Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity
The synthesis, characterization, and reactivity of several new Cr(II) and Cr(III) complexes featuring an NCN pincer ligand with an arene backbone connected to amine donors $ NEt_{2} $ and Ni$ Pr_{2} $ via $ CH_{2} $-linkers is described. Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH...
Ausführliche Beschreibung
Gespeichert in:
| Autor*in: |
Käfer, Matthias G. [verfasserIn] |
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| Format: |
E-Artikel |
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| Sprache: |
Englisch |
| Erschienen: |
2023 |
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| Schlagwörter: |
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| Anmerkung: |
© The Author(s) 2023 |
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| Übergeordnetes Werk: |
Enthalten in: Monatshefte für Chemie - Wien [u.a.] : Springer, 1880, 154(2023), 11 vom: 10. Okt., Seite 1263-1273 |
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| Übergeordnetes Werk: |
volume:154 ; year:2023 ; number:11 ; day:10 ; month:10 ; pages:1263-1273 |
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| DOI / URN: |
10.1007/s00706-023-03128-6 |
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| Katalog-ID: |
SPR053597931 |
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| 041 | |a eng | ||
| 100 | 1 | |a Käfer, Matthias G. |e verfasserin |0 (orcid)0009-0006-4395-0286 |4 aut | |
| 245 | 1 | 0 | |a Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity |
| 264 | 1 | |c 2023 | |
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| 337 | |a Computermedien |b c |2 rdamedia | ||
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| 500 | |a © The Author(s) 2023 | ||
| 520 | |a The synthesis, characterization, and reactivity of several new Cr(II) and Cr(III) complexes featuring an NCN pincer ligand with an arene backbone connected to amine donors $ NEt_{2} $ and Ni$ Pr_{2} $ via $ CH_{2} $-linkers is described. Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH2} $-Et with [$ CrCl_{3} $(THF)3] resulted in the formation of the Cr(III) complex trans-[Cr($ κ^{3} $NCN-$ NCN^{CH2} $-Et)(Cl)2(THF)]. Upon reaction of lithiated N(C–Br)$ N^{CH2} $-iPr with a suspension of anhydrous $ CrCl_{2} $, the Cr(II) complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)2] is formed featuring two NCN ligands bound in $ κ^{2} $NC-fashion. In contrast, when lithiated N(C–Br)$ N^{CH2} $-iPr is reacted with a homogeneous solution of anhydrous CrX2 (X = Cl, Br), complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)X] are obtained. Treatment of [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)Cl] with 1 equiv of $ PhCH_{2} $MgCl and $ LiCH_{2} %$ SiMe_{3} $ afforded the alkyl complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} $Ph)] and [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)]. All Cr(II) complexes exhibit effective magnetic moments in the range of 4.7–4.9 µB which is indicative for d4 high spin systems. If a solution of lithiated N(C–Br)$ N^{CH2} $-iPr is treated with $ CrCl_{2} $, followed by addition of an excess of Na[HB(Et)3], the dimeric complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)($ μ_{2} $-H)]2 is obtained bearing two bridging hydride ligands. [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)] turned out to be catalytically active for the hydrosilylation of ketones at room temperature with a catalyst loading of 1 mol%. X-ray structures of all complexes are presented. Graphical abstract | ||
| 650 | 4 | |a Pincer complexes |7 (dpeaa)DE-He213 | |
| 650 | 4 | |a Chromium |7 (dpeaa)DE-He213 | |
| 650 | 4 | |a Hydrosilylation |7 (dpeaa)DE-He213 | |
| 650 | 4 | |a Silanes |7 (dpeaa)DE-He213 | |
| 650 | 4 | |a Ketones |7 (dpeaa)DE-He213 | |
| 700 | 1 | |a Eder, Wolfgang |0 (orcid)0000-0001-7494-1098 |4 aut | |
| 700 | 1 | |a Pecak, Jan |4 aut | |
| 700 | 1 | |a Stöger, Berthold |0 (orcid)0000-0002-0087-474X |4 aut | |
| 700 | 1 | |a Pignitter, Marc |4 aut | |
| 700 | 1 | |a Veiros, Luis F. |4 aut | |
| 700 | 1 | |a Kirchner, Karl |0 (orcid)0000-0003-0872-6159 |4 aut | |
| 773 | 0 | 8 | |i Enthalten in |t Monatshefte für Chemie |d Wien [u.a.] : Springer, 1880 |g 154(2023), 11 vom: 10. Okt., Seite 1263-1273 |w (DE-627)25462992X |w (DE-600)1462037-6 |x 1434-4475 |7 nnns |
| 773 | 1 | 8 | |g volume:154 |g year:2023 |g number:11 |g day:10 |g month:10 |g pages:1263-1273 |
| 856 | 4 | 0 | |u https://dx.doi.org/10.1007/s00706-023-03128-6 |z kostenfrei |3 Volltext |
