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  • Author: Soheila Chitsaz x
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Colourless single crystals of Ph3AsCl2 as well as of β-Ph3AsBr2 were obtained from acetonitrile solutions and were suitable for X-ray structure determinations. Ph3AsCl2: Space group P212121, Z = 4, lattice dimensions at -90 °C: a = 1247.9(2), b = 1267.5(1), c = 1033.4(1) pm, R x = 0.0484.

β-Ph3AsBr2: Space group P1̄ , Z = 4, lattice dimensions at -80 °C: a = 949.1(1), b = 1189.7(1), c = 1693.7(2) pm, a = 98.32(1)°, ß = 103.64(1)°, γ = 109.44(1)°, R x - 0.0628. The structures consist of Ph3AsX2 molecules (X = Cl, Br) with trigonalbipyramidal coordination of the arsenic atom with the halogen atoms in the axial positions.

Yellow-orange single crystals of [Ph3AsBr]2[TeBr6] have been prepared from saturated solutions of Ph3AsBr2 and TeBr4 in acetonitrile and characterized by a crystal structure determination. Space group R3̄c, Z = 12, lattice dimensions at -70 °C: a = b = 1337.9(2), c = 7953.8(4) pm, R = 0.0691. The structure consists of discrete ions [Ph3AsBr]+ and nearly perfectly octahedral [TeBr6]2-.

The crystal structures of the monoclinic form of Ph2P(O)NH2 and of its cesium salt, [Cs{Ph2P(O)NH}] have been determined by X-ray methods.

Ph2P(O)NH2: Space group P21/c, Z = 16, lattice dimensions (-80°C): a = 2530.2(3), b = 858.9(2), c = 2135.5(3) pm, β = 110.78(1)°, R , = 0.055. Diphenylphosphinic acid amide forms dimeric molecules via N-H ··· O hydrogen bonds, the dimeric units again are associated via hydrogen bonds to form infinite double chains along the crystallographic c axis.

[Cs{Ph2P(O)NH}]: Space group Pccn, Z = 8 , lattice dimensions (-83°C): a = 1262.8(1), b = 2632.3(2), c = 769.1(1) pm , R1 = 0.024. The compound is associated via Cs-O and Cs-N contacts along the crystallographic [001] axis forming a tubular arrangement. There are no hydrogen bonds.

[(THF)2LiCl2VCl2(THF)2] (1) and [Li(THF)4][OMoCl4(THF)] (2) can be prepared by the reactions of VCI3 with LiCl in THF and of Li(H)PtBu with OM0 CI4 in THF, respectively. 1 and 2 were characterized by IR spectroscopy, MS spectrometry (2) and X-ray crystallography. 1 can be obtained in two modifications depending on the temperature of crystallization. At -30 °C a triclinic form, 1a, was isolated from THF solution with one unique molecule per asymmetric unit. However, at 20 °C, 1b crystallized in the monoclinic space group P2/c. It possesses four independent molecules per asymmetric unit. According to the structure analyses 1 consists of a dinuclear complex with a planar LiCl2V four-membered ring while 2 consists of seperate ions [Li(THF)4]+ and [OMoCl4(THF)]-

Abstract

Single crystals of [(TMEDA)LiCl]2 · toluene (1) and [(MeCN)2LiCl]n (2) can be obtained by dissolving LiCl in TMEDA or acetonitrile and crystallization (after addition of toluene for 1) at -30 °C. 1 is a dimer in the solid state while 2 is polymeric. 1 crystallizes in the space group I 2/a, Z = 4, with lattice dimensions at -90 °C: a = 1475.3(1), b=1112.7(2), c = 1615.0(2) pm, β = 103.44(1)°; Rx = 0.0739 with a disorder of the TMEDA ligand in two twist-positions. Crystals of 2 possess the space group Pbcm, Z = 4, with lattice dimensions at -80 °C: a = 1256.8(2), b = 775.2(1), c = 758.6(1) pm;R1 = 0.0419.