U. Diefenbach et al., STRUCTURAL-ANALYSIS OF AN INORGANIC-ORGAN IC SPIRO COMPOUND FROM CYCLOTRIPHOSPHAZENE AND 9,10-DIAMINOPHENANTHRENE, Acta crystallographica. Section C, Crystal structure communications, 51, 1995, pp. 1215-1218
Spiro[4,4,6,6-tetrachloro-2 lambda(5),4 lambda(5),6 phaza-1,3,5-triene
-2,2,9',10'-diaminophenanthrene] tehahydrofuran solvate, C14H10Cl4N5P3
.2C(4)H(8)O, was synthesized from hexachlorocyclotriphosphazene and 9,
10-diaminophenanthrene in THF in the presence of triethylamine. It cry
stallizes from THF/hexane mixtures to give crystals which include two
THF molecules attached to one molecule of the compound by weak hydroge
n bonds between the NH groups and the THF O atoms. N-H ... O bond dist
ances are approximately 2.03(4) Angstrom The cyclotriphosphazene ring
is slightly twisted with P-N-P-N torsion angles of 16.1(3), -7.5(2) an
d -8.1(3)degrees. The spiro-attached five-membered organic ring is als
o slightly out of the ring plane with torsion angles for P-N-C-C of 1.
0(5)degrees, for N-C-C-N of -1.1(6)degrees and for N-P-N-C of -0.3(4)d
egrees. The endocyclic N-P-N angle of 91.6(3)degrees in the organic fi
ve-membered ring is significantly smaller than that found for comparab
le spiro systems. P-N distances and angles in the phosphazene ring are
in good agreement with those in other spirophosphazenes.