Fluoride und Fluorosäuren, VIII [1]. Über eine fehlgeordnete feste Phase des SF4 sowie die Kristallstrukturen von Produkten seiner unbeabsichtigten Hydrolyse in Glasapparaturen, SiF4 (Neubestimmung) und SOF2 / Fluorides and Fluoro Acids, VIII [1]. On a Disordered Solid Phase of SF4 and the Crystal Structures of Products of its Unintentional Hydrolysis in Glass Apparatus, SiF4 (Redetermination) and SOF2

Abstract

A structural investigation on single crystals of SF4 yielded the cubic space group Fm3m with a = 676.1(5) pm and Z = 4 and from this cubic close packing and at least sixfold disorder of isolated molecules. In one of the experiments of manipulating SF4 unintentional hydrolysis of the compound in a Duran-glass vacuum line occurred. The products SiF4 and SOF2 could be characterized by structure analysis after a miniature zone-melting separation and crystal growth in one and the same thin-walled capillary. The results for SiF4 [14̄3m, a = 547.6(1) pm, Z = 2 at -117 °C] confirm earlier work with a higher numerical accuracy. SOF2 crystallizes in the monoclinic space group P21/c with a = 524.7(1), b = 704.9(2), c = 1449.3(4) pm, β = 97.20(2)° at - 137 °C and Z = 8. Isolated molecules of pyramidal geometry are arranged in strongly folded layers with intermolecular S···O contacts.