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.     

Zur Kristallstruktur von SrZn(OH)4 · H2O

Crystal Structure of SrZn(OH)₄ · H₂O Colorless crystals of SrZn(OH)₄ · H₂O are obtained by electrochemical oxidation of Zn in a zinc/iron pair in an aqueous ammonia solution saturated with strontium hydroxide. The X-ray crystal structure determination was now successful including all hydrogen positions: P1 , Z = 2, a = 6.244(1) Å, b = 6.3000(8) Å, c = 7.701(1) Å, α = 90.59(1)°, β = 112.56(2)°, γ = 108.66(2)°, N(F ≥ 3σF) = 1967, N(Var.) = 84, R/R_w = 0.020/0.024. In SrZn(OH)₄ · H₂O Zn²⁺ is tetrahedrally coordinated by four OH^? -ions while Sr²⁺ has 6 OH^? and one H₂O as neighbours. The polyhedra around Sr²⁺ are connected to chains which are linked three-dimensionally by isolated tetrahedra [Zn(OH)₄]. Hydrogen bonds between H₂O as donor and OH^? are characterized by raman spectroscopy.     

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°.     

Synthese und Kristallstruktur eines Natrium-tetraoxonitridowolframats(VI), Na5WO4N

Synthesis and Crystal Structure of Sodium Tetraoxo Nitrido Tungstate(VI), Na₅WO₄N Colourless crystals of Na₅WO₄N are obtained besides Na₄WO₂N₂ [1] by the reaction of WO₃ with NaNH₂ (15:1) at 350°C ≥ T ≥ 750°C in autoclaves to prevent early decomposition of sodium amide. X-ray single crystal investigations are characterized by the following data:

• Na₅WO₄N: Cmc2₁ (No. 36), Z = 4
• a = 9.873(2) Å, b = 5.769(1) Å, c = 10.648(2) Å
• Z(F)≥ 3σ(F) = 2182, Z(Var.) = 55, R/R_w = 0.029/0.039

The structure contains the tetragonal pyramidal ion WO₄N^5? with nitrogen at the apex connected via Na⁺ ions irregularly coordinated by one nitrogen and four oxygen atoms of different anions.     

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,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 Struktur neuer Natriumhydrogensulfate Na(H3O)(HSO4)2; Na2(HSO4)2(H2SO4) und Na(HSO4)(H2SO4)2

Synthesis and Structure of New Sodium Hydrogen Sulfates Na(H₃O)(HSO₄)₂, Na₂(HSO₄)₂(H₂SO₄), and Na(HSO₄)(H₂SO₄)₂ Three acidic sodium sulfates have been synthesized from the system sodium sulfate/sulfuric acid and have been crystallographically characterized. Na(H₃O)(HSO₄)₂ ( A ) crystallizes in the space group P2₁/c with the unit cell parameters a = 6.974(2), b = 13.086(2), c = 8.080(3) Å, α = 105.90(4)°, V = 709.1 Å3, Z = 4. Na₂(HSO₄)₂(H₂SO₄) ( B ) is orthorhombic (space group Pna2₁) with the unit cell parameters a = 9.970(2), b = 6.951(1), c = 13.949(3) Å, V = 966.7 ų and Z = 4. Na(HSO₄)(H₂SO₄)₂ ( C ) crystallizes in the triclinic space group P1 with the unit cell parameters a = 5.084(1), b = 8.746(1), c = 11.765(3) Å, α = 68.86(2)°, β = 88.44(2)°, γ = 88.97(2)°, V = 487.8 Å3 and Z = 2. All three compounds contain SO₄ tetrahedra as HSO₄^? anions and additionally in B and C in form of H₂SO₄ molecules. The ratio H:SO₄ determines the connectivity degree in the hydrogen bond system. In A , there are zigzag chains and dimers additionally connected via oxonium ions. Complex chains consisting of cyclic trimers (two HSO₄^? and one H₂SO₄) are present in B . In structure C , several parallel chains are connected to columns due to the greater content of H₂SO₄. Sodium cations show a distorted octahedral coordination by oxygen in all three structures, the NaO₆ octahedra being “isolated” (connected via SO₄ tetrahedra only) in A . Pairs of octahedra with common edge form Na₂O₁₀ dimeric units in C . Such double octahedra are connected via common corners forming zigzag chains in B .     

