Die Kristallstruktur von AgCu3Cu(AsO4)3 und ihre strukturellen Beziehungen zu AgCo3H2(AsO4)3 bzw. AgZn3H2(AsO4)3

Crystal Structure of AgCu₃Cu(AsO₄)₃ and its Structural Relations to AgCo₃H₂(AsO₄)₃ and AgZn₃H₂ (AsO₄)₃ The compound AgCu₃Cu(AsO₄)₃ was synthesized and investigated by X-rays. It crystallizes in the monoclinic space group C2/c with a = 1 212.7(2), b = 1 249.0(2), c = 727.8(1) pm, β = 117.94(1)°, Z = 4. The structure is closely related to the structures of AgCo₃H₂(AsO₄)₃ and AgZn₃H₂(AsO₄)₃. Only two hydrogen atoms are replaced by an additional copper atom forming a copper coordination square instead of two hydrogen bridges. The remaining copper atoms are sixfold coordinated with the generally observed Jahn-Teller distortion. Whereas in AgCo₃H₂(AsO₄)₃ and AgZn₃H₂(AsO₄)₃ silver has a (4+4) coordination, it is in this compound distinctly eightfold coordinated.     

Darstellung und Kristallstruktur von Cs2Mn(PO3)4

Synthesis and Crystal Structure of Cs₂Mn(PO₃)₄ On heating mixtures of Cs₂CO₃, MnO and H₃PO₄ with Cs:Mn:P = 3:1:5 at 500°C Cs₂Mn(PO₃)₄ is formed. The by-product (CsPO₃)_n may be removed by leaching with water. The x-ray structure determination (P2₁/n; a = 797.62(3), b = 1324.91(6), c = 1154.62(8) pm; β = 101.97(1)°; Z = 4) proves the title compound to contain an infinite chain of corner sharing tetrahedra.     

Zur Darstellung und Kristallstruktur der Thiotellurite BaTeS3 · 2 H2O und (NH4)2TeS3

Preparation and Crystal Structure of the Thiotellurites BaTeS₃·2H₂O and (NH₄)₂TeS₃ The new compounds BaTeS₃ · 2 H₂O and (NH₄)₂TeS₃ have been prepared and their structures determined. According to these the anion of the trithiotelluric acid in these compounds represents a distorted trigonal TeS?pyramid. The Te? S-distances are 2.34–2.36 Å. Crystallographic data see ?Inhaltsübersicht”?.     

Darstellung und Kristallstruktur von Ba(en)4(SbSe2)2

Preparation and Crystal Structure of Ba(en)₄(SbSe₂)₂ The new compound Ba(en)₄(SbSe₂)₂ can be synthesized by dissolving of Ba₄Sb₄Se₁₁ in ethylenediamine. It crystallizes in the monoclinic system, space group P2₁/c, with lattice constants see “Inhaltsübersicht”. Characteristic elements of the structure are [SbSe₂^?]_n chains, which are formed by distorted trigonal SbSe₃ pyramids connected by common corners.     

Darstellung und Kristallstruktur von Cadmiumazid Cd(N3)2

Preparation and Crystal Structure of Cadmium Azide Cd(N₃)₂ Solvent free, binary cadmium azide was synthesized by the reaction of cadmium carbonate and a 24 weight% solution of HN₃ in water. Cadmium azide is a colorless, crystalline powder which is highly sensitive to percussion and heat. Caution, the manipulation of Cd(N₃)₂ is very dangerous! The crystal structure was solved by single‐crystal methods and the phase purity was verified by a Rietveld refinement (Cd(N₃)₂, Pbca, no. 61; a = 7.820(2), b = 6.440(2), c = 16.073(3) Å; Z = 8, 1174 independent reflections, 64 parameters, R1 = 0.022). Cadmium azide crystallizes in a new structure type. In the crystal there are edge‐sharing Cd₂(N₃)₁₀ double octahedrons which are further connected to other units by azide bridges. Vibrational spectroscopic investigations (Raman an IR) are discussed with respect to the crystal structure data.     

