Multiple bonds between main-group elements and transition metals: Part 157 neutral and cationic ansa -metallocenes of niobium(V) and tantalum(V): Synthesis, structures and stereochemical non-rigidity
Identifieur interne : 004237 ( Istex/Corpus ); précédent : 004236; suivant : 004238Multiple bonds between main-group elements and transition metals: Part 157 neutral and cationic ansa -metallocenes of niobium(V) and tantalum(V): Synthesis, structures and stereochemical non-rigidity
Auteurs : Wolfgang A. Herrmann ; Walter Baratta ; Eberhardt HerdtweckSource :
- Journal of Organometallic Chemistry [ 0022-328X ] ; 1997.
English descriptors
- KwdEn :
Abstract
The metal amide route has been exploited to synthesize η5:η1- and η5:η5 ansa-metallocenes of pentavalent niobium and tantalum. Tris(dimethylamido)(2,6-diisopropylphenylimido)-niobium(V) 2a and -tantalum(V) 2b were found to be appropriate starting compounds to cleanly react with CH-acidic ligand precursors such as cyclopentadiene and 2,2-bis(cyclopentadienyl)propane. In the latter case, the novel ansa-metallocenes of formula [C5H4-C(CH3)2-C5H4]M[=N(2,6-iPr2C6H3)][N(CH3)2] (4a, M = Nb; 4b, M = Ta) result in high yields. While the hydrocarbon ligand adopts an η1:η5-coordination to the metals in the solid state (X-ray diffraction studies), a rapid η1:η5-η5:η1 equilibration occurs in solution. Complexes 4a,b react promptly with (CH3)3SiCl, thus affording the ansa-metallocenes [C5H4-C(CH3)2-C5H4]M[-N(2,6-iPr2C6H3)]Cl (5a, M = Nb; 5b, M = Ta) quantitatively. The crystal structures of the niobium(V) and tantalum(V) chloro derivatives 5a,b reveal a ‘conventional’ η5:η5-coordination for the chelating bis(cyclopentadienyl) ligand. Protonolysis of 4a,b with [NHMe3][B(C6H5)4] afforded the first cationic ansa-metallocenes [C5H4-C(CH3)2-C5H4]M[=N(2,6-iPr2C6H3)][NH(CH3)2][B(C6H5)4] (6a, M = Nb; 6b, M = Ta) in high yields. The crystal structure of 6a shows an η5:η5-coordination mode for the bis(cyclopentadienyl) ligand. The 1J(C,H) coupling constants of the bis(cyclopentadienyl) ligand of the ansa-metallocenes 4a,b, 5a,b and 6a,b are related to its hapticity, which is a result of the electronic properties of the metal center.
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DOI: 10.1016/S0022-328X(97)00121-6
Links to Exploration step
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<front><div type="abstract" xml:lang="en">The metal amide route has been exploited to synthesize η5:η1- and η5:η5 ansa-metallocenes of pentavalent niobium and tantalum. Tris(dimethylamido)(2,6-diisopropylphenylimido)-niobium(V) 2a and -tantalum(V) 2b were found to be appropriate starting compounds to cleanly react with CH-acidic ligand precursors such as cyclopentadiene and 2,2-bis(cyclopentadienyl)propane. In the latter case, the novel ansa-metallocenes of formula [C5H4-C(CH3)2-C5H4]M[=N(2,6-iPr2C6H3)][N(CH3)2] (4a, M = Nb; 4b, M = Ta) result in high yields. While the hydrocarbon ligand adopts an η1:η5-coordination to the metals in the solid state (X-ray diffraction studies), a rapid η1:η5-η5:η1 equilibration occurs in solution. Complexes 4a,b react promptly with (CH3)3SiCl, thus affording the