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/sup 1/H, /sup 47/Ti, and /sup 49/Ti ENDOR study on frozen solutions of ((eta/sup 5/-C/sub 5/H/sub 5/)Ti(eta/sup 8/-C/sub 8/H/sub 8/)) and ((eta/sup 5/-CH/sub 3/ x C/sub 5/H/sub 4/)Ti(eta/sup 8/-C/sub 8/H/sub 8/))

Journal Article · · J. Am. Chem. Soc.; (United States)
DOI:https://doi.org/10.1021/ja00249a020· OSTI ID:6181949

The paramagnetic mixed sandwich compounds CpTicot and Me-CpTicot (Cp = eta/sup 5/-C/sub 5/H/sub 5/, Me-Cp = eta/sup 5/-CH/sub 3/-C/sub 5/H/sub 4/, cot = eta/sup 8/-C/sub 8/H/sub 8/) were studied by ENDOR. It is shown for the first time that signals due to /sup 47/Ti and /sup 49/Ti nuclei in natural abundance can be resolved in dilute frozen solutions. These data yielded a measure of the quadrupole interaction from which a negative field gradient at the Ti nucleus could be deduced, indicating that the d/sub x/sup 2/-y/sup 2// and d/sub xy/ metal orbitals are significantly occupied. Proton ENDOR below 60 K allowed us to measure the principal values of the hyperfine tensor and to deduce proton coordinates from a simple point dipole model. The onset of fast ring reorientation above 60 K is clearly manifested by a gradual transformation of the low-temperature, powderlike ENDOR spectrum into a single crystallike spectrum. The effect of methyl substitution on Cp rings demonstrates that the ring reorientation is only governed by intermolecular interactions.

OSTI ID:
6181949
Journal Information:
J. Am. Chem. Soc.; (United States), Journal Name: J. Am. Chem. Soc.; (United States) Vol. 109:15; ISSN JACSA
Country of Publication:
United States
Language:
English