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Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand
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| Zeitschriftentitel: | European Journal of Inorganic Chemistry |
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| Personen und Körperschaften: | , , , , , , |
| In: | European Journal of Inorganic Chemistry, 2003, 2003, 4, S. 633-637 |
| Format: | E-Article |
| Sprache: | Englisch |
| veröffentlicht: |
Wiley
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| Schlagwörter: |
| author_facet |
Poulard, Cyril Perrey, Danièle Boni, Gilles Vigier, Estelle Blacque, Olivier Kubicki, Marek M. Moïse, Claude Poulard, Cyril Perrey, Danièle Boni, Gilles Vigier, Estelle Blacque, Olivier Kubicki, Marek M. Moïse, Claude |
|---|---|
| author |
Poulard, Cyril Perrey, Danièle Boni, Gilles Vigier, Estelle Blacque, Olivier Kubicki, Marek M. Moïse, Claude |
| spellingShingle |
Poulard, Cyril Perrey, Danièle Boni, Gilles Vigier, Estelle Blacque, Olivier Kubicki, Marek M. Moïse, Claude European Journal of Inorganic Chemistry Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand Inorganic Chemistry |
| author_sort |
poulard, cyril |
| spelling |
Poulard, Cyril Perrey, Danièle Boni, Gilles Vigier, Estelle Blacque, Olivier Kubicki, Marek M. Moïse, Claude 1434-1948 1099-0682 Wiley Inorganic Chemistry http://dx.doi.org/10.1002/ejic.200390087 <jats:title>Abstract</jats:title><jats:p>The complex [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaCl<jats:sub>2</jats:sub>] (<jats:bold>1</jats:bold>) was synthesised by reaction of the lithium salt LiC<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>) with the tantalum compound [Cp*TaCl<jats:sub>3</jats:sub>(PMe<jats:sub>3</jats:sub>)]. Reduction of <jats:bold>1</jats:bold> with NaAl(H)<jats:sub>2</jats:sub>(OCH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>OMe)<jats:sub>2</jats:sub> leads to the trihydride derivative [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>3</jats:sub>] (<jats:bold>2</jats:bold>). The oxidation of <jats:bold>2</jats:bold> in THF with ferrocenium ion leads to a cationic dihydride intermediate [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>2</jats:sub>]PF<jats:sub>6</jats:sub> (<jats:bold>3</jats:bold>) with an intramolecular stabilization by the aminoethyl side‐chain of the cyclopentadienyl ligand. The hemilabile character of the functionalised cyclopentadienyl ligand was checked by treating <jats:bold>3</jats:bold> with electron‐donating ligands (e.g. phosphanes, sulfides, anions); in all cases, no displacement of the amino group was observed. When treated with HBF<jats:sub>4</jats:sub>, <jats:bold>2</jats:bold> undergoes a loss of the hydride and the resulting cation can be isolated as a solvento adduct by carrying out the reaction in dimethyl sulfide. Acidolysis of <jats:bold>2</jats:bold> in the presence of an excess of trifluoroacetic acid affords the compound [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NHMe<jats:sub>2</jats:sub>)}TaH(OCOCF<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>](CF<jats:sub>3</jats:sub>COO) (<jats:bold>5</jats:bold>). Microanalytical and NMR spectroscopic data for these complexes are given. The X‐ray crystal structures are reported for [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>2</jats:sub>]PF<jats:sub>6</jats:sub> (<jats:bold>3</jats:bold>) and [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NHMe<jats:sub>2</jats:sub>)}TaH(OCOCF<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>](CF<jats:sub>3</jats:sub>COO) (<jats:bold>5</jats:bold>). (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003)</jats:p> Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand European Journal of Inorganic Chemistry |
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2003 |
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Wiley |
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European Journal of Inorganic Chemistry |
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49 |
| title |
Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_unstemmed |
Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_full |
Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_fullStr |
Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_full_unstemmed |
Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_short |
Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_sort |
formation and reactivity of a tantalocene trihydride containing an aminoethyl‐functionalised ligand |
