Darstellung,Kristallstruktur und Eigenschaften von Kaliumhydrogencyanamid

Preparation, Crystal Structure, and Properties of Potassium Hydrogen Cyanamide For the preparation of KHCN₂ melamine has been reacted with potassium amide in liquid ammonia. After evaporation of the solvent the resulting solid has been transformed at 210°C. KHCN₂ (P2₁2₁2₁, a = 708.7(2), b = 909.0(2), c = 901.4(2) pm, Z = 8, R = 0.039, wR = 0.016) is yielded as a coarse crystalline product. In the solid K⁺ and HCN ions occur. As expected two significantly differing bond-distances C? N (117.3(5) pm) and HN? C (128.7(5) pm) have been found in the anion. According to IR-spectroscopy a non linear group N? C? N (174.4(4)°) is observed.     

Darstellung,Kristallstruktur und magnetische Eigenschaften von In2Ni21B6

Preparation, Crystal Structure, and Magnetic Properties of In₂Ni₂₁B₆ In₂Ni₂₁B₆ was prepared by solid state reaction of the elements at 1223 K. The single‐crystals, obtained for the first time, exhibit metallic luster and crystallize in space group Fm 3 m (a = 1059.11(2) pm; Z = 4; 128 symmetry independent reflections; R1 = 0.027; wR2 = 0.125). In₂Ni₂₁B₆ is related to the Cr₂₃C₆‐structure and belongs to the structural family of τ‐borides. The compound melts at 1426 K. Polycrystalline samples of In₂Ni₂₁B₆ are ferromagnetic with a Curie‐Temperature of T_C = 596 K and show metallic conductivity in the range from 12 K to 320 K.     

Darstellung und Kristallstruktur von NaBi2AuO5

Synthesis and Crystal Structure of NaBi₂AuO₅ NaBi₂AuO₅ was obtained by hydrothermal reaction of ‘Bi₂O₅’, Au₂O₃ · 2H₂O and saturated aqueous NaOH solution at temperatures from 300 to 600°C and oxygen pressure from 3 × 10⁸ to 6 × 10⁸ Pa for the first time. The crystal structure (P4 b2; a = 1 220.02(6) pm; b = 386.68(3) pm; Z = 4; R_w = 0.022) consists of bisphenoidic distorted AuO₄ groups, which are stacked in c-direction. They are connected by square pyramidal BiO₅ units. Sodium is occupying holes within the Au/Bi/O framework thus formed.     

Darstellung und Kristallstruktur von CsBO2

Preparation and Crystal Structure of CsBO₂ Colourless single crystals of CsBO₂ have been prepared from intimate mixtures of CsO_0.57 and B₂O₃ (Cs:B = 3.2:1.0; 600°C, 38 d). The structure determination from fourcircle diffractometer data (MoK, 443 I_o (h k l), R = 3.1%, R_w = 2.0%) confirms the isotypy with NaBO₂ and KBO₂: space group R 3 c; a = 1 363.7(2) pm, c = 836.5(2) pm; Z = 18. A characteristic structure unit is the planar cyclic anion [B₃O₆]^3?. Effective Coordination Numbers (ECoN), Mean Fictive Ionic Radii (MEFIR), the Madelung Part of Lattice Energy (MAPLE) and the Charge Distribution (CHARDI) are calculated and 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).     

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.     

Darstellung,Eigenschaften und Kristallstruktur von Bis(phthalocyaninato)cer(IV)

Preparation, Properties and Crystal Structure of Bis(phthalocyaninato)cerium(IV) The anodic or chemical oxidation with dibenzoylperoxide of solutions of bis(phthalocyaninato)cerate(III) in dichloromethane yields selectively sparely soluble bis(phthalocyaninato)cerium(IV), [Ce(Pc(2-)) 2 ]. Green, monoclinic needles cristallize with a = 18.783(12) Å b = 18.739(16) Å c= 15.618(10) Å ß114.30(7)°; Z = 4; space group C2/c. [Ce(Pc(2–)) 2 ] is a sandwich complex in which the cerium Atom is eightfold coordinated by the isoindole nitrogens of the two staggered convex Pc-rings. The u.v.-vis., m.i.r., f.i.r. and resonance Raman spectra are consistent with the structure.     