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10.1007/s00706-023-03128-6 doi (DE-627)SPR053597931 (SPR)s00706-023-03128-6-e DE-627 ger DE-627 rakwb eng Käfer, Matthias G. verfasserin (orcid)0009-0006-4395-0286 aut Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity 2023 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier © The Author(s) 2023 The synthesis, characterization, and reactivity of several new Cr(II) and Cr(III) complexes featuring an NCN pincer ligand with an arene backbone connected to amine donors $ NEt_{2} $ and Ni$ Pr_{2} $ via $ CH_{2} $-linkers is described. Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH2} $-Et with [$ CrCl_{3} $(THF)3] resulted in the formation of the Cr(III) complex trans-[Cr($ κ^{3} $NCN-$ NCN^{CH2} $-Et)(Cl)2(THF)]. Upon reaction of lithiated N(C–Br)$ N^{CH2} $-iPr with a suspension of anhydrous $ CrCl_{2} $, the Cr(II) complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)2] is formed featuring two NCN ligands bound in $ κ^{2} $NC-fashion. In contrast, when lithiated N(C–Br)$ N^{CH2} $-iPr is reacted with a homogeneous solution of anhydrous CrX2 (X = Cl, Br), complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)X] are obtained. Treatment of [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)Cl] with 1 equiv of $ PhCH_{2} $MgCl and $ LiCH_{2} %$ SiMe_{3} $ afforded the alkyl complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} $Ph)] and [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)]. All Cr(II) complexes exhibit effective magnetic moments in the range of 4.7–4.9 µB which is indicative for d4 high spin systems. If a solution of lithiated N(C–Br)$ N^{CH2} $-iPr is treated with $ CrCl_{2} $, followed by addition of an excess of Na[HB(Et)3], the dimeric complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)($ μ_{2} $-H)]2 is obtained bearing two bridging hydride ligands. [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)] turned out to be catalytically active for the hydrosilylation of ketones at room temperature with a catalyst loading of 1 mol%. X-ray structures of all complexes are presented. Graphical abstract Pincer complexes (dpeaa)DE-He213 Chromium (dpeaa)DE-He213 Hydrosilylation (dpeaa)DE-He213 Silanes (dpeaa)DE-He213 Ketones (dpeaa)DE-He213 Eder, Wolfgang (orcid)0000-0001-7494-1098 aut Pecak, Jan aut Stöger, Berthold (orcid)0000-0002-0087-474X aut Pignitter, Marc aut Veiros, Luis F. aut Kirchner, Karl (orcid)0000-0003-0872-6159 aut Enthalten in Monatshefte für Chemie Wien [u.a.] : Springer, 1880 154(2023), 11 vom: 10. Okt., Seite 1263-1273 (DE-627)25462992X (DE-600)1462037-6 1434-4475 nnns volume:154 year:2023 number:11 day:10 month:10 pages:1263-1273 https://dx.doi.org/10.1007/s00706-023-03128-6 kostenfrei Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_120 GBV_ILN_138 GBV_ILN_150 GBV_ILN_151 GBV_ILN_152 GBV_ILN_161 GBV_ILN_170 GBV_ILN_171 GBV_ILN_187 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_250 GBV_ILN_267 GBV_ILN_281 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_636 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2006 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2031 GBV_ILN_2034 GBV_ILN_2037 GBV_ILN_2038 GBV_ILN_2039 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2057 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2065 GBV_ILN_2068 GBV_ILN_2088 GBV_ILN_2093 GBV_ILN_2106 GBV_ILN_2107 GBV_ILN_2108 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2113 GBV_ILN_2118 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2144 GBV_ILN_2147 GBV_ILN_2148 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2188 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2446 GBV_ILN_2470 GBV_ILN_2472 GBV_ILN_2507 GBV_ILN_2522 GBV_ILN_2548 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4046 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4242 GBV_ILN_4246 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4328 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4335 GBV_ILN_4336 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 AR 154 2023 11 10 10 1263-1273 |
