Terminal dysprosium and holmium organoimides
Terminal rare-earth-metal imide complexes Tp t Bu,Me Ln(NC 6 H 3 iPr 2 -2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized via double methane elimination of Lewis acid stabilized dialkyl precursors Tp t Bu,Me LnMe(GaMe 4 ) with primary aniline derivative H 2 NC 6...
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Published in | Chemical science (Cambridge) Vol. 15; no. 1; pp. 3562 - 357 |
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Main Authors | , , , |
Format | Journal Article |
Language | English |
Published |
England
Royal Society of Chemistry
06.03.2024
The Royal Society of Chemistry |
Subjects | |
Online Access | Get full text |
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Abstract | Terminal rare-earth-metal imide complexes Tp
t
Bu,Me
Ln(NC
6
H
3
iPr
2
-2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized
via
double methane elimination of Lewis acid stabilized dialkyl precursors Tp
t
Bu,Me
LnMe(GaMe
4
) with primary aniline derivative H
2
NC
6
H
3
iPr
2
-2,6 (H
2
NAr
iPr
). Exploiting the weaker Ln-CH
3
[GaMe
3
] interaction compared to the aluminium congener, addition of the aniline derivative leads to the mixed methyl/anilido species Tp
t
Bu,Me
LnMe(HNAr
iPr
) which readily eliminate methane after being exposed to the Lewis base DMAP (&z.dbd;
N
,
N
-dimethyl-4-aminopyridine). Under the same conditions, [AlMe
3
]-stabilized dimethyl rare-earth-metal complexes transform immediately to Lewis acid bridged imides Tp
t
Bu,Me
Ln(μ
2
-NC
6
H
3
Me
2
-2,6)(μ
2
-Me)AlMe
2
(Ln = Dy, Ho). DMAP/THF donor exchange is accomplished by treatment of Tp
t
Bu,Me
Ln(NC
6
H
3
iPr
2
-2,6)(dmap) with 9-BBN in THF while the terminal imides readily insert carbon dioxide to afford carbamate complexes.
Tp
t
Bu,Me
Ln(&z.dbd;NC
6
H
3
iPr
2
-2,6)(dmap) (Ln = Dy, Ho) display the first terminal imides of open-shell mid-sized lanthanides, exhibiting reactivity similar to Chen's seminal scandium terminal imide. |
---|---|
AbstractList | Terminal rare-earth-metal imide complexes TptBu,MeLn(NC6H3iPr2-2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized via double methane elimination of Lewis acid stabilized dialkyl precursors TptBu,MeLnMe(GaMe4) with primary aniline derivative H2NC6H3iPr2-2,6 (H2NAriPr). Exploiting the weaker Ln–CH3⋯[GaMe3] interaction compared to the aluminium congener, addition of the aniline derivative leads to the mixed methyl/anilido species TptBu,MeLnMe(HNAriPr) which readily eliminate methane after being exposed to the Lewis base DMAP (=N,N-dimethyl-4-aminopyridine). Under the same conditions, [AlMe3]-stabilized dimethyl rare-earth-metal complexes transform immediately to Lewis acid bridged imides TptBu,MeLn(μ2-NC6H3Me2-2,6)(μ2-Me)AlMe2 (Ln = Dy, Ho). DMAP/THF donor exchange is accomplished by treatment of TptBu,MeLn(NC6H3iPr2-2,6)(dmap) with 9-BBN in THF while the terminal imides readily insert carbon dioxide to afford carbamate complexes. Terminal rare-earth-metal imide complexes TptBu,MeLn(NC6H3iPr2-2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized via double methane elimination of Lewis acid stabilized dialkyl precursors TptBu,MeLnMe(GaMe4) with primary aniline derivative H2NC6H3iPr2-2,6 (H2NAriPr). Exploiting the weaker Ln-CH3⋯[GaMe3] interaction compared to the aluminium congener, addition of the aniline