Darstellung und Kristallstruktur von [(Me3SiCH2)2InP(H)Ad]2

Preparation and Crystal Structure of [(Me₃SiCH₂)₂InP(H)Ad]₂ Reaction of (Me₃SiCH₂)₃ In with AdPH₂ (Ad = adamantyl) in the presence of AgNO₃ leads to [(Me₃SiCH₂)₂InP(H)Ad]₂ 1 in 30% yield. The crystal structure of 1 is discussed.     

Darstellung und Kristallstruktur von Rb2Ni3Se4

Preparation and Crystal Structure of Rb₂Ni₃Se₄ The compound Rb₂Ni₃Se₄ was synthesized by heating a mixture of rubidium carbonate, nickel and selenium at 850°C in an atmosphere of hydrogen. The compound has a golden lustre and crystallizes with the K₂Pd₃S₄-type structure; a = 10.555(3) Å, b = 27.588(6) Å, c = 6.031(6) Å, Z = 8, Fddd (No. 70). The structure can be described as a stacking of layers of the composition Rb₂Ni₃Se₄ with a stacking sequence abcd. The electrostatic part of lattice energy (MAPLE) will be discussed for compounds of the compositions A₂M₃X₄ (A K, Rb, Cs; M Ni, Pd, Pt and X S, Se).     

Zur Darstellung und Kristallstruktur von CrSO4 · 3 H2O

Preparation and Crystal Structure of CrSO₄ · 3 H₂O Evaporating a solution of Cr²⁺ in dilute sulphuric acid at 70°C light blue crystals of CrSO₄ · 3 H₂O were grown. Its x-ray powder diffraction pattern is quite similar to that of CuSO₄ · 3 H₂O. The crystal structure refinement of CrSO₄ · 3 H₂O (space group Ce, a = 5.7056(8) Å, b = 13.211(2) Å, c = 7.485(1) Å, β = 96.73(1)°, Z = 4) from single crystal data, using the parameters of the copper compound as starting values, results in a final R-value of R = 3.8%. The surrounding of the Cr²⁺ ion can be described as a strongly elongated octahedron. The basal plane of the CrO₆-octahedron consists of three hydrate oxygen atoms and one sulphate oxygen atom. The two more distant axial oxygen atoms also belong to sulphate groups. Thus they are forming chains of alterning CrO₆-octahedra and SO₄-tetrahedra along [110] and [1–10] linked via common corners. These chains are connected via sulphate groups and by bridging hydrogen bonds to a 3-dimensional network.     

Darstellung und Kristallstruktur von Diamminmagnesiumdiazid Mg(NH3)2(N3)2

Preparation and Crystal Structure of Diammin Magnesium Diazide Mg(NH₃)₂(N₃)₂ Diammin magnesium diazide was synthesized from Mg₃N₂ and NH₄N₃ in liquid ammonia and crystallized at 150 °C under autogenous atmosphere of HN₃ and NH₃ using sealed ampoules. Mg(NH₃)₂(N₃)₂ is a colorless, microcrystalline powder which can detonate above 180 °C. Caution, preparation and manipulation of Mg(NH₃)₂(N₃)₂ is very dangerous! The crystal structure was solved from powder data using the Patterson method and a Rietveld refinement was performed (Mg(NH₃)₂(N₃)₂, I 4/m, no. 87; a = 6.3519(1), c = 7.9176(2) Å; Z = 2, R(F²)= 0.1162). The crystal structure of Mg(NH₃)₂(N₃)₂ is related to that of SnF₄. It consists of planes built up from corner sharing Mg(NH₃)₂(N₃)₄ octahedra connected equatorially over their four azide bridges with the ammonia ligands being in trans position. IR data were collected and interpreted in accordance with the structural data.     

Darstellung und Kristallstruktur neuer AM2X2-Verbindungen in den Systemen Erdalkalimetall-Platinmetall-Germanium

Preparation and Crystal Structure of New AM₂X₂ Compounds in the Systems Earthalkali Metal/Platinum Metal/Germanium . Four new ternary compounds in the systems earthalkali metal/platinum metal/germanium have been prepared and characterised by single crystal X-ray investigation. BaRu₂Ge₂ crystallizes orthorhombically, space group Fddd, a=634.4(1) pm, b=1 056.5(3) pm, c=1 273,1(3) pm. SrRu₂Ge₂ (a=430.6(1) pm, c=1 030.3(2) pm), BaRh₂Ge₂ (a=418.9(5) pm, c=1 175.7(10) pm) and SrRh₂Ge₂ (a=418.3(3) pm, c=1 071.8(6) pm) crystallize in the ThCr₂Si₂-type structure (tetragonal, space group I4/mmm).     

