Synthese und Kristallstruktur von (PPh4)2Se6

Synthesis and Crystal Structure of (PPh₄)₂Se₆ (PPh₄)₂Se₆ has been prepared by the reaction of selenium with K₂Se₂ in dimethylformamide solution in the presence of K₃[Mn(CN)₆] and PPh₄Br, forming black crystal needles. According to the crystal structure determination the compound consists of PPh⁺₄ ions and chainlike hexaselenide ions. Space group P6 , Z = 2,4683 Observed unique reflections, R = 0.066. Lattice dimensions at ?90°C: a = 951.0, b = 1094.8, c = 2137.4 pm, α = 82.66°, β = 83.36°, γ = 89.96°.     

[Na(12-Krone-4)2]2[Ni(Se4)2] · DMF; Synthese,Kristallstruktur und magnetisches Verhalten

[Na(12-Crown-4)₂]₂[Ni(Se₄)₂] · DMF; Synthesis, Crystal Structure, and Magnetic Behaviour The title compound has been prepared from NiCl₂ and sodium polyselenide in dimethylformamide solution in the presence of 12-crown-4, forming black crystal needles. They were characterized by an X-ray structure determination, by FIR spectroscopy as well as by the magnetic behaviour. [Na(12-crown-4)₂]₂[Ni(Se₄)₂] · DMF crystallizes monoclinically in the space group P2₁, 3650 observed unique reflections, R = 0.046. Lattice dimensions at ?80°C: a = 1020.3(2); b = 1889.5(2); c = 1498.7(3) pm; β = 108.29(1)°. The compound has an ionic structure, in which the sodium atoms of the [Na(12-crown-4)₂]⁺ cations are coordinated by the oxygen atoms of the crown ether molecules in an antiprismatic fashion. The nickel atom of the anion [Ni(Se₄)₂]^2? is surrounded by four selenium atoms of the tetraselenide chelates in an almost planar environment. The DMF molecules are inserted in the lattice without a bonding interaction. The magnetic susceptibility observed in the temperature interval 4.2 to 330K can be interpreted by means of a ³E ground term and D₂ as local symmetry, which was established by X-ray crystallography.     

Synthese und Kristallstruktur von [Fe(MeCN)6][Fe2OCl6]

Synthesis and Crystal Structure of [Fe(MeCN)₆][Fe₂OCl₆] [Fe(MeCN)₆][Fe₂OCl₆] ( 2 ) is obtained by passing dry air through a solution of FeCl₂ in acetonitrile in almost quantitative yield. 2 crystallises in the trigonal space group R 3 [a = b = 12.121(1), c = 29.875(6) Å, Z = 6]. The oxygen atom in the Fe₂OCl₆ anion occupies the 3 position and causes therefore an Fe–O–Fe angle of 180°. The refinement in the triclinic space group P1 leads to a slightly bent arrangement of the Fe–O–Fe fragment.     

Synthese und Kristallstruktur von [Na(12-Krone-4)2]2[Hg(Se4)2] · 1,5 DMF

Synthesis and Crystal Structure of [Na(12-Crown-4)₂]₂[Hg(Se₄)₂] · 1.5 DMF . The title compound has been prepared by the reaction of Na₂Se₄ with mercury acetate in DMF solution in the presence of 15-crown-5, forming dark red crystal needles. [Na(12-crown-4)₂]₂[Hg(Se₄)₂] · 1.5 DMF crystallizes in the space group C2/c with eight formula units per unit cell. The structure was determined with 3 824 observed unique reflections, R = 0.085. Lattice dimensions at - 70°C: a = 2 884(2), b = 1 407.7(7), c = 2 843(2) pm, β = 93.93(5)°. The structure consists of [Na(12-crown-4)₂]⁺ ions with a sandwichlike coordination of the crown ether molecules, and of [Hg(Se₄)₂]^2? ions, in which the mercury atom is coordinated by two tetraselenido ions in a chelating fashion. The [Hg(Se₄)₂]^2? ions are arranged to infinite chains via Se…?Se contacts.     

