; b = 12.4407(6) Å and c = 20.2051(9) Å; Z = 4; R = 6.28%, R_w = 3.74%. The structure consists of two types of Nb? O-polyhedra. Especially remarkable are chains of edge-sharing pentagonal NbO₇-bipyramids, which are interconnected by corner-sharing NbO₆-octahedra. Tunnels running in a-direction are created by this framework of NbO₆- and NbO₇-polyhedra. Lanthanum atoms are located in these tunnels at levels inbetween the niobium atoms. The relationship to O? LaTa₃O₉ and M? CeTa₃O₉ type structures will be discussed.     

Darstellung,Struktur und Eigenschaften von Ag10Si3S11

Preparation, Crystal Structure and Properties of Ag₁₀Si₃S₁₁ The novel orange-red thiosilicate Ag₁₀Si₃S₁₁ is formed besides Ag₈SiS₆ by the high - temperature reaction between Ag₂S, Si and S. The single crystal structure analysis shows the compound to be silver orthothiosilicate thiodisilicate-(1:1) Ag₁₀(SiS₄)(Si₂S₇). The mean Si? S bond lengths are 2.137 Å for SiS₄^(4?) and 2.129 Å for the hitherto unknown Si₂S₇^(6?). The cation sublattice is slightly imperfect. inferring a certain mobility of the Ag⁺ ions. Ag₁₀Si₃S₁₁ crystallizes in the triclinic space group P1 . Lattice constants see ?Inhaltsübersicht”?. The vibrational spectrum (IR) shows absorptions within the characteristic spectral regions for asymmetric and symmetric stretching vibrations of the SiS₄ tetrahedra at 490–515 and 423–433 cm^?1.     

Darstellung,Kristallstruktur und spektroskopische Charakterisierung von P4O6Se3

Synthesis, Crystal Structure, and Spectroscopic Characterization of P₄O₆Se₃ P₄O₆Se₃ has been prepared for the first time as a pure substance by photochemical selenation of P₄O₆ with red selenium. The compound crystallizes in a monoclinic system with space group P2₁/a (a = 973.6(2); b = 846.9(2); c = 1277.7(3) pm; β = 90.56(2)°; Z = 4; 1358 diffractometer data; R₁ = 0.044; wR² = 0.099). Bond lengths and angles within the molecule as well as the arrangement of the molecules within the crystal are discussed; vibrational (IR and Raman) and ³¹P-n.m.r. (solution) data are given.     

Darstellung und Kristallstruktur von Na2Mn3O7

Synthesis and Crystal-Structure of Na₂Mn₃O₇ Single crystals of Na₂Mn₃O₇ have been grown hydrothermally applying high oxygen pressure (p = 2 kbar). The new compound cystallizes triclinic; space group P1 ; a = 6.636(6) Å, b = 6.854(6) Å, c = 7.548(6) Å, α = 105.76(6)°, β = 106.86(6)°, γ = 111.60(6)°; Z = 2. The crystal structure has been solved and refined to R = 7.9% and R_w = 6.2% (diffractometer data, 1044 independent reflexions). The crystal structure consists of Mn₃O₇^2? anions with manganese coordinated octahedrally by oxygen. These layered anions are hold together by Na⁺ ions (coordination numbers 5 and 6).     

Darstellung und Struktur von Ag2C4O4

Preparation and Structure of Ag₂C₄O₄ Ag₂C₄O₄ occurs in a yellow and a colourless modification. Both forms decompose to metallic silver upon heating. Ag⁺ is coordinated in two different fashions in the yellow Ag₂C₄O₄. Ag(1) shows distorted tetrahedral coordination, Ag(2) is coordinated in an unusual distorted square planar manner. The connection of Ag⁺ and C₄O₄^2? leads to a complicated three-dimensional framework. C₄O₄^2? is planar with C? O and C? C bonds lengths typical of complete delocalization of the π-electron system.