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DKCIAIMER >k w*^t«wWesM>ieOTuntotwQ>k JportWedbyanagencvolthe UnitM Stjta Gowrnrnem. the Uniied S I M M GcNtrnnwti nor any agency thereof, nor any of their tmploym, m»k«»ny v, eicreu or (melted, W aWumw any legal liability 0* resooniioll'tv lor the accuracy, enns, or uMfu'nea of any informellon, apparatus, prodixl, or procen diMoaetf. or »• mat itt me would not infringe p'ivalely o w » , righw. Rclerenc* herein 10 any specific •demark, manulaclurer, or olhervrfw, d o « LBL-10497 id Stuei Governfneni or any agency th I. II. The Synthesis• »and Characterization of Annulated Uranocenes The Variable Temperature ^ H NMR of Uranocenes Abstract A general synthetic route to alkyl annulated cycloocta- tetraene dianions and the corresponding annulated uranocenes has been developed. Dideprotonation of bicyclooctai ienes resulting from reaction of cyclooctatetraene dianion vith l,n-dialkylbromides or methanesulfonates, affords alk} annulated cyclooctatetraene dianions in moderate yields. Three diannulated uranocenes, dicyclopenteno-, bisdimethylcyclopen- teno- and dicyclohexenouranocene were prepared from the corresponding cyclooctatetraene dianions and UC1.. The structures of dicyclobuteno- and dicyclopentenouranocene v.ere elucidated by single crystal X-ray diffraction and the effects of annulation on the uranocene skeleton are discussed. Attempted synthesis of benzocyclooctatetraene and a benz- annulated uranocene are reported. The variable temperature H NMR spectrum of uranocene has The isotropic shift been reinvestigated from -100 to 100°C. was found to be linear in T of 0 at T with an extrapolated intercept H NMR spectra, from The Variable temperature o 70°C, of 17 substituted uranocenes are reported. energy barrier to ring rotation in 1,1',4,4'-tetra-t-butyl- uranocene was determined to be 8.24 + 0.5 kcal/mole while the barrier in the corresponding 1,1',3,3'-tetra-t-butylferrocene was determined to be 13.1 kcal/mole. Conformational analysis of 1,1'-dialkyluranocenes by •ISTWJUTION OF THIS DOCUMENT IS UNUMITI ma

I. The synthesis and characterization of annulated uranocenes. II. The variable temperature /sup 1/H NMR of uranocenes