Darstellung und Eigenschaften von Organoindiumbromiden

Synthesis and Properties of Organoindium Bromides i-Pr₃In gives with InBr₃ (molar ratio 2:1, toluene, 50°C) i-Pr₂InBr ( 1 ) and (molar ratio 1:2, toluene, 80°C) i-PrInBr₂ ( 2 ). The corresponding reaction of (PhCH₂)₃In and InBr₃ (2:1) gives (PhCH₂)₂InBr ( 3 ), while PhCH₂InBr₂ could be isolated only as ether adduct [PhCH₂InBr₂(OEt₂)_n] ( 4 ). With DME/MeCN and 2 and 4 with THF, respectively, yields the solvate complexes [InBr₃(DME)(MeCN)] ( 5 ), [i-PrInBr₂(THF)₂] ( 6 ) and [PhCH₂InBr₂(THF)₂] ( 7 ). The compounds 1–7 were investigated with NMR-, IR- and MS-techniques. Pyrolysis of the raw material of i-Pr₃In, which contains “MgBrCl” and additional treatment with Et₂O yields the salt [Mg₃Cl_4,65Br_0,35(Et₂O)₆][i-PrInBr_2,7Cl_0,3] ( 8 ). The cation, a trinuclear magnesium complex, possesses local D_3h-symmetric of the Mg₃X₅ backbone (X = Cl, Br).     

Darstellung,Kristallstruktur und Eigenschaften von Cäsiumozonid

Synthesis, Crystal Structure and Properties of Cesium Ozonide By reaction between CsO₂ and mixtures of O₂ and O₃ in the temperature range from 25°C to ?70°C and subsequent extraction with liquid ammonia pure CsO₃ was obtained in grammeamounts. By X-ray powder and thermal techniques a reversible, structural phase transition was detected at +8°C, and decomposition into CsO₂ and O₂ at +53°C. The low-temperature form (T? CsO₃) is isostructural to RbO₃ (P2₁/c; a = 675.1(2), c = 901.5(3) pm, β = 120.74(3)°l Z = 4), the crystal structure of H? CsO₃, which shows orientational disorder with respect to the ozonide ion, corresponds to the CsCl-type of structure (a = 436.06(3) pm). Using the geometry as determined for KO₃ and RbO₃, and the vibrational frequencies of different isotopomeres, the force constants of O₃^? have been redetermined.     

Darstellung und Kristallstruktur von Calciumimid,CaNH

Synthesis and Crystal Structure of Calcium Imide, CaNH Single-crystals of calcium imide were obtained for the first time by the reaction of a mixture of calcium amide with sodium amide at 850°C in an autoclave for salt melts. After cooling the autoclave to room temperature the crystals are embedded in solid Na which was extracted by liquid ammonia. The structure of calcium imide was determined from single-crystal diffractometer data: space group Fm3 m, Z = 4, a = 5.143(1) Å, R/R_w = 0.032/0.028 mit N(F ${}_{\text{º}}^{\text{2}}$ ? 3σ(F ${}_{\text{º}}^{\text{2}}$ )) = 26, N(Var.) = 5. Ca and N atoms are arranged in the motif of the NaCl structure type. The hydrogen atoms of the imide groups are disordered within the Ca octahedra, and they occupy a six fold split position.     

Darstellung und Kristallstruktur von Tetrakis(pentafluorphenylamino)silan

Synthesis and Crystal Structure of Tetrakis(pentafluorophenylamino)silane Colourless single-crystals of Tetrakis(pentafluorophenylamino) silane were obtained from the reaction of SiCl₄ with monolithiated pentafluoroaniline at low temperatures. The aminosilane has been characterized by various spectroscopic methods and its crystal structure has been determined by x-ray diffraction (for details see “Inhaltsübersicht”). Thermal condensation has not been achieved. However, reaction of silicon(IV)-chloride with pentafluoroaniline in the presence of triethylamine yielded the respective tricyclosilazane.     

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.     

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)°.     

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.     