Synthese,Kristallstruktur und 121Sb-Mößbauer-Spektrum von [SbCl2(18-Krone-6)]+SbCl6−

Synthesis, Crystal Structure, and ¹²Sb-Mössbauer Spectrum of [SbCl₂(18-Crown-6)]⁺SbCl₆^? The title compound, which has been prepared by the reaction of antimony trichloride and antimony pentachloride in the presence of 18-crown-6 in acetonitrile solution, is characterized by its ¹²¹Sb-Mössbauer spectrum and by an X-ray structure determination. Space group P2₁, Z = 2, 2439 observed unique reflections, R = 0.045, wR = 0.043. Lattice dimensions at ?80°C: a = 780.6(7), b = 1297.5(9), c = 1 278.5(10) pm, β = 100.56(7)°. The structure of [SbCl₂(18-crown-6)]⁺SbCl₆^? contains cations in which the antimony atom in the first coordination sphere is surrounded in a ?-trigonal-bipyramidal fashion by two oxygen atoms of the crown ether in axial position as well as in the equatorial position by the two chlorine atoms and the lone electron pair.     

Synthese und Kristallstruktur von Sr2Zn(OH)6 und Ba2Zn(OH)6

Synthesis and Crystal Structure of Sr₂Zn(OH)₆ and Ba₂Zn(OH)₆ Crystallization from supersaturated sodium hydroxozincate solutions by adding solutions of alkali earth metal hydroxides yields crystals of Sr₂Zn(OH)₆ and Ba₂Zn(OH)₆. The X-ray structure determination on these crystals was successful including all hydrogen positions: Sr₂Zn(OH)₆: P2₁/n, Z = 2, a = 5.794(1) Å, b = 6.160(1) Å, c = 8.141(1) Å, b = 91.23(1)°, N(F ³° 2σ F) = 1127, N(Var.) = 53, R₁/wR₂ = 0.047/0.081Ba₂Zn(OH)₆: P2₁/n, Z = 2, a = 6.043(1) Å, b = 6.336(1) Å, c = 8.451(2) Å, b = 91.23(2)°, N(F ° 2σ F) = 1669, N(Var.) = 54, R₁/wR₂ = 0.029/0.067. Sr₂Zn(OH)₆ and Ba₂Zn(OH)₆ crystallize isotypic in a distorted Li₂O structure type. Sr²⁺ resp. Ba²⁺ form a cubic primitive arrangement. Distorted octahedra of OH^– around Zn²⁺ fill therein alternating cubic gaps in an ordered way.     

[Na(15-Krone-5)][ReFCl3(NO)(CH3CN)] Synthese,IR-Spektrum und Kristallstruktur

[Na(15-crown-5)][ReFCl₃(NO)(CH₃CN)] Synthesis, IR Spectrum, and Crystal Structure The title compound has been prepared by the reaction of [ReCl₃(NO)₂(CH₃CN)] with the equivalent amount of sodium fluoride in the presence of 15-crown-5 in boiling acetonitrile, forming blue crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. Space group P2₁/n, Z = 4,2117 observed independent reflections, R = 0.037, wR = 0.029. Lattice dimensions at 20°C: a = 834.0(2), b = 1600.0(3), c = 1670.0(3) pm; β = 104.19(3)°. The compound forms an ion pair via one Na F contact of 234.4 pm and one Na Cl contact of 293.4 pm; the nitrosyl ligand ist in trans-position to the F atom of the anion [ReFCl₃(NO)(CH₃CN)]⁻.     

Darstellung und Kristallstruktur von [Li(DME)2I]

Synthesis and Crystal Structure of [Li(DME)₂I] . LiI can be dissolved at 50°C in toluene/DME (2:1). At - 20°C [Li(DME)₂I] ( 1 ) was isolated in 75% yield. 1 was characterized by NMR techniques as well as an X-Ray structure determination. 1 crystallizes in the space group C2/c with a = 1 356.9(2), b = 813.2(1), c = 1 259.1(2) pm, and β = 99.74(1)°.     

