Synthesis and characterization of phenoxyphosphazenes. Structure of 2, 2-[2,20-metheylenebis(4-chlorophenoxy)]-4,4,6,6-tetrachlorocyclo-2l5, 4l5,6l5-triphosphazatriene (spiro)

The reactions of trimericphosphazenes with sodium [2, 20-methylenebis(4-chlorophenoxide)] have been investigated. Experimental studies were carried out in argon atmosphere. The sodium aryloxides were prepared from methylenebis (4-chlorophenol) and sodium. The phosphazene and phenolate were reacted at K20 8C and then refluxed. After the reaction products (1 and 2) were separated by column chromatography, the structures of the compounds were characterized by elemental analysis, IR, 1H–, 13C–, 31P-NMR, and mass spectroscopy. The compound 1 (spiro) crystallizes in the monoclinic space group Cm with unit cell parameters: aZ8.231(1), bZ16.242(2), cZ7.731(1) A ° , bZ103.31(1)8, VZ1005.8(2) A ° 3, DxZ1.796 g cmK3 respectively. The crystal structures were solved by direct methods and refined by full-matrix least squares. q 2005 Elsevier B.V. All rights reserved