Phosphorus-nitrogen compounds: Novel spiro-crypta-phosphazenes. Structure of pentane-3-oxa-N,N′-bis(1,5-oxybenzyl)-spiro (propane-1′,3′- diamino)-4,4,6,6-tetrachlorocyclo- 2λ 5,4λ 5, 6λ 5-triphosphazatriene. Part IX

Selen B., Kilic Z., Caylak N., Hokelek T.

Journal of Molecular Structure, cilt.707, sa.1-3, ss.139-146, 2004 (SCI-Expanded) identifier identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 707 Sayı: 1-3
  • Basım Tarihi: 2004
  • Doi Numarası: 10.1016/j.molstruc.2004.07.009
  • Dergi Adı: Journal of Molecular Structure
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Sayfa Sayıları: ss.139-146
  • Anahtar Kelimeler: synthesis of phosphazenes, spiro-crypta-phosphazenes, crystal structures of phosphazenes, spectroscopic studies of phosphazenes, anisochronism, PNP-LARIAT ETHER, CRYSTAL-STRUCTURES, MACROCYCLES, COMPLEXES, HEXACHLOROCYCLOTRIPHOSPHAZATRIENE, CYCLOPHOSPHAZENES, SODIUM, LIGAND
  • Ankara Üniversitesi Adresli: Evet

Özet

The condensation reactions between hexachlorocyclotriphosphazatriene (1), N 3P 3Cl 6, and dibenzo-diaza crown ethers (2 and 3) afforded two novel spiro-crypta-phosphazene derivatives (4 and 5). Compounds (4 and 5) have been characterized by elemental analyses, FTIR, 1H-, 13C-, 31P NMR, HETCOR and MS. The structure of crypta-phosphazene (5) has been determined crystallographically. Compounds (4 and 5) are the first examples of the crypta-phosphazene derivatives. The 31P NMR spectra of compounds (4 and 5) indicate that both of the compounds have anisochrony, possibly because of the stereogenic nitrogen atoms. In compound (5), the pyramidal geometries of four spiro-cyclic nitrogen atoms give rise to stereogenic properties. The sum of the bond angles around N4, N4A, N5 and N5A nitrogens are 346.2(4), 348.8(3), 347.1(3) and 345.8(4)°, respectively. Compound (5) crystallizes in the P2 1 space group with a=11.831(2), b=21.108(2), c=11.936(1) , β=102.70(1)°, V=2907.9(6) 3, Z=2 and D x=1.442 g cm -3. The absolute structure was determined successfully. There are two molecules in the asymmetric unit. The structure consists of a non-centrosymmetric, non-planar phosphazene ring with a bulky dibenzo-diaza crown ether side group. © 2004 Elsevier B.V. All rights reserved.