Synthesis and crystal structure of tetraacetyldiazidoacetylhexaazaisowurtzitane (C18H22N12O6 center dot 0.5CH(3)COCH(3))

Citation
Lh. Liu et al., Synthesis and crystal structure of tetraacetyldiazidoacetylhexaazaisowurtzitane (C18H22N12O6 center dot 0.5CH(3)COCH(3)), CHIN J ST C, 20(1), 2001, pp. 15-18
Citations number
13
Language
INGLESE
art.tipo
Article
Categorie Soggetti
Inorganic & Nuclear Chemistry
Journal title
CHINESE JOURNAL OF STRUCTURAL CHEMISTRY
ISSN journal
0254-5861 → ACNP
Volume
20
Issue
1
Year of publication
2001
Pages
15 - 18
Database
ISI
SICI code
0254-5861(2001)20:1<15:SACSOT>2.0.ZU;2-F
Abstract
Tetraacetyldiazidoacetylhexaazaisowurtzitane (TADAIW) was synthesized by hy drogenolysis debenzylation, chloroacetylation and azidation, starting with tetraacetyldibenzylhexaazaisowurtzitane (TADBIW) M-r = 531.5. Its crystal b elongs to the monoclinic system and space group P2(1)/n, with parameters: a = 12.333(3), b = 9.230(2), c = 21.264(4) Angstrom, beta = 94.27(3)degrees, V = 2413. 8(8) Angstrom (3), Z = 4, D-c = 1.463 g.cm(-1), F(000) = 1112, m u (MoK alpha) = 0.114 mm(-1), lambda = 0.71073 Angstrom. The final refineme nt with 357 parameters and 4237 independent reflections gave R = 0.0722 and wR = 0.1916. The cell contains four TADAIW molecules and two acetone molec ules. TADAIW is a caged polycyclic molecule composed of two five-membered r ings and one six-membered ring. The bond angles of N(51) - N(53) - N(53) an d N(61) - N (62) - N(63) in the azidoacetyl groups are 170.9(7)degrees and 170.2(8)degrees, respectively.