ansa-metallocenes [C5H4-C(CH3)2-C5H4]M[-N(2,6-iPr2C6H3)]Cl (5a, M = Nb; 5b, M = Ta) quantitatively. The crystal structures of the niobium(V) and tantalum(V) chloro derivatives 5a,b reveal a ‘conventional’ η5:η5-coordination for the chelating bis(cyclopentadienyl) ligand. Protonolysis of 4a,b with [NHMe3][B(C6H5)4] afforded the first cationic ansa-metallocenes [C5H4-C(CH3)2-C5H4]M[=N(2,6-iPr2C6H3)][NH(CH3)2][B(C6H5)4] (6a, M = Nb; 6b, M = Ta) in high yields. The crystal structure of 6a shows an η5:η5-coordination mode for the bis(cyclopentadienyl) ligand. The 1J(C,H) coupling constants of the bis(cyclopentadienyl) ligand of the ansa-metallocenes 4a,b, 5a,b and 6a,b are related to its hapticity, which is a result of the electronic properties of the metal center.</div>
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<abstract>The metal amide route has been exploited to synthesize η5:η1- and η5:η5 ansa-metallocenes of pentavalent niobium and tantalum. Tris(dimethylamido)(2,6-diisopropylphenylimido)-niobium(V) 2a and -tantalum(V) 2b were found to be appropriate starting compounds to cleanly react with CH-acidic ligand precursors such as cyclopentadiene and 2,2-bis(cyclopentadienyl)propane. In the latter case, the novel ansa-metallocenes of formula [C5H4-C(CH3)2-C5H4]M[=N(2,6-iPr2C6H3)][N(CH3)2] (4a, M = Nb; 4b, M = Ta) result in high yields. While the hydrocarbon ligand adopts an η1:η5-coordination to the metals in the solid state (X-ray diffraction studies), a rapid η1:η5-η5:η1 equilibration occurs in solution. Complexes 4a,b react promptly with (CH3)3SiCl, thus affording the ansa-metallocenes [C5H4-C(CH3)2-C5H4]M[-N(2,6-iPr2C6H3)]Cl (5a, M = Nb; 5b, M = Ta) quantitatively. The crystal structures of the niobium(V) and tantalum(V) chloro derivatives 5a,b reveal a ‘conventional’ η5:η5-coordination for the chelating bis(cyclopentadienyl) ligand. Protonolysis of 4a,b with [NHMe3][B(C6H5)4] afforded the first cationic ansa-metallocenes [C5H4-C(CH3)2-C5H4]M[=N(2,6-iPr2C6H3)][NH(CH3)2][B(C6H5)4] (6a, M = Nb; 6b, M = Ta) in high yields. The crystal structure of 6a shows an η5:η5-coordination mode for the bis(cyclopentadienyl) ligand. The 1J(C,H) coupling constants of the bis(cyclopentadienyl) ligand of the ansa-metallocenes 4a,b, 5a,b and 6a,b are related to its hapticity, which is a result of the electronic properties of the metal center.</abstract>
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<abstract xml:lang="en"><p>The metal amide route has been exploited to synthesize η5:η1- and η5:η5 ansa-metallocenes of pentavalent niobium and tantalum. Tris(dimethylamido)(2,6-diisopropylphenylimido)-niobium(V) 2a and -tantalum(V) 2b were found to be appropriate starting compounds to cleanly react with CH-acidic ligand precursors such as cyclopentadiene and 2,2-bis(cyclopentadienyl)propane. In the latter case, the novel ansa-metallocenes of formula [C5H4-C(CH3)2-C5H4]M[=N(2,6-iPr2C6H3)][N(CH3)2] (4a, M = Nb; 4b, M = Ta) result in high yields. While the hydrocarbon ligand adopts an η1:η5-coordination to the metals in the solid state (X-ray diffraction studies), a rapid η1:η5-η5:η1 equilibration occurs in solution. Complexes 