Na2C2 und K2C2: Synthese,Kristallstruktur und spektroskopische Eigenschaften

Na₂C₂ and K₂C₂: Synthesis, Crystal Structure, and Spectroscopic Properties By the reaction of sodium or potassium solved in liquid ammonia with acetylene and subsequent heating in high vacuum Na₂C₂ and K₂C₂ could be synthesised as single phase products. The crystal structures described by Föppl could be confirmed by X-ray and neutron diffraction experiments (K₂C₂) on powdered samples. Both compounds crystallise in a tetragonal structure (I4₁/acd, no. 142, Z = 8) which can be described as a distorted variant of the antifluorite-structure type. At temperatures above room temperature (Na₂C₂: 580 K, K₂C₂: 420 K) a reversible phase transition (1^st order transition) to a cubic modification (Fm 3 m, no. 225, Z = 4) has been observed, analogous to the alkaline earth metal acetylides. This high temperature modification represents an undistorted antifluorite structure with disordered C₂^2– dumbbells. The results of raman- and ¹³C-MAS-NMR-spectroscopic investigations are in agreement with acetylide dumbbells in the title compounds and allow a comparison to the respective monoalkalimetal and alkaline earth metal acetylides.     

Darstellung,Kristallstruktur und IR-spektroskopische Untersuchung von Phosphor(V)-nitrid-imid,HPN2

Preparation, Crystal Structure, and IR-spectroscopic Investigation of Phosphorus Nitride Imide, HPN₂ Pure and fine crystalline phosphorus nitride imide (HPN₂) is obtained by heterogeneous ammonolysis of P₃N₅ with gaseous NH₃ (T = 580°C, p = 30 bar, 6 d). X-ray powder diffraction data has been used to refine the crystal structure of HPN₂ by the Rietveld full-profile technique (I4 2d; a = 461.82(2) pm, c = 702.04(3) pm; Z = 4; 41 reflections observed, 17° < 2Θ < 125°, CuKα₁, germanium monochromator; R(wp) = 0.072, R(I,hkl) = 0.048). In the solid HPN₂ contains a three-dimensional framework of corner-sharing PN₄-tetrahedra (P N: 159.9(4) pm; P N P: 130.1(4)°. The hydrogen atoms are covalently bonded to half of the nitrogen atoms. The IR spectrum exhibits six vibrational modes v(N H): 3224; v_as(PNP): 1330, 1223; v_as(PNHP): 971, 901: δ(PNP): 531 cm⁻¹).     

CsC2H: Synthese,Kristallstruktur und spektroskopische Eigenschaften

CsC₂H: Synthesis, Crystal Structure, and Spectroscopic Properties CsC₂H was synthesised by the reaction of caesium solved in liquid ammonia with acetylene. The crystal structure could be solved and refined from X‐ray and neutron powder diffraction data (space group: R3c, Z = 18). The structure is characterised by C₂H^– trimers which are surrounded by caesium ions. Spectroscopic investigations (IR and Raman) of the stable monoalkalimetal acetylides mainly confirm the data given in the literature and show that the alkalimetal cation has a marked influence on the vibrational properties of the C₂H^– anion.     

Darstellung und Kristallstruktur von KSbS2

Preparation and Crystal Structure of KSbS₂ Red KSbS₂ was prepared in a aqueous solution of KHS and Sb₂S₃ under mild hydrothermal conditions. For crystallographic data see ?Inhaltsübersicht”?. There are SbS-chains, built up by ψ-trigonal bipyramids, which are connected by sharing edges. The K⁺-Ions between these chains have a nearly octaedric coordination.     

Kristallstruktur und Phasenumwandlungen von As(CH3)4I

Crystal Structure and Phase Transitions of As(CH₃)₄I The crystal structure of α-As(CH₃)₄I at room temperature was determined using single crystal data: cubic, space group Pa3 , a = 1 198.0(2) pm. Therefore α-As(CH₃)₄I displays a novel crystal structure, which is not comparable to known AB-Typ structures with respect to the arrangement of anions and the baricenters of the complex cations. Differential thermal analysis showed three phase transitions at 103, 175 and 215°C. The lattice parameters of the high temperature phases (temperature dependent Guinier measurements) are: β-As(CH₃)₄I (tetragonal): a = 845.2(2) pm, c = 615.0(2) pm; γ-As(CH₃)₄I (hexagonal): a = 737.7(2) pm, c = 1 082.2(3) pm; and to δ-As(CH₃)₄I (hexagonal): a = 705.8(2) pm, c = 1 147(1) pm. β-and γ-As[(CH₃)]₄I are isotypic to N(CH₃)₄Cl and As(CH₃)₄Br, respectively.