Kationische und anionische kantenverknüpfte Dimere in [Dy2(Dibenzo-18-Krone-6)2Cl4][Dy2(CH3CN)2Cl8]. Synthese und Kristallstruktur

Cationic and Anionic Edge-Connected Dimers in [Dy₂(dibenzo-18-crown-6)₂Cl₄][Dy₂(CH₃CN)₂Cl₈]. Synthesis and Crystal Structure Colourless single crystals of 2 DyCl₃ · dibenzo-18-crown-6 · CH₃CN are obtained upon reaction of DyCl₃ or KDy₂Cl₇ with dibenzo-18-crown-6-ether in acetonitrile. The crystal structure (triclinic, P1 , Z = 2; a = 1 105.6(2); b = 1 144.5(3); c = 1 367.8(3); α = 93.46(1); β = 92.27(1); γ = 117.45(1); R = 0.046; R_w = 0.033) contains cationic and anionic edge-connected dimers according to [Dy₂(dibenzo-18-crown-6)₂Cl₄]²⁺ [Dy₂(CH₃CN)₂Cl₈]²⁺ where Dy1 and Dy2 are coordinated by 3 and 5 chloride ions, respectively.     

Synthese und Kristallstruktur von LiAl[(P2O6)2]

Synthesis and Crystal Structure Determination of LiAl[(P₂O₆)₂] Single crystals of previously unknown LiAl[(P₂O₆)₂] have been obtained by reaction of Li₂CO₃, Al₂O₃ and H₃PO₄ (1:1:16) at 350°C. The title compound crystallizes in Pbcn (a = 1 244.54(1), b = 823.40(1), c = 892.46(1) pm; Z = 4). The least-squares refinement (with anisotropic temperature factors) was performed using 766 observed reflections yielding R = 0.029 and R(w) = 0.075. Four anion chains are running parallel to the shortest axis in the unit cell, the period of identity amounting to four. Aluminium is surrounded by an almost regular octahedron, lithium by a distorted tetrahedron of oxygen.     

Synthese und Kristallstruktur des tetrameren Nitridokomplexes [Cu(CH3CN)4]2[W4N4Cl14(CH3CN)2]

Synthesis and Crystal Structure of the Tetrameric Nitrido Complex [Cu(CH₃CN)₄]₂[W₄N₄Cl₁₄(CH₃CN)₂] . The title compound has been prepared by the reaction of CuCl with WNCl₃ in acetonitrile solution, forming red, moisture sensitive crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. Space group I2/a, Z = 4, 2 027 observed unique reflections, R = 0.049. Lattice dimensions at -80°C: a = 2 527.0, b = 971.9, c = 2 137.5 pm, β = 106.01°. The compound consists of [Cu(CH₃CN)₄]⁺ ions, which are arranged to form strands, and of anions [W₄N₄Cl₁₄(CH₃CN)₂]^2?, in which the tungsten atoms were located at the vertices of a square and are linked with one another via linear W?N? W bridges. Two of the four tungsten atoms have four chlorine atoms as terminal ligands, the other two tungsten atoms have three chlorine atoms and an acetonitrile molecule as terminal ligands.     

Synthese und Kristallstruktur von [Na(15-Krone-5)]4[Cd4Te12] · 8 DMF

Synthesis and Crystal Structure of [Na(15-Crown-5)]₄[Cd₄Te₁₂] · 8 DMF The title compound has been prepared by reaction of Na₂Te₃ with cadmium acetate in DMF solution in the presence of 15-crown-5, forming black crystal needles, which were characterized by an X-ray structure determination. Space group P2₁/n, Z = 2, 5 716 observed unique reflections, R = 0.038. Lattice dimensions at ?50°C: a = 1 622.9, b = 2 038.2, c = 1 739.8 pm, β = 92.26°. The compound has an ionic structure. The cations [Na(15-crown-5)(DMF)]⁺ and [Na(15-crown-5) · (DMF)₂]⁺ together with two further DMF molecules form tetrameric units. In the centrosymmetric anions [Cd₄Te₁₂]^4? the cadmium atoms are linked by μ₂-Te^2?-, μ₄-Te₂^2?-, and μ₂-Te₃^2?-units.     

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 Ba6Lu4Zn10O22 mit [OBa6]-Oktaedern

On the Synthesis and Crystal Structure of Ba₆Lu₄Zn₁₀O₂₂ with [OBa₆] Octahedra Single crystals of Ba₆Lu₄Zn₁₀O₂₂ have been prepared by high temperature reactions and investigated by X-ray techniques. This compound is isotypic to Ba₃In₂Zn₅O₁₁ and the first member of the Rare Earth elements. Ba₆Lu₄Zn₁₀O₂₂ crystallizes with cubic symmetry, space group T-F4 3m, a = 13.452(1) Å and Z = 4. Zn²⁺ shows a tetrahedral, Lu³⁺ an octahedral and Ba²⁺ a three-fold capped trigonal prismatic coordination by O^2?. The ZnO₄ tetrahedra and LuO₆ octahedra are forming macro polyhedra of the type Zn₁₀O₂₀ and Lu₄O₁₆. A discussion is given for the Ba₆O₃₃ and Ba₆O₄₂ groups.     