| topic |
Inorganic Chemistry |
| url |
http://dx.doi.org/10.1002/ejic.200390087 |
| publishDate |
2003 |
| physical |
633-637 |
| description |
<jats:title>Abstract</jats:title><jats:p>The complex [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaCl<jats:sub>2</jats:sub>] (<jats:bold>1</jats:bold>) was synthesised by reaction of the lithium salt LiC<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>) with the tantalum compound [Cp*TaCl<jats:sub>3</jats:sub>(PMe<jats:sub>3</jats:sub>)]. Reduction of <jats:bold>1</jats:bold> with NaAl(H)<jats:sub>2</jats:sub>(OCH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>OMe)<jats:sub>2</jats:sub> leads to the trihydride derivative [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>3</jats:sub>] (<jats:bold>2</jats:bold>). The oxidation of <jats:bold>2</jats:bold> in THF with ferrocenium ion leads to a cationic dihydride intermediate [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>2</jats:sub>]PF<jats:sub>6</jats:sub> (<jats:bold>3</jats:bold>) with an intramolecular stabilization by the aminoethyl side‐chain of the cyclopentadienyl ligand. The hemilabile character of the functionalised cyclopentadienyl ligand was checked by treating <jats:bold>3</jats:bold> with electron‐donating ligands (e.g. phosphanes, sulfides, anions); in all cases, no displacement of the amino group was observed. When treated with HBF<jats:sub>4</jats:sub>, <jats:bold>2</jats:bold> undergoes a loss of the hydride and the resulting cation can be isolated as a solvento adduct by carrying out the reaction in dimethyl sulfide. Acidolysis of <jats:bold>2</jats:bold> in the presence of an excess of trifluoroacetic acid affords the compound [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NHMe<jats:sub>2</jats:sub>)}TaH(OCOCF<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>](CF<jats:sub>3</jats:sub>COO) (<jats:bold>5</jats:bold>). Microanalytical and NMR spectroscopic data for these complexes are given. The X‐ray crystal structures are reported for [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>2</jats:sub>]PF<jats:sub>6</jats:sub> (<jats:bold>3</jats:bold>) and [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NHMe<jats:sub>2</jats:sub>)}TaH(OCOCF<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>](CF<jats:sub>3</jats:sub>COO) (<jats:bold>5</jats:bold>). (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003)</jats:p> |
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| author | Poulard, Cyril, Perrey, Danièle, Boni, Gilles, Vigier, Estelle, Blacque, Olivier, Kubicki, Marek M., Moïse, Claude |
| author_facet | Poulard, Cyril, Perrey, Danièle, Boni, Gilles, Vigier, Estelle, Blacque, Olivier, Kubicki, Marek M., Moïse, Claude, Poulard, Cyril, Perrey, Danièle, Boni, Gilles, Vigier, Estelle, Blacque, Olivier, Kubicki, Marek M., Moïse, Claude |
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| description | <jats:title>Abstract</jats:title><jats:p>The complex [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaCl<jats:sub>2</jats:sub>] (<jats:bold>1</jats:bold>) was synthesised by reaction of the lithium salt LiC<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>) with the tantalum compound [Cp*TaCl<jats:sub>3</jats:sub>(PMe<jats:sub>3</jats:sub>)]. Reduction of <jats:bold>1</jats:bold> with NaAl(H)<jats:sub>2</jats:sub>(OCH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>OMe)<jats:sub>2</jats:sub> leads to the trihydride derivative [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>3</jats:sub>] (<jats:bold>2</jats:bold>). The oxidation of <jats:bold>2</jats:bold> in THF with ferrocenium ion leads to a cationic dihydride intermediate [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>2</jats:sub>]PF<jats:sub>6</jats:sub> (<jats:bold>3</jats:bold>) with an intramolecular stabilization by the aminoethyl side‐chain of the cyclopentadienyl ligand. The hemilabile character of the functionalised cyclopentadienyl ligand was checked by treating <jats:bold>3</jats:bold> with electron‐donating ligands (e.g. phosphanes, sulfides, anions); in all cases, no displacement of the amino group was observed. When treated with HBF<jats:sub>4</jats:sub>, <jats:bold>2</jats:bold> undergoes a loss of the hydride and the resulting cation can be isolated as a solvento adduct by carrying out the reaction in dimethyl sulfide. Acidolysis of <jats:bold>2</jats:bold> in the presence of an excess of trifluoroacetic acid affords the compound [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NHMe<jats:sub>2</jats:sub>)}TaH(OCOCF<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>](CF<jats:sub>3</jats:sub>COO) (<jats:bold>5</jats:bold>). Microanalytical and NMR spectroscopic data for these complexes are given. The X‐ray crystal structures are reported for [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>2</jats:sub>]PF<jats:sub>6</jats:sub> (<jats:bold>3</jats:bold>) and [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NHMe<jats:sub>2</jats:sub>)}TaH(OCOCF<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>](CF<jats:sub>3</jats:sub>COO) (<jats:bold>5</jats:bold>). (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003)</jats:p> |