derivative leads to the mixed methyl/anilido species TptBu,MeLnMe(HNAriPr) which readily eliminate methane after being exposed to the Lewis base DMAP ([double bond, length as m-dash]N,N-dimethyl-4-aminopyridine). Under the same conditions, [AlMe3]-stabilized dimethyl rare-earth-metal complexes transform immediately to Lewis acid bridged imides TptBu,MeLn(μ2-NC6H3Me2-2,6)(μ2-Me)AlMe2 (Ln = Dy, Ho). DMAP/THF donor exchange is accomplished by treatment of TptBu,MeLn(NC6H3iPr2-2,6)(dmap) with 9-BBN in THF while the terminal imides readily insert carbon dioxide to afford carbamate complexes. Terminal rare-earth-metal imide complexes Tp t Bu,Me Ln(NC 6 H 3 iPr 2 -2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized via double methane elimination of Lewis acid stabilized dialkyl precursors Tp t Bu,Me LnMe(GaMe 4 ) with primary aniline derivative H 2 NC 6 H 3 iPr 2 -2,6 (H 2 NAr iPr ). Exploiting the weaker Ln–CH 3 ⋯[GaMe 3 ] interaction compared to the aluminium congener, addition of the aniline derivative leads to the mixed methyl/anilido species Tp t Bu,Me LnMe(HNAr iPr ) which readily eliminate methane after being exposed to the Lewis base DMAP ( Created by potrace 1.16, written by Peter Selinger 2001-2019 N , N -dimethyl-4-aminopyridine). Under the same conditions, [AlMe 3 ]-stabilized dimethyl rare-earth-metal complexes transform immediately to Lewis acid bridged imides Tp t Bu,Me Ln(μ 2 -NC 6 H 3 Me 2 -2,6)(μ 2 -Me)AlMe 2 (Ln = Dy, Ho). DMAP/THF donor exchange is accomplished by treatment of Tp t Bu,Me Ln(NC 6 H 3 iPr 2 -2,6)(dmap) with 9-BBN in THF while the terminal imides readily insert carbon dioxide to afford carbamate complexes. Tp t Bu,Me Ln( NC 6 H 3 iPr 2 -2,6)(dmap) (Ln = Dy, Ho) display the first terminal imides of open-shell mid-sized lanthanides, exhibiting reactivity similar to Chen's seminal scandium terminal imide. Terminal rare-earth-metal imide complexes Tp t Bu,Me Ln(NC 6 H 3 iPr 2 -2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized via double methane elimination of Lewis acid stabilized dialkyl precursors Tp t Bu,Me LnMe(GaMe 4 ) with primary aniline derivative H 2 NC 6 H 3 iPr 2 -2,6 (H 2 NAr iPr ). Exploiting the weaker Ln-CH 3 [GaMe 3 ] interaction compared to the aluminium congener, addition of the aniline derivative leads to the mixed methyl/anilido species Tp t Bu,Me LnMe(HNAr iPr ) which readily eliminate methane after being exposed to the Lewis base DMAP (&z.dbd; N , N -dimethyl-4-aminopyridine). Under the same conditions, [AlMe 3 ]-stabilized dimethyl rare-earth-metal complexes transform immediately to Lewis acid bridged imides Tp t Bu,Me Ln(μ 2 -NC 6 H 3 Me 2 -2,6)(μ 2 -Me)AlMe 2 (Ln = Dy, Ho). DMAP/THF donor exchange is accomplished by treatment of Tp t Bu,Me Ln(NC 6 H 3 iPr 2 -2,6)(dmap) with 9-BBN in THF while the terminal imides readily insert carbon dioxide to afford carbamate complexes. Tp t Bu,Me Ln(&z.dbd;NC 6 H 3 iPr 2 -2,6)(dmap) (Ln = Dy, Ho) display the first terminal imides of open-shell mid-sized lanthanides, exhibiting reactivity similar to Chen's seminal scandium terminal imide. Terminal rare-earth-metal imide complexes Tp t Bu,Me Ln(NC 6 H 3 iPr 2 -2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized via double methane elimination of Lewis acid stabilized dialkyl precursors Tp t Bu,Me LnMe(GaMe 4 ) with primary aniline derivative H 2 NC 6 H 3 