Verfeinerung der Kristallstruktur von K2O2

Refinement of the Crystal Structure of K₂O₂ The crystal structure of K₂O₂ has been refined using 241 diffractometer data (Cmca; a = 6.733(1), b = 6.996(1), c = 6.474(1) Å; Z = 4; R_w = 0.050). The distance O? O (1.541(6) Å) is significantly larger than that one assumed for alkali metal peroxides, so far.     

Verfeinerung der Kristallstruktur von SrO2

Refinement of the Crystal Structure of SrO₂ Single crystals of SrO₂ have been obtained after high pressure/high temperature reaction of a SrO/KClO₃ mixture at 20 kbar, 1 400°C. The crystal structure was refined using 154 unique diffractometer data (I4/mmm; a = 3.5626(3), c = 6.6159(6) Å; Z = 2; R = 0.033, R_w = 0.022, S = 0.932). The O O distance (1.493(4) Å) is significantly longer than the one previously assumed. From a refinement of the site occupation factor for oxygen a composition SrO_1.95(2) has been found for the crystal investigated.     

Die Verfeinerung der Kristallstruktur von Li2Ge2O5

Zusammenfassung Die Kristallstruktur von Li₂Ge₂O₅ wird durchFourier- und Differenz-Fourier-Synthesen verfeinert. Als mittlere Atomabstände werden gefunden: Ge–O=1,71 und Li–O=1,96 Å.

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The crystal structure of Li₂Ge₂O₅ has been refined byFourier and difference syntheses. The average atomic distances are found to be: Ge–O=1,71 and Li–O=1,96 Å.

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Verfeinerung der Kristallstruktur von 1,4-trans-Diaminocyclohexan-dihydrochlorid

The previously described structure of 1, 4-trans-diaminocyclohexane dihydrochloride has been further refined by full-matrix least-squares analysis with an improved weighting scheme.     

Die Verfeinerung der Kristallstruktur von ThOTe

Refinement of the Crystal Structure of ThOTe The crystal structure of ThOTe has been refined with single crystal data. The compound crystallizes in a PbFCl-type arrangement (space group P4/nmm, a = 412.8(2) pm, c = 755.8(7) pm, z(Th) = 0.17081(6), z(Te) = 0.6348(1)).     

Synthese und Kristallstruktur von NaPr2F3(SO4)2

Synthesis and Crystal Strucure of NaPr₂F₃(SO₄)₂ Light green single crystals of NaPr₂F₃(SO₄)₂ have been obtained by the reaction of Pr₂(SO₄)₃ and NaF in sealed gold ampoules at 1050 °C. In the crystal structure (monoclinic, I2/a, Z = 4, a = 822.3(1), b = 692.12(7), c = 1419.9(2) pm, β = 95.88(2)°) Pr³⁺ is coordinated by four F^– ions and six oxygen atoms which belong to five SO₄^– ions. Thus, one of the latter acts as a bidentate ligand. The [PrO₆F₄] units are connected via three common fluoride ions to pairs with a Pr–Pr distance of 386 pm. Na⁺ is sevenfold coordinated by three fluorine and four oxygen atoms.     

Verfeinerung der Kristallstruktur des Minerals Claudetit,As2O3 (“Claudetit I”)

The mineral claudetite crystallizes monoclinic (a ₀=5.25,b ₀=12.99,c ₀=4.53 Å, =93.88⁰;Z=4) with space group P 2₁/n-C _2h ⁵ . For 680 independent x-ray intensities, collected on aWeissenberg-type diffractometer, an R-factor of 4.9% was obtained. The AsO₃-groups of the structure are connected by common oxygen corners in two dimensions forming puckered layers ² As₂O₃.

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Zur Kenntnis von LiSi2N3: Synthese und Verfeinerung der Kristallstruktur

On LiSi₂N₃ – Synthesis and Crystal Structure Refinement Single-crystalline LiSi₂N₃ was obtained by the reaction of lithium and silicon diimide under N₂ atmosphere in a radio-frequency furnace at 1300 °C. LiSi₂N₃ is isotypic with Li₂SiO₃ and it crystallizes as an ordered variant of wurtzite. A single-crystal X-ray diffraction analysis (Cmc2₁, a = 922.15(9), b = 529.64(8), c = 477.98(5) pm, Z = 4, R1 = 0.0173, wR2 = 0.0382) confirms and improves the structural data which previously had been obtained from powder diffraction data.     

Saure Sulfate des Neodyms: Synthese und Kristallstruktur von (H5O2)(H3O)2Nd(SO4)3 und (H3O)2Nd(HSO4)3SO4

Acidic Sulfates of Neodymium: Synthesis and Crystal Structure of (H₅O₂)(H₃O)₂Nd(SO₄)₃ and (H₃O)₂Nd(HSO₄)₃SO₄ Light violett single crystals of (H₅O₂)(H₃O)₂ · Nd(SO₄)₃ are obtained by cooling of a solution prepared by dissolving neodymium oxalate in sulfuric acid (80%). According to X‐ray single crystal investigations there are H₃O⁺ ions and H₅O₂⁺ ions present in the monoclinic structure (P2₁/n, Z = 4, a = 1159.9(4), b = 710.9(3), c = 1594.7(6) pm, β = 96.75(4)°, R_all = 0.0260). Nd³⁺ is nine‐coordinate by oxygen atoms. The same coordination number is found for Nd³⁺ in the crystal structure of (H₃O)₂Nd(HSO₄)₃SO₄ (triclinic, P1, Z = 2, a = 910.0(1), b = 940.3(1), c = 952.6(1) pm, α = 100.14(1)°, β = 112.35(1)°, γ = 105.01(1)°, R_all = 0.0283). The compound has been prepared by the reaction of Nd₂O₃ with chlorosulfonic acid in the presence of air. In the crystal structure both sulfate and hydrogensulfate groups occur. In both compounds pronounced hydrogen bonding is observed.     

