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Synthesis, characterization, and reactivity of (1)-metallocenophane complexes of titanium and zirconium

Thesis/Dissertation ·
OSTI ID:6950324

A series of modified metallocene dichloride compounds, (SiR/sub 2/(C/sub 2/H/sub 5/)/sub 2/)MCl/sub 2/ (M = Ti, R = CH/sub 3/; M = Zr, R = CH/sub 3/, C/sub 2/H/sub 5/, n-C/sub 3/H/sub 7/), have been prepared to investigate the stereochemical influence of the dialkylsilyl bridge on the chemical behavior of these modified metallocenes. These compounds have been characterized by elemental analysis and /sup 1/H and /sup 13/C NMR, and the molecular structures of (Si(CH/sub 3/)/sub 2/(C/sub 5/H/sub 4/)/sub 2/)MCl/sub 2/, M = Ti, Zr have been determined by X-ray diffraction methods. The susceptibility of these complexes to undergo reduction has been examined both by electrochemical and chemical means. Cyclic voltammetric measurements have shown that these (1)-metallocenophane dichlorides exhibit only one reversible reduction in THF within a scan range of 1.0 to -3.0 volts vs. SCE. Complementary EPR studies were conducted to identify and monitor the stability of the paramagnetic species generated during the electrochemical reduction of (Si(CH/sub 3/)/sub 2/(C/sub 5/H/sub 4/)/sub 2/)TiCl/sub 2/ and sodium naphthalide reduction of (Si(CH/sub 3/)/sub 2/(C/sub 5/H/sub 4/)/sub 2/)MCl/sub 2/, M = Ti, Zr. These reduction processes similarly proceed with the formation of only one stable paramagnetic product, (Si(CH/sub 3/)/sub 2/(C/sub 5/H/sub 4/)/sub 2/)MCl/sub 2/-.

Research Organization:
West Virginia Univ., Morgantown (USA)
OSTI ID:
6950324
Country of Publication:
United States
Language:
English