Synthese und Kristallstruktur von [Cr(NH3)6][Cr(NH3)2F4][BF4]2

Synthesis and Crystal Structure of [Cr(NH₃)₆][Cr(NH₃)₂F₄][BF₄]₂ The action of ammonium fluoride on a mixture of boron and chromium in a sealed Monel ampoule at 300 °C yields single crystals of [Cr(NH₃)₆][Cr(NH₃)₂F₄][BF₄]₂. The crystal structure (tetragonal, P4/mbm, Z = 2, a = 1056.0(1), c = 781.7(1) pm; R₁ = 0.0414; wR₂ = 0.1087 for 411 reflections with I₀ > 2σ(I)) contains [Cr(NH₃)₆]³⁺ and [Cr(NH₃)₂F₄]^– octahedra and twice as many [BF₄]^– tetrahedra that are arranged in a quadrupled super‐structure of the CsCl‐type of structure.     

Synthese,Kristallstruktur und spektroskopische Charakterisierung von Tetraphosphorhexaoxiddiselenid P4O6Se2

Synthesis, Crystal Structure, and Spectroscopic Characterization of Tetraphosphorus Hexaoxide Diselenide P₄O₆Se₂ P₄O₆Se₂ has been prepared by photochemical selenation of P₄O₆ with red selenium in CS₂ in presence of catalytical amounts of iodine. Isolation and single crystal growth were performed by fractional crystallization and subsequent sublimation. The compound crystallizes in the monoclinic space group P2₁/c (Nr. 14) with a = 11.473(2); b = 6.536(1); c = 11.796(2) Å; β = 90.06(1)°; Z = 4; R₁ = 0.030; wR² = 0.073. Within the limits of experimental error, the P₄O₆Se₂ molecules exhibit C_2v symmetry in the crystal. Bond lengths and angles within the molecule as well as the arrangement of the molecules within the crystal are discussed; IR-, Raman-, and ³¹P solution NMR data are reported.     

Kronenetherkomplexe von Blei(II). Die Kristallstrukturen von [PbCl(18-Krone-6)][SbCl6], [Pb(18-Krone-6)(CH3CN)3][SbCl6]2, and [Pb(15-Krone-5)2][SbCl6]2

Crown Ether Complexes of Lead(II). The Crystal Structures of [PbCl(18-Krone-6)][SbCl₆], [Pb(18-Krone-6)(CH₃CN)₃][SbCl₆]₂ und [Pb(15-Krone-5)₂][SbCl₆]₂ . [PbCl(18-crown-6)][SbCl₆] has been prepared in low yield besides [Pb(CH₃)₂(18-crown-6)][SbCl₆]₂ by the reaction of Pb(CH₃)₂Cl₂ with antimony pentachloride in acetonitrile solution in the presence of 18-crown-6, forming pale-yellow crystals. The other two title compounds are formed as colourless crystals by the reaction of PbCl₂ with antimony pentachloride in acetonitrile solutions in the presence of 18-crown-6 and 15-crown-5, respectively. The complexes were characterized by IR spectroscopy and by crystal structure determinations. [PbCl(18-crown-6)][SbCl₆]: Space group P2₁/c, Z = 8, 5 003 observed unique reflections, R = 0.046. Lattice dimensions at - 80°C: a = 1 386.9; b = 1 642.7; c = 2 172.1 pm, β = 92.95°. The lead atom in the cation [PbCl(18-crown-6)]⁺ is surrounded in an almost hexagonal-planar construction by the six oxygen atoms of the crown ether and an axially oriented Cl atom. [Pb(18-crown-6)(CH₃CN)₃][SbCl₆]₂: Space group P1 , Z = 2, 6 128 observed unique reflections, R = 0.076. Lattice dimensions at - 70°C: a = 1 228.0; b = 1 422.9; c = 1 463.2 pm, α = 69.08°; β = 65.71°; γ = 64.51°. In the cation [Pb(18-crown-6)(CH₃CN)₃]²⁺ the lead atom is coordinated by the six oxygen atoms of the crown ether and by the three nitrogen atoms of the acetonitrile molecules. The structure determination is restricted by disorder. [Pb( 15-crown-5)₂][SbCI₆]₂: Space group P6₃/m, Z = 6, 5 857 observed unique reflections, R = 0.059. Lattice dimensions at -70°C: a = b = 2 198.5; c = 1499.4 pm, α = β = 90°, γ = 120°. In the cation [Pb(l5-crown-5)₂]² the lead atom is sandwich-like coordinated by the ten oxygen atoms of the two crown ether molecules. The structure determination is restricted by disorder.     