Darstellung und Kristallstruktur von Cs4SnO3

Preparation and Crystal Structure of Cs₄SnO₃ Crystals of Cs₄SnO₃ were synthesized by reaction of SnO with elemental Cs. The compound crystallizes with the triclinic spacegroup P1 with lattice constants a = 737.61(9) pm, b = 1171.3(1) pm, c = 1199.2(1) pm, α = 66.08(3)°, β = 80.88(2)°, γ = 82.28(3)° and Z = 4. The crystal structure exhibits isolated stannate(II) ions [Sn^IIO₃]^4– of ψ-tetrahedral form. Whereas a new structure type is present, there is a close relationship with the structures of the Cs stanntates and plumbates(IV).     

Darstellung und Kristallstruktur von K3La(NH2)6

Preparation and Crystal Structure of K₃La(NH₂)₆. Single crystals of K₃La(NH₂)₆ were obtained by the reaction of the metals (3 K + 1 La) during five days at 200°C and 4000 atm NH₃ pressure. The compound crystallizes monoclinic with a = 6.74, b = 11.67, c = 7.23 Å and β = 108.1°; the space group is C2/m (No. 12). The lattice contains 2 formula units. The amide ions are arranged in a strongly distorted cubic closepacking. All cations occupy edging anion-octahedra.     

Darstellung und Kristallstruktur von HgPb2O(OH)Br3

Inhaltsübersicht. Die erstmals dargestellte Verbindung HgPb₂O(OH)Br₃ kristallisiert orthorhombisch in der Raumgruppe Aba2 (Nr. 41) mit den Gitterkonstanten a = 14,652(3) Å, b = 14,6491(8) Å, c = 7,782(2) Å und Z = 8. Die Bestimmung der Kristallstruktur mit Einkristallmethoden zeigte “isolierte”, verzerrt würfelförmige Baugruppen der Zusammensetzung [Hg₂Pb₄O₂(OH)₂]. Diese Einheiten werden von Bromidionen umhüllt. HgPb₂O(OH)Br₃ stellt damit hinsichtlich des strukturellen Aufbaus ein Bindeglied zwischen den Verbindungen [Pb₄(OH)₄](ClO₄)₄ · 2H₂O [1] und Pb₉O₄Br₁₀ [2] dar. Preparation and Crystal Structure of HgPb₂O(OH)Br₃ The new compound, HgPb₂O(OH)Br₃ was prepared and investigated by X-ray crystal structure analysis. Crystals of orthorhombic symmetry show space group Aba2 (No. 41) with lattice parameters a = 14.652(3) Å, b = 14.6491(8) Å, c = 7.782(2) Å, and Z = 8. Remarcable structural units with heterocubane skeleton were found. The [Hg₂Pb₄O₂(OH)₂] group forms a new member of the structural class between [Pb₄(OH)₄] and [Pb₈O₄] units with the relating compounds [Pb₄(OH)₄)](ClO₄)₄ · 2 H₂O [1] und Pb₉O₄Br₁₀ [2].     

Darstellung und Kristallstruktur der Verbindung Li4H2Si2O7

Zusammenfassung Die Verbindung Li₄H₂Si₂O₇ wird durch Umsetzung von Li₆Si₂O₇ mit Methanol bzw. Wasserdampf dargestellt und ihre Kristallstruktur an Hand von Einkristallaufnahmen bestimmt. Die tetragonale Elementarzelle ( ) mita=7,59₅ undc=5,06 Å enthält zwei Formeleinheiten. Die Verbindung zählt zu den Sorosilicaten, mit [Si₂O₇]-Gruppen, die gleich angeordnet sind wie in Li₆Si₂O₇. Im Gegensatz zu Li₆Si₂O₇, das die Lithiumatome teils in einer vierzähligen Lage (KZ=5) teils einer achtzähligen Lage (KZ=4) enthält, ist in der Verbindung Li₄H₂Si₂O₇ nur letztere Position mit Lithiumatonen besetzt. Die Verteilung der Wasserstoffatome wird diskutiert.