4a,b react promptly with (CH3)3SiCl, thus affording the ansa-metallocenes [C5H4-C(CH3)2-C5H4]M[-N(2,6-iPr2C6H3)]Cl (5a, M = Nb; 5b, M = Ta) quantitatively. The crystal structures of the niobium(V) and tantalum(V) chloro derivatives 5a,b reveal a ‘conventional’ η5:η5-coordination for the chelating bis(cyclopentadienyl) ligand. Protonolysis of 4a,b with [NHMe3][B(C6H5)4] afforded the first cationic ansa-metallocenes [C5H4-C(CH3)2-C5H4]M[=N(2,6-iPr2C6H3)][NH(CH3)2][B(C6H5)4] (6a, M = Nb; 6b, M = Ta) in high yields. The crystal structure of 6a shows an η5:η5-coordination mode for the bis(cyclopentadienyl) ligand. The 1J(C,H) coupling constants of the bis(cyclopentadienyl) ligand of the ansa-metallocenes 4a,b, 5a,b and 6a,b are related to its hapticity, which is a result of the electronic properties of the metal center.</p>
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<head><ce:article-footnote><ce:label>2</ce:label>
<ce:note-para>For the preceding communication, no. 156 of this series, see Ref. [1].</ce:note-para>
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<ce:title>Multiple bonds between main-group elements and transition metals: Part 157 neutral and cationic <ce:italic>ansa</ce:italic>
-metallocenes of niobium(V) and tantalum(V): Synthesis, structures and stereochemical non-rigidity</ce:title>
<ce:dedication>Dedicated to Professor Gottfried Huttner on the occasion of his 60th birthday.</ce:dedication>
<ce:author-group><ce:author><ce:given-name>Wolfgang A.</ce:given-name>
<ce:surname>Herrmann</ce:surname>
<ce:cross-ref refid="cor1"><ce:sup>*</ce:sup>
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<ce:author><ce:given-name>Walter</ce:given-name>
<ce:surname>Baratta</ce:surname>
</ce:author>
<ce:author><ce:given-name>Eberhardt</ce:given-name>
<ce:surname>Herdtweck</ce:surname>
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<ce:text>Corresponding author.</ce:text>
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<ce:abstract id="ab1" class="author" xml:lang="en"><ce:section-title>Abstract</ce:section-title>
<ce:abstract-sec><ce:simple-para>The metal amide route has been exploited to synthesize <ce:italic>η</ce:italic>
<ce:sup loc="post">5</ce:sup>
:<ce:italic>η</ce:italic>
<ce:sup loc="post">1</ce:sup>
- and <ce:italic>η</ce:italic>
<ce:sup loc="post">5</ce:sup>
:<ce:italic>η</ce:italic>
<ce:sup loc="post">5</ce:sup>
<ce:italic>ansa</ce:italic>
-metallocenes of pentavalent niobium and tantalum. Tris(dimethylamido)(2,6-diisopropylphenylimido)-niobium(V) <ce:bold>2a</ce:bold>
and -tantalum(V) <ce:bold>2b</ce:bold>
were found to be appropriate starting compounds to cleanly react with CH-acidic ligand precursors such as cyclopentadiene and 2,2-bis(cyclopentadienyl)propane. In the latter case, the novel <ce:italic>ansa</ce:italic>
-metallocenes of formula [C<ce:inf loc="post">5</ce:inf>
H<ce:inf loc="post">4</ce:inf>
-C(CH<ce:inf loc="post">3</ce:inf>
)<ce:inf loc="post">2</ce:inf>
-C<ce:inf loc="post">5</ce:inf>
H<ce:inf loc="post">4</ce:inf>
]M[=N(2,6-<ce:sup loc="post">i</ce:sup>
Pr<ce:inf loc="post">2</ce:inf>
C<ce:inf loc="post">6</ce:inf>
H<ce:inf loc="post">3</ce:inf>