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10.1007/s00706-023-03128-6 doi (DE-627)SPR053597931 (SPR)s00706-023-03128-6-e DE-627 ger DE-627 rakwb eng Käfer, Matthias G. verfasserin (orcid)0009-0006-4395-0286 aut Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity 2023 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier © The Author(s) 2023 The synthesis, characterization, and reactivity of several new Cr(II) and Cr(III) complexes featuring an NCN pincer ligand with an arene backbone connected to amine donors $ NEt_{2} $ and Ni$ Pr_{2} $ via $ CH_{2} $-linkers is described. Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH2} $-Et with [$ CrCl_{3} $(THF)3] resulted in the formation of the Cr(III) complex trans-[Cr($ κ^{3} $NCN-$ NCN^{CH2} $-Et)(Cl)2(THF)]. Upon reaction of lithiated N(C–Br)$ N^{CH2} $-iPr with a suspension of anhydrous $ CrCl_{2} $, the Cr(II) complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)2] is formed featuring two NCN ligands bound in $ κ^{2} $NC-fashion. In contrast, when lithiated N(C–Br)$ N^{CH2} $-iPr is reacted with a homogeneous solution of anhydrous CrX2 (X = Cl, Br), complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)X] are obtained. Treatment of [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)Cl] with 1 equiv of $ PhCH_{2} $MgCl and $ LiCH_{2} %$ SiMe_{3} $ afforded the alkyl complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} $Ph)] and [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)]. All Cr(II) complexes exhibit effective magnetic moments in the range of 4.7–4.9 µB which is indicative for d4 high spin systems. If a solution of lithiated N(C–Br)$ N^{CH2} $-iPr is treated with $ CrCl_{2} $, followed by addition of an excess of Na[HB(Et)3], the dimeric complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)($ μ_{2} $-H)]2 is obtained bearing two bridging hydride ligands. [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)] turned out to be catalytically active for the hydrosilylation of ketones at room temperature with a catalyst loading of 1 mol%. X-ray structures of all complexes are presented. Graphical abstract Pincer complexes (dpeaa)DE-He213 Chromium (dpeaa)DE-He213 Hydrosilylation (dpeaa)DE-He213 Silanes (dpeaa)DE-He213 Ketones (dpeaa)DE-He213 Eder, Wolfgang (orcid)0000-0001-7494-1098 aut Pecak, Jan aut Stöger, Berthold (orcid)0000-0002-0087-474X aut Pignitter, Marc aut Veiros, Luis F. aut Kirchner, Karl (orcid)0000-0003-0872-6159 aut Enthalten in Monatshefte für Chemie Wien [u.a.] : Springer, 1880 154(2023), 11 vom: 10. Okt., Seite 1263-1273 (DE-627)25462992X (DE-600)1462037-6 1434-4475 nnns volume:154 year:2023 number:11 day:10 month:10 pages:1263-1273 https://dx.doi.org/10.1007/s00706-023-03128-6 kostenfrei Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_120 GBV_ILN_138 GBV_ILN_150 GBV_ILN_151 GBV_ILN_152 GBV_ILN_161 GBV_ILN_170 GBV_ILN_171 GBV_ILN_187 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_250 GBV_ILN_267 GBV_ILN_281 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_636 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2006 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2031 GBV_ILN_2034 GBV_ILN_2037 GBV_ILN_2038 GBV_ILN_2039 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2057 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2065 GBV_ILN_2068 GBV_ILN_2088 GBV_ILN_2093 GBV_ILN_2106 GBV_ILN_2107 GBV_ILN_2108 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2113 GBV_ILN_2118 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2144 GBV_ILN_2147 GBV_ILN_2148 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2188 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2446 GBV_ILN_2470 GBV_ILN_2472 GBV_ILN_2507 GBV_ILN_2522 GBV_ILN_2548 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4046 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4242 GBV_ILN_4246 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4328 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4335 GBV_ILN_4336 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 AR 154 2023 11 10 10 1263-1273 |
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10.1007/s00706-023-03128-6 doi (DE-627)SPR053597931 (SPR)s00706-023-03128-6-e DE-627 ger DE-627 rakwb eng Käfer, Matthias G. verfasserin (orcid)0009-0006-4395-0286 aut Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity 2023 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier © The Author(s) 2023 The synthesis, characterization, and reactivity of several new Cr(II) and Cr(III) complexes featuring an NCN pincer ligand with an arene backbone connected to amine donors $ NEt_{2} $ and Ni$ Pr_{2} $ via $ CH_{2} $-linkers is described. Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH2} $-Et with [$ CrCl_{3} $(THF)3] resulted in the formation of the Cr(III) complex trans-[Cr($ κ^{3} $NCN-$ NCN^{CH2} $-Et)(Cl)2(THF)]. Upon reaction of lithiated N(C–Br)$ N^{CH2} $-iPr with a suspension of anhydrous $ CrCl_{2} $, the Cr(II) complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)2] is formed featuring two NCN ligands bound in $ κ^{2} $NC-fashion. In contrast, when lithiated N(C–Br)$ N^{CH2} $-iPr is reacted with a homogeneous solution of anhydrous CrX2 (X = Cl, Br), complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)X] are obtained. Treatment of [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)Cl] with 1 equiv of $ PhCH_{2} $MgCl and $ LiCH_{2} %$ SiMe_{3} $ afforded the alkyl complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} $Ph)] and [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)]. All Cr(II) complexes exhibit effective magnetic moments in the range of 4.7–4.9 µB which is indicative for d4 high spin systems. If a solution of lithiated N(C–Br)$ N^{CH2} $-iPr is treated with $ CrCl_{2} $, followed by addition of an excess of Na[HB(Et)3], the dimeric complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)($ μ_{2} $-H)]2 is obtained bearing two bridging hydride ligands. [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)] turned out to be catalytically active for the hydrosilylation of ketones at room temperature with a catalyst loading of 1 mol%. X-ray structures of all complexes are presented. Graphical abstract Pincer complexes (dpeaa)DE-He213 Chromium (dpeaa)DE-He213 Hydrosilylation (dpeaa)DE-He213 Silanes (dpeaa)DE-He213 Ketones (dpeaa)DE-He213 Eder, Wolfgang (orcid)0000-0001-7494-1098 aut Pecak, Jan aut Stöger, Berthold (orcid)0000-0002-0087-474X aut Pignitter, Marc aut Veiros, Luis F. aut Kirchner, Karl (orcid)0000-0003-0872-6159 aut Enthalten in Monatshefte für Chemie Wien [u.a.] : Springer, 1880 154(2023), 11 vom: 10. Okt., Seite 1263-1273 (DE-627)25462992X (DE-600)1462037-6 1434-4475 nnns volume:154 year:2023 number:11 day:10 month:10 pages:1263-1273 https://dx.doi.org/10.1007/s00706-023-03128-6 kostenfrei Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_120 GBV_ILN_138 GBV_ILN_150 GBV_ILN_151 GBV_ILN_152 GBV_ILN_161 GBV_ILN_170 GBV_ILN_171 GBV_ILN_187 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_250 GBV_ILN_267 GBV_ILN_281 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_636 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2006 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2031 GBV_ILN_2034 GBV_ILN_2037 GBV_ILN_2038 GBV_ILN_2039 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2057 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2065 GBV_ILN_2068 GBV_ILN_2088 GBV_ILN_2093 GBV_ILN_2106 GBV_ILN_2107 GBV_ILN_2108 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2113 GBV_ILN_2118 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2144 GBV_ILN_2147 GBV_ILN_2148 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2188 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2446 GBV_ILN_2470 GBV_ILN_2472 GBV_ILN_2507 GBV_ILN_2522 GBV_ILN_2548 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4046 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4242 GBV_ILN_4246 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4328 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4335 GBV_ILN_4336 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 AR 154 2023 11 10 10 1263-1273 |
| allfieldsGer |
10.1007/s00706-023-03128-6 doi (DE-627)SPR053597931 (SPR)s00706-023-03128-6-e DE-627 ger DE-627 rakwb eng Käfer, Matthias G. verfasserin (orcid)0009-0006-4395-0286 aut Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity 2023 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier © The Author(s) 2023 The synthesis, characterization, and reactivity of several new Cr(II) and Cr(III) complexes featuring an NCN pincer ligand with an arene backbone connected to amine donors $ NEt_{2} $ and Ni$ Pr_{2} $ via $ CH_{2} $-linkers is described. Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH2} $-Et with [$ CrCl_{3} $(THF)3] resulted in the formation of the Cr(III) complex trans-[Cr($ κ^{3} $NCN-$ NCN^{CH2} $-Et)(Cl)2(THF)]. Upon reaction of lithiated N(C–Br)$ N^{CH2} $-iPr with a suspension of anhydrous $ CrCl_{2} $, the Cr(II) complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)2] is formed featuring two NCN ligands bound in $ κ^{2} $NC-fashion. In contrast, when lithiated N(C–Br)$ N^{CH2} $-iPr is reacted with a homogeneous solution of anhydrous CrX2 (X = Cl, Br), complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)X] are obtained. Treatment of [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)Cl] with 1 equiv of $ PhCH_{2} $MgCl and $ LiCH_{2} %$ SiMe_{3} $ afforded the alkyl complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} $Ph)] and [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)]. All Cr(II) complexes exhibit effective magnetic moments in the range of 4.7–4.9 µB which is indicative for d4 high spin systems. If a solution of lithiated N(C–Br)$ N^{CH2} $-iPr is treated