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Preparation and crystal structure of the compoundLi ₄H₂Si₂O₇

The compound Li₄H₂Si₂O₇ has been prepared by reaction of Li₆Si₂O₇ with methanol and water vapour, resp. The crystal structure has been determined by single-crystal data. The tetragonal cell ( ):a=7.59₅ andc=5.06 Å contains two formula units. The compound belongs to the soro-silicates the [Si₂O₇]-groups being arranged analogous to Li₆Si₂O₇. In contrast to Li₆Si₂O₇, containing the lithium atoms both in a 4-fold position (c.n.=5) and an 8-fold position (c.n.=4), in the compound Li₄H₂Si₂O₇ only the latter is occupied by lithium atoms. The distribution of the hydrogen atoms is discussed.

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Darstellung und Kristallstruktur von Ag2MnO4

Synthese and Crystal Structure of Ag₂MnO₄ Single crystals of Ag₂MnO₄ have been grown from aqueous solution. The crystal structure has been solved and refined using diffractometer data (Pnma, a = 999.8(2); b = 698.9(1); c = 547.4(2) pm). The mean bond-length Mn? O within the tetrahedral anions is 167.9 pm. In spite of similar lattice constants and identical space group, Ag₂MnO₄ is not isostructural to Olivine. The structural differences are discussed.     

Darstellung und Kristallstruktur von Cu2SrSnS4

Preparation and Crystal Structure of Cu₂SrSnS₄ Cu₂SrSnS₄ was prepared from a mixture of the three binary sulfides at 620-700° C. The structure analyses by single crystal X-ray investigations yields a trigonal C-symmetrie for the unit of the structure with a = 6.29₀ and c = 15.57₈ Å and three formula units. Space group: C–P3₁ (No. 144). Copper and tin have tetrahedral surrounding of S^2?. The neighbourhood of Sr²⁺ has the shape of a deformed archimedic antiprisma.     

Darstellung und Kristallstruktur von (CH3NH3)8[NdCl6][NdCl4(H2O)2]2Cl3

Preparation and Crystal Structure of (CH₃NH₃)₈[NdCl₆][NdCl₄(H₂0)₂]₂Cl₃ (CH₃NH₃)₈[NdCl₆][NdCl₄ (H₂O)₂]₂Cl₃ is for the first time prepared and investigated by X-ray, single crystal work. It crystallizes in the monoclinic system (space group C2/m, Z = 2) with a = 9.358(5), b = 17.424(9), c = 15.360(8) Å, β = 108.30(4)°. The structure contains besides isolated Cl^? ions distorted [NdCl₆]^3? octahedra and [NdCl₄(H₂O)₂]^? chains.     

Darstellung und Kristallstruktur von Barium-Cadmium-Thiostannat (iv) BaCdSnS4

Preparation and Crystal Structure of Barium-Cadmium-Thiostannate (IV) BaCdSnS₄ BaCdSnS₄ was prepared for the first time and the crystal structure determined by single crystal X-ray investigations. Lattice constants: a = 2186 ± 2; b = 2169 ± 1; c = 1318 ± 0.5 pm. Space group: C–Fdd2. There are pairs of edge-sharing tetrahedrons linked together characteristically to form twodimensional endless nets. The crystal structure is described and discussed.     

Darstellung und Kristallstruktur von Tl2PdCl4

Synthesis and Crystal Structure of Tl₂PdCl₄ Single crystals of Tl₂PdCl₄ can be obtained by hydrothermal synthesis [1, 2]. They show tetragonal symmetry with space group P4/mmm (No. 123). The lattice parameters are a = 7.163(1) Å and c = 4.282 (1) Å. The atomic arrangement of Tl₂PdCl₄ is explored by X‐ray crystal structure analysis. Tl₂PdCl₄ is isotypic with K₂PtCl₄.