Die Kristallstrukturen der Polyselenide [Cs(18-Krone-6)]2Se5 · DMF, [Rb(222-Crypt)]2Se6, [Ba(15-Krone-5)2]Se6 · DMF und [Na(12-Krone-4)2]2Se7

Crystal Structures of the Polyselenides [Cs(18-Crown-6)]₂Se₅ · DMF, [Rb(222-Crypt)]₂Se₆, [Ba(15-Crown-5)₂]Se₆ · DMF, and [Na(12-Crown-4)₂]Se₇ . The title compounds have been prepared by reactions of the corresponding diselenides with excess selenium in the presence of crown ethers in dimethylformamide solutions, forming black crystals. [Cs(18-Crown-6)]₂Se₅ · DMF: Space group P2₁/m, Z = 2, 2 194 observed unique reflections, R = 0.119. Lattice dimensions at 20°C: a = 1 041.2; b = 1 496.3; c = 1 459.7 pm; β = 100.39°. The compound forms an ionic triple with Cs…Se-contacts between 374 and 381 pm. [Rb(222-Crypt)]₂Se₆: Space group P1 , Z = 2, 7 405 observed unique reflections, R = 0.056. Lattice dimensions at – 70°C: a = 1 106.8; b = 1 460.8; c = 1 718.8 pm; α = 89.22°; β = 86.65°; γ = 71.53°. The compound contains Se₆^2? chains without direct contact with each other. [Ba(15-Crown-5)₂]Se₆ · DMF: Space group P2₁/n, Z = 4, 2 680 observed unique reflections, R = 0.055. Lattice dimensions at – 80°C: a = 1 051.9; b = 1 322.4; c = 2 729.9 pm; β = 100.93°. The compound contains Se₆^2? chains, which are isolated from each other by the cations and the included DMF molecules. [Na(12-Crown-4)₂]₂Se₇: Space group P1 , Z = 2, 7 313 observed unique reflections, R = 0.042. Lattice dimensions at – 70°C: a = 1 260.9; b = 1 433.6; c = 1 462.9 pm; α = 80.27°; β = 78.60°; γ = 69.34°. The compound contains Se₇^2? chains without direct contacts with each other.     

Synthese und Kristallstruktur von [N(Hex)4][Cu2(CN)3]

Synthesis and Crystal Structure of [N(Hex)₄] [Cu₂(CN)₃] [N(Hex)₄][Cu₂(CN)₃] has been prepared by solvothermal reaction of CuCN with Tetra‐n‐hexylammoniumiodide in acetone. The crystal structure is built up by condensed (CuCN)₆ and (CuCN)₇ rings, forming a zeolith type cyanocuprate(I) framework [Cu₂(CN)₃^—]. Space group R3; α = 44.482(6), c = 21.283(4) Å, V = 36471(9) ų; Z = 9.     

Synthese und Kristallstruktur von Rb8[P4N6(NH)4](NH2)2 mit dem adamantanartigen Anion [P4N6(NH)4]6−

Synthesis and Crystal Structure of Rb₈[P₄N₆(NH)₄](NH₂)₂ with the Adamantane-like Anion [P₄N₆(NH)₄]^6? RbNH₂ reacts with P₃N₅ (molar ratio 6:1) at 400°C within 5 d to colourless Rb₈[P₄N₆(NH)₄](NH₂)₂. Suitable crystals for a X-ray structure determination were obtained: The compound contains adamantane-like molecular anions [P₄N₆(NH)₄]^6?. Their centres of gravity are arranged in a distorted hexagonal primitive array. All trigonal prisms of this array contain one amide ion. Rubidium ions connect the anions irregularly.