Na5Br(OH)4: Darstellung und Kristallstruktur einer Verbindung im System NaOH/NaBr

Na₅Br(OH)₄: Synthesis and Structure of a Compound in the System NaOH/NaBr The pseudobinary system NaOH/NaBr is investigated by X-ray methods. The structure of the compound Na₅Br(OH)₄ was solved by single crystal data: Na₅Br(OH)₄: Pnma, Z = 8, a = 11.846(2) Å, b = 18.782(4) Å, c = 6.431(1) Å, Z(F_o) = 1 202 with (F_o)² ≥ 3σ(F_o)², Z(parameter) = 100, R/R_w = 0.030/0.035 The compound crystallizes in a new type of structure. Pairs of octahedra around O by 5 Na and 1 H to [Na₅(OH)]₂ are orientated in such a way to one another that two ions OH^? form a parallelogram hinting to unusual bent hydrogen bridge bonding.     

Synthese,Kristallstruktur und Magnetismus von Natriumtetrachlorotitanat(II), Na2TiCl4

Synthesis, Crystal Structure and Magnetism of Sodium Tetrachlorotitanate(II), Na₂TiCl₄ Na₂TiCl₄ is obtained as single crystals by metallothermic reduction of TiCl₃ with sodium (525°C, 90 d, Ta container). Pure powder samples may be prepared by synproportionation of TiCl₃ with Ti in the presence of NaCl (950–520°C, 21 d). The structure refinement from four-circle diffractometer data confirms that Na₂TiCl₄ is isotypic with Sr₂PbO₄ (orthorhombic, space group Pbam (No. 55), Z = 2 a = 694.2(1), b = 1 198.9(2), c = 385.6(1) pm, R = 0.055, R_w = 0,038). Ti²⁺ is surrounded by a distorted octahedron of Cl^?. The octahedra are connected via common edges to chains, [TiCl_2/1Cl_4/2]^2?, that run in the [001] direction. Magnetic susceptibility data were recorded in the 2 to 300 K temperature range at various field strengths. The interpretation of the data was carried out with the aid of crystal-field calculations taking magnetic interactions into account. The non-Curie behaviour of the reciprocal magnetic susceptibility of Ti²⁺ in Na₂TiCl₄ is due to the influence of spin-obit coupling.     

Darstellung und Reaktionen von Natriumtellurid,Na2Te – Kristallstruktur von [Na(CH3OH)3]2Te2

Preparation and Reactions of Sodium Telluride, Na₂Te – Crystal Structure of [Na(CH₃OH)₃]₂Te₂ Sodium telluride, Na₂Te 1 , is easily obtained by reaction of sodium with hexagonal tellurium in 1,2-dimethoxy-ethane in the presence of catalytic amounts of naphthalene. Upon exposure to oxygen 1 reacts with methanol forming [Na(CH₃OH)₃]₂Te₂ 2 , which crystal structure was determined. Compound 1 , prepared in situ, can be conveniently converted into dialkyl tellurides, R₂Te (R = C₂H₅, i-C₃H₇, CH₂ = CH? CH₂ 3 ).     

Synthese und Kristallstruktur von Na10[P4(NH)6N4](NH2)6(NH3)0,5 mit dem adamantanartig aufgebauten Anion [P4(NH)6N4]4−

Synthesis and Crystal Structure of Na₁₀[P₄(NH)₆N₄](NH₂)₆(NH₃)_0.5 with an Adamantane-like Anion [P₄(NH)₆N₄]^4? Crystals of Na₁₀[P₄(NH)₆N₄](NH₂)₆(NH₃)_0.5 were obtained by the reaction of P₃N₅ with NaNH₂ (molar ratio 1:20) within 5 d at 600°C in autoclaves. The following data characterize X-ray investigations: Fm3 m, Z = 8, a = 15.423(2) Å, Z(F) = 261 with F ≥ 3 σ(F) Z(Variables) = 27, R/R_w = 0.086/0.089 The compound contains the hitherto unknown anion [P₄(NH)₆N₄]^4?, which resembles adamantane. The total structure can be described as follows: The centers of gravity of units of [Na₈(NH₂)₆(NH₃)]²⁺ – 8Na⁺ on the corners of a cube, 6NH₂^? on the ones of an inscribed octahedron with NH₃ in the center – follow the motif of a cubic-closest packed arrangement. Units of [Na₁₂(NH₂)₆]⁶⁺ – 12Na⁺ on the corners of a cuboctahedron and 6NH₂^? on the ones of an inscribed octahedron – occupy all octahedral and those of [P₄(NH)₆N₄]^4? all tetrahedral sites.     

