Synthesis of Chlorinated Pyrylium Salts

✍ Scribed by Prof. Dr. A. Roedig; Dr. M. Schlosser; Dipl.-Chem. H.-A. Renk

• Publisher: John Wiley and Sons
• Year: 1966
• Tongue: English
• Weight: 198 KB
• Volume: 5
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.196604182

✦ Synopsis

At the reaction temperatures required (between 120 and 14OOC) the product sublimes and deposits in the cooler part of the apparatus as needle-shaped crystals, often twinned; the vanadium tetrachloride formed as by-product is removed in the stream of chlorine (ca. 4 litersihr). In three hours, 500 mg of vanadium nitride can be converted. Weissenberg photographs and Buerger precession diagrams show that CljVNCl is triclinic with lattice parameters a = 7.64 A b = 7.14 cc = 112.4 p = 94.9 y = 107.8

The volume of the unit cell set up by Delaunay's method [21 is 276.6 .&3. This value is about twice that estimated for one molecule from the ionic increments [31, so that the unit cell must contain two formula units of C13VNCl. From these results a value of 2.48 g/cm3 is derived for the density.

It is not yet possible to decide between the two space groups P1 and P I , but preliminary results of a complete structure determination make the centrosymmetric space group appear the more probable. c = 5.91 11