Triethylammonium Tris(o-phenylenedioxy)phosphate. Crystal and Molecular Structure

Abstract

Triethylammonium tris(o-phenylenedioxy(phosphate (III) was isolated from the reaction of tris(o-phenylenedioxyjcyclotriphosphazene (I) with catechol and triethylamine. Crystals of III are trigonal, space group P3, with lattice constants of a = 12.046 (13) A, c = 8.744 (12) A, and with Z = 2. The structure was solved by Patterson and Fourier methods and refined by least-squares techniques to an R value of 0.043 for 529 unique reflections. The phosphorus atom within each spirophosphate anion is bonded octahedrally to six oxygen atoms. A hydrogen atom was unambiguously located within bonding distance of the nitrogen atom in the cation. Important molecular parameters are: P-O = 1.723 (4), 1.706 (4) Á; N-H = 0.94 (8), H. O = 2.36 (7) Á, O-P-O(ring) = 91.4 (2)°. The nonbonding transannular O… O distance is 2.454 (5) A. © 1973, American Chemical Society. All rights reserved.