with $ CrCl_{2} $, followed by addition of an excess of Na[HB(Et)3], the dimeric complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)($ μ_{2} $-H)]2 is obtained bearing two bridging hydride ligands. [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)] turned out to be catalytically active for the hydrosilylation of ketones at room temperature with a catalyst loading of 1 mol%. X-ray structures of all complexes are presented. Graphical abstract Pincer complexes (dpeaa)DE-He213 Chromium (dpeaa)DE-He213 Hydrosilylation (dpeaa)DE-He213 Silanes (dpeaa)DE-He213 Ketones (dpeaa)DE-He213 Eder, Wolfgang (orcid)0000-0001-7494-1098 aut Pecak, Jan aut Stöger, Berthold (orcid)0000-0002-0087-474X aut Pignitter, Marc aut Veiros, Luis F. aut Kirchner, Karl (orcid)0000-0003-0872-6159 aut Enthalten in Monatshefte für Chemie Wien [u.a.] : Springer, 1880 154(2023), 11 vom: 10. Okt., Seite 1263-1273 (DE-627)25462992X (DE-600)1462037-6 1434-4475 nnns volume:154 year:2023 number:11 day:10 month:10 pages:1263-1273 https://dx.doi.org/10.1007/s00706-023-03128-6 kostenfrei Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_120 GBV_ILN_138 GBV_ILN_150 GBV_ILN_151 GBV_ILN_152 GBV_ILN_161 GBV_ILN_170 GBV_ILN_171 GBV_ILN_187 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_250 GBV_ILN_267 GBV_ILN_281 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_636 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2006 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2031 GBV_ILN_2034 GBV_ILN_2037 GBV_ILN_2038 GBV_ILN_2039 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2057 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2065 GBV_ILN_2068 GBV_ILN_2088 GBV_ILN_2093 GBV_ILN_2106 GBV_ILN_2107 GBV_ILN_2108 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2113 GBV_ILN_2118 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2144 GBV_ILN_2147 GBV_ILN_2148 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2188 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2446 GBV_ILN_2470 GBV_ILN_2472 GBV_ILN_2507 GBV_ILN_2522 GBV_ILN_2548 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4046 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4242 GBV_ILN_4246 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4328 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4335 GBV_ILN_4336 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 AR 154 2023 11 10 10 1263-1273 |
| allfieldsSound |
10.1007/s00706-023-03128-6 doi (DE-627)SPR053597931 (SPR)s00706-023-03128-6-e DE-627 ger DE-627 rakwb eng Käfer, Matthias G. verfasserin (orcid)0009-0006-4395-0286 aut Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity 2023 Text txt rdacontent Computermedien c rdamedia Online-Ressource cr rdacarrier © The Author(s) 2023 The synthesis, characterization, and reactivity of several new Cr(II) and Cr(III) complexes featuring an NCN pincer ligand with an arene backbone connected to amine donors $ NEt_{2} $ and Ni$ Pr_{2} $ via $ CH_{2} $-linkers is described. Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH2} $-Et with [$ CrCl_{3} $(THF)3] resulted in the formation of the Cr(III) complex trans-[Cr($ κ^{3} $NCN-$ NCN^{CH2} $-Et)(Cl)2(THF)]. Upon reaction of lithiated N(C–Br)$ N^{CH2} $-iPr with a suspension of anhydrous $ CrCl_{2} $, the Cr(II) complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)2] is formed featuring two NCN ligands bound in $ κ^{2} $NC-fashion. In contrast, when lithiated N(C–Br)$ N^{CH2} $-iPr is reacted with a homogeneous solution of anhydrous CrX2 (X = Cl, Br), complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)X] are obtained. Treatment of [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)Cl] with 1 equiv of $ PhCH_{2} $MgCl and $ LiCH_{2} %$ SiMe_{3} $ afforded the alkyl complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} $Ph)] and [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)]. All Cr(II) complexes exhibit effective magnetic moments in the range of 4.7–4.9 µB which is indicative for d4 high spin systems. If a solution of lithiated N(C–Br)$ N^{CH2} $-iPr is treated with $ CrCl_{2} $, followed by addition of an excess of Na[HB(Et)3], the dimeric complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)($ μ_{2} $-H)]2 is obtained bearing two bridging hydride ligands. [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)] turned out to be catalytically active for the hydrosilylation of ketones at room temperature with a catalyst loading of 1 mol%. X-ray structures of all complexes are presented. Graphical abstract Pincer complexes (dpeaa)DE-He213 Chromium (dpeaa)DE-He213 Hydrosilylation (dpeaa)DE-He213 Silanes (dpeaa)DE-He213 Ketones (dpeaa)DE-He213 Eder, Wolfgang (orcid)0000-0001-7494-1098 aut Pecak, Jan aut Stöger, Berthold (orcid)0000-0002-0087-474X aut Pignitter, Marc aut Veiros, Luis F. aut Kirchner, Karl (orcid)0000-0003-0872-6159 aut Enthalten in Monatshefte für Chemie Wien [u.a.] : Springer, 1880 154(2023), 11 vom: 10. Okt., Seite 1263-1273 (DE-627)25462992X (DE-600)1462037-6 1434-4475 nnns volume:154 year:2023 number:11 day:10 month:10 pages:1263-1273 https://dx.doi.org/10.1007/s00706-023-03128-6 kostenfrei Volltext GBV_USEFLAG_A SYSFLAG_A GBV_SPRINGER GBV_ILN_11 GBV_ILN_20 GBV_ILN_22 GBV_ILN_23 GBV_ILN_24 GBV_ILN_31 GBV_ILN_32 GBV_ILN_39 GBV_ILN_40 GBV_ILN_60 GBV_ILN_62 GBV_ILN_63 GBV_ILN_69 GBV_ILN_70 GBV_ILN_73 GBV_ILN_74 GBV_ILN_90 GBV_ILN_95 GBV_ILN_100 GBV_ILN_101 GBV_ILN_105 GBV_ILN_110 GBV_ILN_120 GBV_ILN_138 GBV_ILN_150 GBV_ILN_151 GBV_ILN_152 GBV_ILN_161 GBV_ILN_170 GBV_ILN_171 GBV_ILN_187 GBV_ILN_213 GBV_ILN_224 GBV_ILN_230 GBV_ILN_250 GBV_ILN_267 GBV_ILN_281 GBV_ILN_285 GBV_ILN_293 GBV_ILN_370 GBV_ILN_602 GBV_ILN_636 GBV_ILN_702 GBV_ILN_2001 GBV_ILN_2003 GBV_ILN_2004 GBV_ILN_2005 GBV_ILN_2006 GBV_ILN_2007 GBV_ILN_2008 GBV_ILN_2009 GBV_ILN_2010 GBV_ILN_2011 GBV_ILN_2014 GBV_ILN_2015 GBV_ILN_2020 GBV_ILN_2021 GBV_ILN_2025 GBV_ILN_2026 GBV_ILN_2027 GBV_ILN_2031 GBV_ILN_2034 GBV_ILN_2037 GBV_ILN_2038 GBV_ILN_2039 GBV_ILN_2044 GBV_ILN_2048 GBV_ILN_2049 GBV_ILN_2050 GBV_ILN_2055 GBV_ILN_2056 GBV_ILN_2057 GBV_ILN_2059 GBV_ILN_2061 GBV_ILN_2064 GBV_ILN_2065 GBV_ILN_2068 GBV_ILN_2088 GBV_ILN_2093 GBV_ILN_2106 GBV_ILN_2107 GBV_ILN_2108 GBV_ILN_2110 GBV_ILN_2111 GBV_ILN_2112 GBV_ILN_2113 GBV_ILN_2118 GBV_ILN_2122 GBV_ILN_2129 GBV_ILN_2143 GBV_ILN_2144 GBV_ILN_2147 GBV_ILN_2148 GBV_ILN_2152 GBV_ILN_2153 GBV_ILN_2188 GBV_ILN_2190 GBV_ILN_2232 GBV_ILN_2336 GBV_ILN_2446 GBV_ILN_2470 GBV_ILN_2472 GBV_ILN_2507 GBV_ILN_2522 GBV_ILN_2548 GBV_ILN_4035 GBV_ILN_4037 GBV_ILN_4046 GBV_ILN_4112 GBV_ILN_4125 GBV_ILN_4126 GBV_ILN_4242 GBV_ILN_4246 GBV_ILN_4249 GBV_ILN_4251 GBV_ILN_4305 GBV_ILN_4306 GBV_ILN_4307 GBV_ILN_4313 GBV_ILN_4322 GBV_ILN_4323 GBV_ILN_4324 GBV_ILN_4325 GBV_ILN_4326 GBV_ILN_4328 GBV_ILN_4333 GBV_ILN_4334 GBV_ILN_4335 GBV_ILN_4336 GBV_ILN_4338 GBV_ILN_4393 GBV_ILN_4700 AR 154 2023 11 10 10 1263-1273 |
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Enthalten in Monatshefte für Chemie 154(2023), 11 vom: 10. Okt., Seite 1263-1273 volume:154 year:2023 number:11 day:10 month:10 pages:1263-1273 |
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Enthalten in Monatshefte für Chemie 154(2023), 11 vom: 10. Okt., Seite 1263-1273 volume:154 year:2023 number:11 day:10 month:10 pages:1263-1273 |
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Pincer complexes Chromium Hydrosilylation Silanes Ketones |
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Monatshefte für Chemie |
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Käfer, Matthias G. @@aut@@ Eder, Wolfgang @@aut@@ Pecak, Jan @@aut@@ Stöger, Berthold @@aut@@ Pignitter, Marc @@aut@@ Veiros, Luis F. @@aut@@ Kirchner, Karl @@aut@@ |
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2023-10-10T00:00:00Z |
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Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH2} $-Et with [$ CrCl_{3} $(THF)3] resulted in the formation of the Cr(III) complex trans-[Cr($ κ^{3} $NCN-$ NCN^{CH2} $-Et)(Cl)2(THF)]. Upon reaction of lithiated N(C–Br)$ N^{CH2} $-iPr with a suspension of anhydrous $ CrCl_{2} $, the Cr(II) complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)2] is formed featuring two NCN ligands bound in $ κ^{2} $NC-fashion. In contrast, when lithiated N(C–Br)$ N^{CH2} $-iPr is reacted with a homogeneous solution of anhydrous CrX2 (X = Cl, Br), complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)X] are obtained. Treatment of [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)Cl] with 1 equiv of $ PhCH_{2} $MgCl and $ LiCH_{2} %$ SiMe_{3} $ afforded the alkyl complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} $Ph)] and [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)]. All Cr(II) complexes exhibit effective magnetic moments in the range of 4.7–4.9 µB which is indicative for d4 high spin systems. If a solution of lithiated N(C–Br)$ N^{CH2} $-iPr is treated with $ CrCl_{2} $, followed by addition of an excess of Na[HB(Et)3], the dimeric complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)($ μ_{2} $-H)]2 is obtained bearing two bridging hydride ligands. [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)] turned out to be catalytically active for the hydrosilylation of ketones at room temperature with a catalyst loading of 1 mol%. X-ray structures of all complexes are presented. 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| author |