iPr 2 -2,6 (H 2 NAr iPr ). Exploiting the weaker Ln–CH 3 ⋯[GaMe 3 ] interaction compared to the aluminium congener, addition of the aniline derivative leads to the mixed methyl/anilido species Tp t Bu,Me LnMe(HNAr iPr ) which readily eliminate methane after being exposed to the Lewis base DMAP ( N , N -dimethyl-4-aminopyridine). Under the same conditions, [AlMe 3 ]-stabilized dimethyl rare-earth-metal complexes transform immediately to Lewis acid bridged imides Tp t Bu,Me Ln(μ 2 -NC 6 H 3 Me 2 -2,6)(μ 2 -Me)AlMe 2 (Ln = Dy, Ho). DMAP/THF donor exchange is accomplished by treatment of Tp t Bu,Me Ln(NC 6 H 3 iPr 2 -2,6)(dmap) with 9-BBN in THF while the terminal imides readily insert carbon dioxide to afford carbamate complexes. Terminal rare-earth-metal imide complexes Tp Ln(NC H iPr -2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized double methane elimination of Lewis acid stabilized dialkyl precursors Tp LnMe(GaMe ) with primary aniline derivative H NC H iPr -2,6 (H NAr ). Exploiting the weaker Ln-CH ⋯[GaMe ] interaction compared to the aluminium congener, addition of the aniline derivative leads to the mixed methyl/anilido species Tp LnMe(HNAr ) which readily eliminate methane after being exposed to the Lewis base DMAP ([double bond, length as m-dash] , -dimethyl-4-aminopyridine). Under the same conditions, [AlMe ]-stabilized dimethyl rare-earth-metal complexes transform immediately to Lewis acid bridged imides Tp Ln(μ -NC H Me -2,6)(μ -Me)AlMe (Ln = Dy, Ho). DMAP/THF donor exchange is accomplished by treatment of Tp Ln(NC H iPr -2,6)(dmap) with 9-BBN in THF while the terminal imides readily insert carbon dioxide to afford carbamate complexes. |
Author | Schädle, Dorothea Rieser, Theresa E Anwander, Reiner Maichle-Mössmer, Cäcilia |
AuthorAffiliation | Institut für Anorganische Chemie Eberhard Karls Universität Tübingen |
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Author_xml | – sequence: 1 givenname: Theresa E surname: Rieser fullname: Rieser, Theresa E – sequence: 2 givenname: Dorothea surname: Schädle fullname: Schädle, Dorothea – sequence: 3 givenname: Cäcilia surname: Maichle-Mössmer fullname: Maichle-Mössmer, Cäcilia – sequence: 4 givenname: Reiner surname: Anwander fullname: Anwander, Reiner |
BackLink | https://www.ncbi.nlm.nih.gov/pubmed/38455031$$D View this record in MEDLINE/PubMed |
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CitedBy_id | crossref_primary_10_1039_D4CC02244K crossref_primary_10_1002_chem_202401687 crossref_primary_10_1021_acs_inorgchem_3c04422 |
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Snippet | Terminal rare-earth-metal imide complexes Tp
t
Bu,Me
Ln(NC
6
H
3
iPr
2
-2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized... Terminal rare-earth-metal imide complexes Tp Ln(NC H iPr -2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized double methane... Terminal rare-earth-metal imide complexes TptBu,MeLn(NC6H3iPr2-2,6)(dmap) of the mid-late rare-earth elements dysprosium and holmium were synthesized via... |
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StartPage | 3562 |
SubjectTerms | Aniline Carbon dioxide Chemistry Coordination compounds Dysprosium Holmium Imides Lewis acid Lewis base Methane Rare earth elements |
Title | Terminal dysprosium and holmium organoimides |
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