Zur Synthese und Kristallstruktur der ternären Carbide Na2PdC2 und Na2PtC2

Syntheses and Crystal Structures of Ternary Carbides Na₂PdC₂ and Na₂PtC₂ Na₂PdC₂ and Na₂PtC₂ were synthesized by the reaction of sodium carbide with palladium and platinum respectively. The crystal structures could be solved from X-ray powder diffraction data (space group: P3 m1, Z = 1). Both compounds crystallize in a new structure type with [M(C₂)_2/2^2?] chains (M?Pd, Pt) as the characteristic structural unit. The existence of a C? C triple bond was confirmed by Raman spectroscopy.     

Synthese und Kristallstruktur von [{(tBu2P)2InCl}2]

Synthesis and Crystal Structure of [{(tBu₂P)₂InCl}₂] The reaction of InCl₃ with tBu₂PSiMe₃ leads to [{(tBu₂P)₂InCl}₂] ( 1 ). 1 crystallizes in the space group P2₁/c. The lattice constants (at 216 K) are: a = 945.9(5) pm, b = 1 604.1(9) pm, c = 1 636.8(8) pm, β = 100.55(4)°. 1 contains a planar In₂P₂ ring. Each In atom is coordinated by two bridging tBu₂P groups, a terminal tBu₂P group and a terminal Cl atom. The coordination geometry of the In atoms is roughly tetrahedral.     

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,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.     

Methanol als Ligand in Natriumphenolat: Darstellung und Struktur von [Na(CH3OH)4][OC6H5]

Methanol as a Ligand in Sodium Phenoxide: The Synthesis and Crystal Structure of [Na(CH₃OH)₄][OC₆H₅] By the reaction of sodium and phenol in N-methyl-?-caprolactam (NMC) sodium phenoxide has been yielded, which forms a complex with the furthermore obtained methanol of [Na(CH₃OH)₄][OC₆H₅]. The single crystals crystallize triclinic, space group P1 , with the lattice constants a = 6.613(3) Å, b = 10.537(4) Å, c = 10.656(4) Å, α = 108.27(2)°, β = 98.21(2) and γ = 95.26(2)°. Sodium is coordinated by six oxygen atoms of methanol in the form of an octahedron. These coordination polyhedrons are connected by sharing edges forming chain, whereas, the oxygen of phenoxide is not involved in the coordination of sodium. Although it is attached to the chain by hydrogen bonding.     

Synthese und Kristallstruktur von Ba25Cu142+Cu43+Zn4O49

Synthesis and Crystal Structure of Ba₂₅Cu₁₄²⁺Cu₄³⁺Zn₄O₄₉ Single crystals of Ba₂₅Cu₁₄²⁺Cu₄³⁺Zn₄O₄₉ were prepared with solid state and flux reactions. X-ray investigations show tetragonal symmetry, space group D⁷_4th–P4/nmm, a = 18.2146, c = 9.3230 Å, Z = 2. The hitherto unknown structure type shows copper in square pyramids and planar polygones, connected to six member rings or Cu₅O₂₀ groups. Slightly bent Cu₅O₁₂ groups produced by edge connection of five CuO₄ polygones are connected with ZnO₄ tetrahedra forming Cu₅Zn₄O₂₀ units. The complicated structure is shown step by step.     

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 KMgCu4V3O13

Synthesis and Crystal Structure of KMgCu₄V₃O₁₃ . Single crystals of KMgCu₄V₃O₁₃ were prepared by supercooled melts. It crystallizes with monoclinic symmetry space group C–P2₁/m (Nr. 11), unit cell dimensions: a = 10.7144 Å, b = 6.0282 Å, c = 8.3365 Å, β = 98.075°, Z = 2. The crystal structure is closely related to the BaMg₂Cu₈O₆O₂₆ type. Cu²⁺ occurs in an unusual trigonal bipyramidal coordination.