New Approach to anionic transition metal alkyls; synthesis and e.s.r. characterisation of the d¹dialkylmetallate(III)'s [M(η-C₅H₄R¹)₂R²₂]^–(M = Ti, Zr, or Hf)

1 January 1979

journal article
research article
Published by Royal Society of Chemistry (RSC) in Journal of the Chemical Society, Chemical Communications

No. 7,p. 305-306
https://doi.org/10.1039/c39790000305

Abstract

Sodium naphthalide in tetrahydrofuran (thf) smoothly converts a d⁰ metallocene dialkyl [M(η-C₅H₄R¹)₂R² ₂](M = Ti, Zr, or Hf; R¹= H, Me, or Prⁱ; R²= Me, PhCH₂, Me₃CCH₂, Me₃SiCH₂, or Ph₂CH) into the corresponding d¹ dialkylmetallate(III)[M(η-C₅H₄R¹)₂R² ₂]^–, characterised by e.s.r. spectroscopy [g_av, 1·991 ± 0·007; a(¹H), 0·26 ± 0·09 mT; a(^47,49Ti), 0·87 ± 0·16 mT; a(⁹¹Zr), 2·06 ± 0·34 mT; a(¹⁷⁷Hf), not observed]; commercial samples of HfCl₄ contain 5–10% of the Zr analogue, as estimated by ¹³C n.m.r. (on an organometallic derivative) or e.s.r. spectroscopy of the derived d¹ dialkylmetallate(III).

Keywords

TRANSITION METAL

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New Approach to anionic transition metal alkyls; synthesis and e.s.r. characterisation of the d1dialkylmetallate(III)'s [M(η-C5H4R1)2R22]–(M = Ti, Zr, or Hf)

Abstract

Keywords

New Approach to anionic transition metal alkyls; synthesis and e.s.r. characterisation of the d¹dialkylmetallate(III)'s [M(η-C₅H₄R¹)₂R²₂]^–(M = Ti, Zr, or Hf)