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| imprint | Wiley, 2003 |
| imprint_str_mv | Wiley, 2003 |
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| physical | 633-637 |
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| series | European Journal of Inorganic Chemistry |
| source_id | 49 |
| spelling | Poulard, Cyril Perrey, Danièle Boni, Gilles Vigier, Estelle Blacque, Olivier Kubicki, Marek M. Moïse, Claude 1434-1948 1099-0682 Wiley Inorganic Chemistry http://dx.doi.org/10.1002/ejic.200390087 <jats:title>Abstract</jats:title><jats:p>The complex [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaCl<jats:sub>2</jats:sub>] (<jats:bold>1</jats:bold>) was synthesised by reaction of the lithium salt LiC<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>) with the tantalum compound [Cp*TaCl<jats:sub>3</jats:sub>(PMe<jats:sub>3</jats:sub>)]. Reduction of <jats:bold>1</jats:bold> with NaAl(H)<jats:sub>2</jats:sub>(OCH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>OMe)<jats:sub>2</jats:sub> leads to the trihydride derivative [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>3</jats:sub>] (<jats:bold>2</jats:bold>). The oxidation of <jats:bold>2</jats:bold> in THF with ferrocenium ion leads to a cationic dihydride intermediate [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>2</jats:sub>]PF<jats:sub>6</jats:sub> (<jats:bold>3</jats:bold>) with an intramolecular stabilization by the aminoethyl side‐chain of the cyclopentadienyl ligand. The hemilabile character of the functionalised cyclopentadienyl ligand was checked by treating <jats:bold>3</jats:bold> with electron‐donating ligands (e.g. phosphanes, sulfides, anions); in all cases, no displacement of the amino group was observed. When treated with HBF<jats:sub>4</jats:sub>, <jats:bold>2</jats:bold> undergoes a loss of the hydride and the resulting cation can be isolated as a solvento adduct by carrying out the reaction in dimethyl sulfide. Acidolysis of <jats:bold>2</jats:bold> in the presence of an excess of trifluoroacetic acid affords the compound [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NHMe<jats:sub>2</jats:sub>)}TaH(OCOCF<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>](CF<jats:sub>3</jats:sub>COO) (<jats:bold>5</jats:bold>). Microanalytical and NMR spectroscopic data for these complexes are given. The X‐ray crystal structures are reported for [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NMe<jats:sub>2</jats:sub>)}TaH<jats:sub>2</jats:sub>]PF<jats:sub>6</jats:sub> (<jats:bold>3</jats:bold>) and [Cp*{C<jats:sub>5</jats:sub>H<jats:sub>4</jats:sub>(CH<jats:sub>2</jats:sub>CH<jats:sub>2</jats:sub>NHMe<jats:sub>2</jats:sub>)}TaH(OCOCF<jats:sub>3</jats:sub>)<jats:sub>2</jats:sub>](CF<jats:sub>3</jats:sub>COO) (<jats:bold>5</jats:bold>). (© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003)</jats:p> Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand European Journal of Inorganic Chemistry |
| spellingShingle | Poulard, Cyril, Perrey, Danièle, Boni, Gilles, Vigier, Estelle, Blacque, Olivier, Kubicki, Marek M., Moïse, Claude, European Journal of Inorganic Chemistry, Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand, Inorganic Chemistry |
| title | Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_full | Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_fullStr | Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_full_unstemmed | Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_short | Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| title_sort | formation and reactivity of a tantalocene trihydride containing an aminoethyl‐functionalised ligand |
| title_unstemmed | Formation and Reactivity of a Tantalocene Trihydride Containing an Aminoethyl‐Functionalised Ligand |
| topic | Inorganic Chemistry |
| url | http://dx.doi.org/10.1002/ejic.200390087 |