Käfer, Matthias G. |
| spellingShingle |
Käfer, Matthias G. misc Pincer complexes misc Chromium misc Hydrosilylation misc Silanes misc Ketones Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity |
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Käfer, Matthias G. |
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Not Illustrated |
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1434-4475 |
| topic_title |
Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity Pincer complexes (dpeaa)DE-He213 Chromium (dpeaa)DE-He213 Hydrosilylation (dpeaa)DE-He213 Silanes (dpeaa)DE-He213 Ketones (dpeaa)DE-He213 |
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misc Pincer complexes misc Chromium misc Hydrosilylation misc Silanes misc Ketones |
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misc Pincer complexes misc Chromium misc Hydrosilylation misc Silanes misc Ketones |
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misc Pincer complexes misc Chromium misc Hydrosilylation misc Silanes misc Ketones |
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Elektronische Aufsätze Aufsätze Elektronische Ressource |
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Monatshefte für Chemie |
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Monatshefte für Chemie |
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Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity |
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(DE-627)SPR053597931 (SPR)s00706-023-03128-6-e |
| title_full |
Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity |
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Käfer, Matthias G. |
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Monatshefte für Chemie |
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Monatshefte für Chemie |
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Käfer, Matthias G. Eder, Wolfgang Pecak, Jan Stöger, Berthold Pignitter, Marc Veiros, Luis F. Kirchner, Karl |
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154 |
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Elektronische Aufsätze |
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Käfer, Matthias G. |
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10.1007/s00706-023-03128-6 |
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(ORCID)0009-0006-4395-0286 (ORCID)0000-0001-7494-1098 (ORCID)0000-0002-0087-474X (ORCID)0000-0003-0872-6159 |
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(orcid)0009-0006-4395-0286 (orcid)0000-0001-7494-1098 (orcid)0000-0002-0087-474X (orcid)0000-0003-0872-6159 |
| title_sort |
cr(ii) and cr(iii) ncn pincer complexes: synthesis, structure, and catalytic reactivity |
| title_auth |
Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity |
| abstract |
The synthesis, characterization, and reactivity of several new Cr(II) and Cr(III) complexes featuring an NCN pincer ligand with an arene backbone connected to amine donors $ NEt_{2} $ and Ni$ Pr_{2} $ via $ CH_{2} $-linkers is described. Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH2} $-Et with [$ CrCl_{3} $(THF)3] resulted in the formation of the Cr(III) complex trans-[Cr($ κ^{3} $NCN-$ NCN^{CH2} $-Et)(Cl)2(THF)]. Upon reaction of lithiated N(C–Br)$ N^{CH2} $-iPr with a suspension of anhydrous $ CrCl_{2} $, the Cr(II) complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)2] is formed featuring two NCN ligands bound in $ κ^{2} $NC-fashion. In contrast, when lithiated N(C–Br)$ N^{CH2} $-iPr is reacted with a homogeneous solution of anhydrous CrX2 (X = Cl, Br), complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)X] are obtained. Treatment of [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)Cl] with 1 equiv of $ PhCH_{2} $MgCl and $ LiCH_{2} %$ SiMe_{3} $ afforded the alkyl complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} $Ph)] and [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)]. All Cr(II) complexes exhibit effective magnetic moments in the range of 4.7–4.9 µB which is indicative for d4 high spin systems. If a solution of lithiated N(C–Br)$ N^{CH2} $-iPr is treated with $ CrCl_{2} $, followed by addition of an excess of Na[HB(Et)3], the dimeric complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)($ μ_{2} $-H)]2 is obtained bearing two bridging hydride ligands. [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)] turned out to be catalytically active for the hydrosilylation of ketones at room temperature with a catalyst loading of 1 mol%. X-ray structures of all complexes are presented. Graphical abstract © The Author(s) 2023 |