)][N(CH<ce:inf loc="post">3</ce:inf>
)<ce:inf loc="post">2</ce:inf>
] (<ce:bold>4a</ce:bold>
, M = Nb; <ce:bold>4b</ce:bold>
, M = Ta) result in high yields. While the hydrocarbon ligand adopts an <ce:italic>η</ce:italic>
<ce:sup loc="post">1</ce:sup>
:<ce:italic>η</ce:italic>
<ce:sup loc="post">5</ce:sup>
-coordination to the metals in the solid state (X-ray diffraction studies), a rapid <ce:italic>η</ce:italic>
<ce:sup loc="post">1</ce:sup>
:<ce:italic>η</ce:italic>
<ce:sup loc="post">5</ce:sup>
-<ce:italic>η</ce:italic>
<ce:sup loc="post">5</ce:sup>
:<ce:italic>η</ce:italic>
<ce:sup loc="post">1</ce:sup>
equilibration occurs in solution. Complexes <ce:bold>4a,b</ce:bold>
react promptly with (CH<ce:inf loc="post">3</ce:inf>
)<ce:inf loc="post">3</ce:inf>
SiCl, thus affording the <ce:italic>ansa</ce:italic>
-metallocenes [C<ce:inf loc="post">5</ce:inf>
H<ce:inf loc="post">4</ce:inf>
-C(CH<ce:inf loc="post">3</ce:inf>
)<ce:inf loc="post">2</ce:inf>
-C<ce:inf loc="post">5</ce:inf>
H<ce:inf loc="post">4</ce:inf>
]M[-N(2,6-<ce:sup loc="post">i</ce:sup>
Pr<ce:inf loc="post">2</ce:inf>
C<ce:inf loc="post">6</ce:inf>
H<ce:inf loc="post">3</ce:inf>
)]Cl (<ce:bold>5a</ce:bold>
, M = Nb; <ce:bold>5b</ce:bold>
, M = Ta) quantitatively. The crystal structures of the niobium(V) and tantalum(V) chloro derivatives <ce:bold>5a,b</ce:bold>
reveal a ‘conventional’ <ce:italic>η</ce:italic>
<ce:sup loc="post">5</ce:sup>
:<ce:italic>η</ce:italic>
<ce:sup loc="post">5</ce:sup>
-coordination for the chelating bis(cyclopentadienyl) ligand. Protonolysis of <ce:bold>4a,b</ce:bold>
with [NHMe<ce:inf loc="post">3</ce:inf>
][B(C<ce:inf loc="post">6</ce:inf>
H<ce:inf loc="post">5</ce:inf>
)<ce:inf loc="post">4</ce:inf>
] afforded the first cationic <ce:italic>ansa</ce:italic>
-metallocenes [C<ce:inf loc="post">5</ce:inf>
H<ce:inf loc="post">4</ce:inf>
-C(CH<ce:inf loc="post">3</ce:inf>
)<ce:inf loc="post">2</ce:inf>
-C<ce:inf loc="post">5</ce:inf>
H<ce:inf loc="post">4</ce:inf>
]M[=N(2,6-<ce:sup loc="post">i</ce:sup>
Pr<ce:inf loc="post">2</ce:inf>
C<ce:inf loc="post">6</ce:inf>
H<ce:inf loc="post">3</ce:inf>
)][NH(CH<ce:inf loc="post">3</ce:inf>
)<ce:inf loc="post">2</ce:inf>
][B(C<ce:inf loc="post">6</ce:inf>
H<ce:inf loc="post">5</ce:inf>
)<ce:inf loc="post">4</ce:inf>
] (<ce:bold>6a</ce:bold>
, M = Nb; <ce:bold>6b</ce:bold>
, M = Ta) in high yields. The crystal structure of <ce:bold>6a</ce:bold>
shows an <ce:italic>η</ce:italic>
<ce:sup loc="post">5</ce:sup>
:<ce:italic>η</ce:italic>
<ce:sup loc="post">5</ce:sup>
-coordination mode for the bis(cyclopentadienyl) ligand. The <ce:sup loc="post">1</ce:sup>
<ce:italic>J</ce:italic>
(C,H) coupling constants of the bis(cyclopentadienyl) ligand of the <ce:italic>ansa</ce:italic>
-metallocenes <ce:bold>4a,b</ce:bold>
, <ce:bold>5a,b</ce:bold>
and <ce:bold>6a,b</ce:bold>
are related to its hapticity, which is a result of the electronic properties of the metal center.</ce:simple-para>
</ce:abstract-sec>
</ce:abstract>
<ce:keywords class="keyword" xml:lang="en"><ce:section-title>Keywords</ce:section-title>
<ce:keyword><ce:text>Multiple bonds</ce:text>
</ce:keyword>
<ce:keyword><ce:text>Niobium (V)</ce:text>
</ce:keyword>
