Synthesis and Structures of Ti<sup>III</sup> and Ti<sup>IV</sup> Complexes Supported by a Bulky Guanidinate Ligand
In this work, titanium complexes of the bidentate bulky guanidine ligand [{(Dip)N}<sub>2</sub>CNR<sub>2</sub>]H (where Dip = C<sub>6</sub>H<sub>3</sub>iPr<sub>2</sub>-2,6 and R = CH(CH<sub>3</sub>)<sub>2</sub>) (LH)...
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MDPI AG
2021-07-01
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author | Awal Noor |
author_facet | Awal Noor |
author_sort | Awal Noor |
collection | DOAJ |
description | In this work, titanium complexes of the bidentate bulky guanidine ligand [{(Dip)N}<sub>2</sub>CNR<sub>2</sub>]H (where Dip = C<sub>6</sub>H<sub>3</sub>iPr<sub>2</sub>-2,6 and R = CH(CH<sub>3</sub>)<sub>2</sub>) (LH) were prepared. Reaction of LH with one equivalent of [(CH<sub>3</sub>)<sub>2</sub>NTiCl<sub>3</sub>] underwent amine elimination to afford the monomeric complex [LTiCl<sub>3</sub>] (<b>1</b>) in high yield. Attempts to reduce <b>1</b> with potassium graphite (KC<sub>8</sub>) in tetrahydrofuran (THF) were unsuccessful. However, reacting <b>1</b> with 3.3 equivalents of KC<sub>8</sub> in hexane led to the first example of structurally characterized mono-guanidinate ligand stabilized dimeric Ti<sup>III</sup> complex [LTiCl(μ–Cl)]<sub>2</sub> (<b>2</b>). The synthesized complexes were characterized by NMR spectroscopy and the structures were further confirmed by X-ray crystallography. |
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language | English |
last_indexed | 2024-03-10T08:54:47Z |
publishDate | 2021-07-01 |
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spelling | doaj.art-b29f06189feb460087adf0301a1874be2023-11-22T07:16:21ZengMDPI AGCrystals2073-43522021-07-0111888610.3390/cryst11080886Synthesis and Structures of Ti<sup>III</sup> and Ti<sup>IV</sup> Complexes Supported by a Bulky Guanidinate LigandAwal Noor0Department of Basic Sciences, Preparatory Year Deanship, King Faisal University, Al-Hassa 31982, Saudi ArabiaIn this work, titanium complexes of the bidentate bulky guanidine ligand [{(Dip)N}<sub>2</sub>CNR<sub>2</sub>]H (where Dip = C<sub>6</sub>H<sub>3</sub>iPr<sub>2</sub>-2,6 and R = CH(CH<sub>3</sub>)<sub>2</sub>) (LH) were prepared. Reaction of LH with one equivalent of [(CH<sub>3</sub>)<sub>2</sub>NTiCl<sub>3</sub>] underwent amine elimination to afford the monomeric complex [LTiCl<sub>3</sub>] (<b>1</b>) in high yield. Attempts to reduce <b>1</b> with potassium graphite (KC<sub>8</sub>) in tetrahydrofuran (THF) were unsuccessful. However, reacting <b>1</b> with 3.3 equivalents of KC<sub>8</sub> in hexane led to the first example of structurally characterized mono-guanidinate ligand stabilized dimeric Ti<sup>III</sup> complex [LTiCl(μ–Cl)]<sub>2</sub> (<b>2</b>). The synthesized complexes were characterized by NMR spectroscopy and the structures were further confirmed by X-ray crystallography.https://www.mdpi.com/2073-4352/11/8/886guanidinateN-ligandssingle crystaltitaniumX-ray analysis |
spellingShingle | Awal Noor Synthesis and Structures of Ti<sup>III</sup> and Ti<sup>IV</sup> Complexes Supported by a Bulky Guanidinate Ligand Crystals guanidinate N-ligands single crystal titanium X-ray analysis |
title | Synthesis and Structures of Ti<sup>III</sup> and Ti<sup>IV</sup> Complexes Supported by a Bulky Guanidinate Ligand |
title_full | Synthesis and Structures of Ti<sup>III</sup> and Ti<sup>IV</sup> Complexes Supported by a Bulky Guanidinate Ligand |
title_fullStr | Synthesis and Structures of Ti<sup>III</sup> and Ti<sup>IV</sup> Complexes Supported by a Bulky Guanidinate Ligand |
title_full_unstemmed | Synthesis and Structures of Ti<sup>III</sup> and Ti<sup>IV</sup> Complexes Supported by a Bulky Guanidinate Ligand |
title_short | Synthesis and Structures of Ti<sup>III</sup> and Ti<sup>IV</sup> Complexes Supported by a Bulky Guanidinate Ligand |
title_sort | synthesis and structures of ti sup iii sup and ti sup iv sup complexes supported by a bulky guanidinate ligand |
topic | guanidinate N-ligands single crystal titanium X-ray analysis |
url | https://www.mdpi.com/2073-4352/11/8/886 |
work_keys_str_mv | AT awalnoor synthesisandstructuresoftisupiiisupandtisupivsupcomplexessupportedbyabulkyguanidinateligand |