Phosphorus-nitrogen compounds. spiro- and crypta-phosphazene derivatives: Synthesis and spectral investigations. Structure of butane-N,N′-bis(1,4- oxybenzyl)-spiro(propane-1,3-diamino)tetrachlorocyclo-2λ5, 4λ5, 6λ5-triphosphazatriene. Part VII


Ilter E., Çaylak N., Işiklan M., ASMAFİLİZ N., Kiliç Z., HÖKELEK T.

Journal of Molecular Structure, cilt.697, sa.1-3, ss.119-129, 2004 (SCI-Expanded) identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 697 Sayı: 1-3
  • Basım Tarihi: 2004
  • Doi Numarası: 10.1016/j.molstruc.2004.03.043
  • Dergi Adı: Journal of Molecular Structure
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Sayfa Sayıları: ss.119-129
  • Anahtar Kelimeler: Anisochrony, Crypta-phosphazenes, Crystal structure of crypta-phosphazene, Diazacrown ligand, Spiro-phosphazenes
  • Ankara Üniversitesi Adresli: Evet

Özet

The condensation reactions between trimer, N3P 3Cl6, and diamines, 2 and 4 and {1-{N-[1-(2- hydroxynaphthylmethyl)aminomethylidene]}-2(1H)-naphthalenone, 3, yielded the new spiro-cyclic- (5 and 8) and the novel spiro-phosphazene (7) derivatives, respectively. The fully substituted phosphazene (6) was also obtained from the reaction of 5 with the excess of pyrrolidine. Compounds (4-8) have been characterized by elemental analyses, FTIR, 1H-, 13C-, 31P-NMR, HETCOR, COSY and MS. The structure of crypta-phosphazene, 8, has been examined crystallographically. Compound 8 is the first example of the crypta-phosphazene derivatives. The 31P-NMR spectra of compounds 7 and 8 indicate that, both of the compounds have anisochronism because of the stereogenic centers. The pyramidal geometry of two spiro-cyclic nitrogen atoms in compound 8, gives rise to stereogenic property. The sums of the bond angles around N4 and N5 nitrogens are 350.6(2) and 349.6(3)°, respectively. Compound 8 crystallizes in the triclinic space group P1 with a=8.798(3), b=10.498(3) and c=15.689(4)Å; α=91.35(2), β=103.39(4) and γ=102.88(4)°; V=1369.9(7)Å3, Z=2 and Dx=1.491gcm-3. It consists of a non-centrosymmetric, non-planar phosphazene ring with a bulky dibenzo-diazacrown etheric side group. © 2004 Elsevier B.V. All rights reserved.