ansa-Metallocene derivatives : Molecular structure and proton magnetic resonance spectra or methylene- and ethylene-bridged dicyclopentadienyltitanium compounds

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1979
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Smith, James A.
von Seyerl, Joachim
Huttner, Gottfried
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Journal of Organometallic Chemistry. 1979, 173(2), pp. 175-185. ISSN 0022-328X. Available under: doi: 10.1016/S0022-328X(00)81287-5
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The molecular structure of the methylene-bridged titanocene dichloride, CH2(C5H4)2TiCl2, and that of the novel, ethylene-bridged derivative, (CH2)2-(C5H4)2TiCl2 have been determined by X-ray diffraction methods. In these molecules the cyclopentadienyl ligands are highly restricted in their torsional mobility. An angle of 65° between the two ring planes, a C-C-C angle of 97.5° at the methylene carbon atom, and other geometrical data, indicate a high degree of strain in the methylene-bridged derivative, whereas the ligand geometry of the ethylene-bridged derivative does not deviate significantly from that of unbridged titanocene dichloride. 1H NMR spectra for ansa-titanocene derivatives of general type (CH2)n-C5H4)2TiX2 (n = 1–3, X = Cl, CH3, CO) are reported; the varying degrees of splitting between the high-field and the low-field portions of an A2B2 resonance pattern due to the cyclopentadienyl hydrogen atoms are interpreted in terms of bonding goemetries.

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ISO 690SMITH, James A., Joachim VON SEYERL, Gottfried HUTTNER, Hans-Herbert BRINTZINGER, 1979. ansa-Metallocene derivatives : Molecular structure and proton magnetic resonance spectra or methylene- and ethylene-bridged dicyclopentadienyltitanium compounds. In: Journal of Organometallic Chemistry. 1979, 173(2), pp. 175-185. ISSN 0022-328X. Available under: doi: 10.1016/S0022-328X(00)81287-5
BibTex
@article{Smith1979ansaM-23915,
  year={1979},
  doi={10.1016/S0022-328X(00)81287-5},
  title={ansa-Metallocene derivatives : Molecular structure and proton magnetic resonance spectra or methylene- and ethylene-bridged dicyclopentadienyltitanium compounds},
  number={2},
  volume={173},
  issn={0022-328X},
  journal={Journal of Organometallic Chemistry},
  pages={175--185},
  author={Smith, James A. and von Seyerl, Joachim and Huttner, Gottfried and Brintzinger, Hans-Herbert}
}
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    <dcterms:abstract xml:lang="eng">The molecular structure of the methylene-bridged titanocene dichloride, CH&lt;sub&gt;2&lt;/sub&gt;(C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;TiCl&lt;sub&gt;2&lt;/sub&gt;, and that of the novel, ethylene-bridged derivative, (CH&lt;sub&gt;2&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;-(C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;TiCl&lt;sub&gt;2&lt;/sub&gt; have been determined by X-ray diffraction methods. In these molecules the cyclopentadienyl ligands are highly restricted in their torsional mobility. An angle of 65° between the two ring planes, a C-C-C angle of 97.5° at the methylene carbon atom, and other geometrical data, indicate a high degree of strain in the methylene-bridged derivative, whereas the ligand geometry of the ethylene-bridged derivative does not deviate significantly from that of unbridged titanocene dichloride. &lt;sup&gt;1&lt;/sup&gt;H NMR spectra for ansa-titanocene derivatives of general type (CH&lt;sub&gt;2&lt;/sub&gt;)&lt;sub&gt;n&lt;/sub&gt;-C&lt;sub&gt;5&lt;/sub&gt;H&lt;sub&gt;4&lt;/sub&gt;)&lt;sub&gt;2&lt;/sub&gt;TiX&lt;sub&gt;2&lt;/sub&gt; (n = 1–3, X = Cl, CH&lt;sub&gt;3&lt;/sub&gt;, CO) are reported; the varying degrees of splitting between the high-field and the low-field portions of an A&lt;sub&gt;2&lt;/sub&gt;B&lt;sub&gt;2&lt;/sub&gt; resonance pattern due to the cyclopentadienyl hydrogen atoms are interpreted in terms of bonding goemetries.</dcterms:abstract>
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