Synthese und Kristallstruktur von CsAu(SO4)2

Synthesis and Crystal Structure of CsAu(SO₄)₂ Light yellow single crystals of CsAu(SO₄)₂ were obtained upon evaporation of a solution of Au(OH)₃ and Cs₂SO₄ in sulfuric acid (96 % H₂SO₄). In the crystal structure (monoclinic, P2₁/c, Z = 4, a = 1029.7(2), b = 893.4(2), c = 901.0(1) pm, β = 111.08(1)°) Au³⁺ is in square planar coordination of oxygen atoms which belong to four SO₄^— ions. According to [Au(SO₄)_4/2]^— puckered layers are formed which are connected by the Cs⁺ ions. The latter are surrounded by five chelating and three monodentate sulfate groups leading to a CN of 13.     

Verfeinerung der Kristallstruktur von Kupfer(II)-hydroxichlorid,Cu(OH)Cl

The crystal structure of Cu(OH)Cl [a=5.555 (2) Å,b=6.671 (4) Å,c=6.127 (2) Å, =114.88 (3)°, space group P2_I/a,Z=4] was refined for 810 observed reflections with sin /0.80 Å^–1 toR=0.035. Crystals were synthesized under hydrothermal conditions. The copper atom is planar four coordinated by three oxygen atoms and one chlorine atom; two further chlorine atoms complete its coordination. The copper polyhedra share edges to build up sheets, which are connected by hydrogen bonds to the chlorine atoms of adjacent sheets.

     

Verfeinerung der Kristallstruktur des Dicaesium-Tetraazido-Zinkates Cs2Zn(N3)4 und die Kristallstrukturen komplexer Zinkazide

Summary The crystal structure of dicesium-tetraazido-zincate, Cs₂Zn(N₃)₄, has been refined from single crystal X-ray-diffractometer data. The previously reported orthorhombic structure, consisting of isolated Zn(N₃)₄-tetrahedra was confirmed and improved lattice parameters and atomic distances were determined. The azide groups are asymmetric and the coordination of central nitrogen atoms to cesium was observed. A table of structure data and mean atomic distances for fourteen zinc-azide compounds is added and the structures are discussed.

Herrn Prof. Dr. Karl Torkar zum 70. Geburtstag gewidmet     

Die Kristallstruktur von Dikalium-trikobalt(II)-dihydroxid-trisulfat-dihydrat,K2Co3(OH)2(SO4)3·2H2O

Crystals of K₂Co₃(OH)₂(SO₄)₃·2H₂O were synthesized under hydrothermal conditions. The crystal structure [a=17.945 (4) Å,b=7.557 (2) Å,c=9.760 (3) Å, space group Cmc2₁,Z=4] was determined by direct methods and refined with single crystal X-ray data. The H atoms were located byFourier syntheses. Their structural parameters were refined, too. The finalR-values areR=0.025 andR _w =0.028 (w=1/) for 612 reflections withF ₀>3 (F ₀). Both Co(II) atoms are octahedral six coordinated and form zigzag chains running parallel [001]. These chains are connected via sulfate groups to built up sheets parallel (100). The KO₉ polyhedron and one of the four hydrogen bonds link these sheets.

     

Wasserfreie Sulfate der Selten‐Erd‐Elemente: Synthese und Kristallstruktur von Y2(SO4)3 und Sc2(SO4)3

Anhydrous Sulfates of Rare Earth Elements: Syntheses and Crystal Structures of Y₂(SO₄)₃ and Sc₂(SO₄)₃ The reaction of YCl₃ and Li₂SO₄ in sealed gold ampoules yields colorless single crystals of Y₂(SO₄)₃. According to the X‐ray single crystal determination the compound crystallizes with orthorhombic symmetry (Pbcn, Z = 4, a = 1273.97(13), b = 916.76(9), c = 926.08(7) pm, R_all = 0.0274). The crystal structure is buildt up from [YO₆] octahedra and sulfate tetrahedra connected via all vertices. In the same way [ScO₆] octahedra and sulfate groups are connected in the crystal structure of Sc₂(SO₄)₃ (trigonal, R‐3, Z = 6, a = 870.7(1), c = 2247.0(4) pm, R_all = 0.0255). Single crystals of Sc₂(SO₄)₃ were obtained via crystallisation of powder samples from a NaCl melt. The crystal structures of both compounds are closely related to each other and to the binary sulfides Rh₂S₃ and Lu₂S₃; the structures are the same with the complex SO₄^2– ions replacing the S^2– ions of the sulfides.     

Verfeinerung der Kristallstruktur des Natriummetagermanats,Na2GeO3

Zusammenfassung Die Kristallstruktur des Natriummetagermanats, Na₂GeO₃, wurde mit dreidimensionalen Daten bis zu einemR-Wert von 4.4% verfeinert. Daraus ergab sich für die Metagermanatkette ein mittlerer Ge–O-Abstand von 1.836 Å für das Brückensauerstoffatom und von 1.713 Å für das terminale Sauerstoffatom. Der mittlere Na–O-Abstand beträgt 2.39 Å (KZ=5).

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Refinement of the crystal structure of sodium metagermanate, Na₂GeO₃

The crystal structure of sodium metagermanate, Na₂GeO₃, has been refined by three-dimensional data resulting anR-value of 4.4%. The mean Ge–O distances in the metagermanate chain were found to be 1.836 Å for the bridging oxygen atom and 1.713 Å for the terminal oxygen atom. An average value of 2.39 Å was calculated for the Na–O distance (c.n.=5).

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