| abstractGer |
The synthesis, characterization, and reactivity of several new Cr(II) and Cr(III) complexes featuring an NCN pincer ligand with an arene backbone connected to amine donors $ NEt_{2} $ and Ni$ Pr_{2} $ via $ CH_{2} $-linkers is described. Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH2} $-Et with [$ CrCl_{3} $(THF)3] resulted in the formation of the Cr(III) complex trans-[Cr($ κ^{3} $NCN-$ NCN^{CH2} $-Et)(Cl)2(THF)]. Upon reaction of lithiated N(C–Br)$ N^{CH2} $-iPr with a suspension of anhydrous $ CrCl_{2} $, the Cr(II) complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)2] is formed featuring two NCN ligands bound in $ κ^{2} $NC-fashion. In contrast, when lithiated N(C–Br)$ N^{CH2} $-iPr is reacted with a homogeneous solution of anhydrous CrX2 (X = Cl, Br), complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)X] are obtained. Treatment of [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)Cl] with 1 equiv of $ PhCH_{2} $MgCl and $ LiCH_{2} %$ SiMe_{3} $ afforded the alkyl complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} $Ph)] and [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)]. All Cr(II) complexes exhibit effective magnetic moments in the range of 4.7–4.9 µB which is indicative for d4 high spin systems. If a solution of lithiated N(C–Br)$ N^{CH2} $-iPr is treated with $ CrCl_{2} $, followed by addition of an excess of Na[HB(Et)3], the dimeric complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)($ μ_{2} $-H)]2 is obtained bearing two bridging hydride ligands. [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)] turned out to be catalytically active for the hydrosilylation of ketones at room temperature with a catalyst loading of 1 mol%. X-ray structures of all complexes are presented. Graphical abstract © The Author(s) 2023 |
| abstract_unstemmed |
The synthesis, characterization, and reactivity of several new Cr(II) and Cr(III) complexes featuring an NCN pincer ligand with an arene backbone connected to amine donors $ NEt_{2} $ and Ni$ Pr_{2} $ via $ CH_{2} $-linkers is described. Reacting the in situ lithiated ligand precursor N(C–Br)$ N^{CH2} $-Et with [$ CrCl_{3} $(THF)3] resulted in the formation of the Cr(III) complex trans-[Cr($ κ^{3} $NCN-$ NCN^{CH2} $-Et)(Cl)2(THF)]. Upon reaction of lithiated N(C–Br)$ N^{CH2} $-iPr with a suspension of anhydrous $ CrCl_{2} $, the Cr(II) complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)2] is formed featuring two NCN ligands bound in $ κ^{2} $NC-fashion. In contrast, when lithiated N(C–Br)$ N^{CH2} $-iPr is reacted with a homogeneous solution of anhydrous CrX2 (X = Cl, Br), complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)X] are obtained. Treatment of [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)Cl] with 1 equiv of $ PhCH_{2} $MgCl and $ LiCH_{2} %$ SiMe_{3} $ afforded the alkyl complexes [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} $Ph)] and [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)]. All Cr(II) complexes exhibit effective magnetic moments in the range of 4.7–4.9 µB which is indicative for d4 high spin systems. If a solution of lithiated N(C–Br)$ N^{CH2} $-iPr is treated with $ CrCl_{2} $, followed by addition of an excess of Na[HB(Et)3], the dimeric complex [Cr($ κ^{2} $NC-$ NCN^{CH2} $-iPr)($ μ_{2} $-H)]2 is obtained bearing two bridging hydride ligands. [Cr($ κ^{3} $NCN-$ NCN^{CH2} $-iPr)($ CH_{2} %$ SiMe_{3} $)] turned out to be catalytically active for the hydrosilylation of ketones at room temperature with a catalyst loading of 1 mol%. X-ray structures of all complexes are presented. Graphical abstract © The Author(s) 2023 |
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| title_short |
Cr(II) and Cr(III) NCN pincer complexes: synthesis, structure, and catalytic reactivity |
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https://dx.doi.org/10.1007/s00706-023-03128-6 |
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Eder, Wolfgang Pecak, Jan Stöger, Berthold Pignitter, Marc Veiros, Luis F. Kirchner, Karl |
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Eder, Wolfgang Pecak, Jan Stöger, Berthold Pignitter, Marc Veiros, Luis F. Kirchner, Karl |
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| doi_str |
10.1007/s00706-023-03128-6 |
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2024-07-03T20:40:57.502Z |
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| score |
7.4008284 |