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;1060°;C and ~22 kbar. Ultrahigh-temperature conditions persisted even after a significant drop in pressure. We dated monazite, zircon, rutile, garnet and apatite from felsic granulite by U;Pb, biotite from retrogressed felsic granulite by Rb;Sr, and titanite from mafic granulite by U;Pb. Zircon and titanite give within analytical uncertainties the same age at 341·;5 ±; 0·;8 Ma (2{sigma}) and 342·;0 ±; 0·;8 Ma (2{sigma}), respectively, demonstrating (1) a similar closure temperature for both minerals in dry systems and (2) a closure temperature for titanite considerably higher than 550°;C. Monazite plots discordantly and yields a 207Pb/206Pb age at 338·;0 ±;0·;5 Ma (2{sigma}), which represents a minimum age because of the possibility of excess 206Pb. Rutile, garnet and apatite have little radiogenic lead and show a wide range of apparent 206Pb/238U ages, which reflects initial isotopic heterogeneities originating from the reaction history rather than later disturbances. Biotite yields an Rb;Sr age at 323·;0 ±; 2·;3 Ma (2{sigma}). The age data in combination with the P;T path demonstrate that exhumation of the Saxon Granulite Massif to a middle- to upper-crustal level proceeded at a fast average rate (>9;18 mm/yr) and subsequently slowed down significantly (<2 mm/yr).
DFT-GIAO-NBO and 13C NMR study of the delta-syn-axial effect in 2,4-disubstituted adamantanes
(2008)
Six groups of diastereomeric 2,4-disubstituted adamantanes were studied with DFT-GIAO-NBO (natural orbital analysis) methods. The calculated 13C chemical shifts reproduce well the experimental data. It was found that among all diastereomers, those bearing substituents in -syn-axial positions showed the largest overall deshielding, i.e. the sum of all 13C chemical shifts [;;(13C)] was the greatest and also had the highest delocalization contribution to the molecular energy evaluated with NBO. The higher delocalization energy is proposed to be the origin of the deshielding -syn-axial effect
Through the ring closures of tetrahydroisoquinoline 1,3-amino alcohols bearing a phenyl group in the side- chain, diastereomers of novel 1- or 2-phenyl-substituted 1,3,2-oxazaphosphino[4,3-a]isoquinoline 4-oxides, and 1,2,3- oxathiazino[4,3-a]isoquinoline 4-oxides and 4,4-dioxides were prepared. NMR analysis and DFT calculations on the prepared tetrahydroisoquinoline-condensed 1,2,3-heterocycles revealed that their conformational equilibria of cis1-trans-cis2 type are influenced by the relative configuration of P-4 in the 1,3,2-oxazaphosphinanes, and by the position of the phenyl group in the 1,2,3-oxathiazines.