6533b839fe1ef96bd12a5b68

RESEARCH PRODUCT

Über antimon-haltige heterocyclen

Harald M. HoffmannMartin Dräger

subject

StereochemistryChemistryOrganic ChemistryIntermolecular forceDithiolEthanedithiolCrystal structureNuclear magnetic resonance spectroscopyCarbon-13 NMRDihedral angleRing (chemistry)BiochemistryInorganic Chemistrychemistry.chemical_compoundCrystallographyOctahedronX-ray crystallographyMass spectrumMaterials ChemistryProton NMRSingle bondMoleculePhysical and Theoretical Chemistry

description

Abstract p -Nitrophenyl- and p -tolyl-oxadithia- and trithiastibocanes have been synthesized from the respective aryldichlorostibane and dithiole. The compounds have been characterised by means of 13 C NMR and vibrational spectra (ν(SBS 2 ) 350–320 cm −1 ). The crystal structure of p -nitrophenyltrithiastibocane has been determined ( R = 0.042). The eight-membered ring exhibits a boat-chair conformation. Single-bond distances of SbC and SbS (219, 244 and 245 pm), a 1,5-transannular Sb⋯S interaction (319 pm), and Sb⋯S and Sb⋯O (339 and 353 pm) intermolecular contacts, result in a six-coordinated Sb III (ψ-monocapped octahedral) species. The two additional Sb⋯S distances are in accordance with the vibrational (Sb⋯S) bands at 236 and 218 cm −1 . A logarithmic correlation between the transannular distances and the respective vibrations are discussed for a series of related trithiastibocanes.

https://doi.org/10.1016/s0022-328x(00)98894-6