Walter Petter

Preparation and X-ray crystal structures of Li4[Hg2(edta)2] · 8H2O and Ba2[Hg2(teta)2] · 9H2O (teta = N,N,N′,N′-diaminobutanetetraacetate)

Abstract The Hg(II) complexes of the N,N,N′,N′ -tetraacetate of 1,2-deaminoethane (edta) and 1,4-diaminobutane (teta) were crystallized from concentrated aqueous solutions. The first ligand gave crystals of Li 4 Hg 2 (edta) 2 ] · 8H 2 O. Its single crystal X-ray structure determination (triclinic space group P ¯ with a = 9.369)(3), b = 9.354(3), c = 11.584(4) A, α = 67.90(2), β = 67.50(2), γ = 80.42(3)° and Z = 1) showed that each mercury(II) is mainly bound to six donor atoms of the same ligand anion. The coordinated anionic is strained and leaves sufficient space for a seventh donor atom, i.e. a coordinated oxygen atom of the nearest complex ion bound with a much shorter Hg-O distance. The second ligand gave Ba 2 [Hg 2 (teta) 2 ] · 9H 2 O (space group C / c with a = 17.840(2), b = 15.243(2), c = 18.962(6), β = 113.84(1)° and Z = 4) containing two equivalent ligand anions giving the simplest polymeric structure, i.e. a dimer. These results are in agreement with the data obtained from equilibrium studies.

1,3,2λ5-Oxazaphosphinan-4-ones: synthesis and X-ray analysis of a new type of phosphorus-containing heterocycle

Reaction of 3-hydroxycarboxylic acid azides with phosphorus(III) reagents yields 3-hydroxyacyl iminophosphoranes or 1,3,2λ5-oxazaphosphinan-4-ones depending upon the nature of the phosphorus reagent.

Synthesis and X-Ray Analysis of New Spirophosphoranes

Abstract 2- and 3-hydroxyalkyliminophosphoranes and their valencetautomeric pentacoordinated phosphoranes are deprotonated by KH to give anionic pentacoordinated phosphoranes. Upon methylation the latter are converted into N-methyl derivatives. The geometries of these compounds are determined by X-ray analysis and n.m.r. spectroscopy.

Preparation, Crystal Structure and Properties of Spirophosphoranes Derived from Hydroxycarboxylic Acid Azides

Abstract Spirophosphoranes are produced by reaction of 2–phenyl–1,3,2–dioxaphospholane with both 2- and 3–hydroxycarboxylic acid azides, whereas 1–phenyl–phospholane yields spirophosphoranes only upon reaction with the former. The structures of two spirophosphoranes have been determined by X-ray analysis.

Synthesis and X-Ray Crystal Structure of an Annelated Spirophosphorane

Abstract Reaction of the 2-azidoalcohol 1 with 2-phenyl1-1,3,2-dioxaphospholane leads to a 4:1 mixture of the pentacoordinate phosphorane 3 and the diazadiphosphetidine 4. In solution, these compounds are in equilibrium, presumably involving the not detectable iminophosphorane 2. A single X-ray analysis carried out on 3 proves the structure of this type of compound which has been postulated earlier as intermediate in the synthesis of aziridines from azidoalcohols1,2