<ce:keyword><ce:text>Tantalum (V)</ce:text>
</ce:keyword>
</ce:keywords>
</head>
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<abstract lang="en">The metal amide route has been exploited to synthesize η5:η1- and η5:η5 ansa-metallocenes of pentavalent niobium and tantalum. Tris(dimethylamido)(2,6-diisopropylphenylimido)-niobium(V) 2a and -tantalum(V) 2b were found to be appropriate starting compounds to cleanly react with CH-acidic ligand precursors such as cyclopentadiene and 2,2-bis(cyclopentadienyl)propane. In the latter case, the novel ansa-metallocenes of formula [C5H4-C(CH3)2-C5H4]M[=N(2,6-iPr2C6H3)][N(CH3)2] (4a, M = Nb; 4b, M = Ta) result in high yields. While the hydrocarbon ligand adopts an η1:η5-coordination to the metals in the solid state (X-ray diffraction studies), a rapid η1:η5-η5:η1 equilibration occurs in solution. Complexes 4a,b react promptly with (CH3)3SiCl, thus affording the ansa-metallocenes [C5H4-C(CH3)2-C5H4]M[-N(2,6-iPr2C6H3)]Cl (5a, M = Nb; 5b, M = Ta) quantitatively. The crystal structures of the niobium(V) and tantalum(V) chloro derivatives 5a,b reveal a ‘conventional’ η5:η5-coordination for the chelating bis(cyclopentadienyl) ligand. Protonolysis of 4a,b with [NHMe3][B(C6H5)4] afforded the first cationic ansa-metallocenes [C5H4-C(CH3)2-C5H4]M[=N(2,6-iPr2C6H3)][NH(CH3)2][B(C6H5)4] (6a, M = Nb; 6b, M = Ta) in high yields. The crystal structure of 6a shows an η5:η5-coordination mode for the bis(cyclopentadienyl) ligand. The 1J(C,H) coupling constants of the bis(cyclopentadienyl) ligand of the ansa-metallocenes 4a,b, 5a,b and 6a,b are related to its hapticity, which is a result of the electronic properties of the metal center.</abstract>
<note>For the preceding communication, no. 156 of this series, see Ref. [1].</note>
<subject lang="en"><genre>Keywords</genre>
<topic>Multiple bonds</topic>
<topic>Niobium (V)</topic>
<topic>Tantalum (V)</topic>
</subject>
<relatedItem type="host"><titleInfo><title>Journal of Organometallic Chemistry</title>
</titleInfo>
<titleInfo type="abbreviated"><title>JOM</title>
</titleInfo>
<genre type="Journal">journal</genre>
<originInfo><dateIssued encoding="w3cdtf">19970815</dateIssued>
</originInfo>
<identifier type="ISSN">0022-328X</identifier>
<identifier type="PII">S0022-328X(00)X1452-0</identifier>
<part><date>19970815</date>
<detail type="volume"><number>541</number>
<caption>vol.</caption>
</detail>
<detail type="issue"><number>1–2</number>
<caption>no.</caption>
</detail>
<extent unit="issue pages"><start>1</start>
<end>482</end>
</extent>
<extent unit="pages"><start>445</start>
<end>460</end>
</extent>
</part>
</relatedItem>
<identifier type="istex">41CB0416E99360E9FA83347C4AC6662777E99448</identifier>
<identifier type="DOI">10.1016/S0022-328X(97)00121-6</identifier>
<identifier type="PII">S0022-328X(97)00121-6</identifier>
<identifier type="ArticleID">97001216</identifier>
<accessCondition type="use and reproduction" contentType="">© 1997Elsevier Science S.A.</accessCondition>
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<recordOrigin>Elsevier Science S.A., ©1997</recordOrigin>
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