Syntheses, Reactivities, Characterization, and Crystal Structures of Dipalladium Complexes Containing the 1,3-pyrimidinyl Ligand: Structures of [Pd(PPh<sub>3</sub>)(Br)]<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>, [Pd(Br)]<sub>2</sub>(μ,η<sup>2</sup>-Hdppa)<sub>2</sub>, and [{Pd(PPh<sub>3</sub>)(CH<sub>3</sub>CN)}<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>][BF<sub>4</sub>]<sub>2</sub>
In a refluxing chloroform solution, the η<sup>1</sup>-pyrimidinyl {pyrimidinyl = C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>} palladium complex [Pd(PPh<sub>3</sub>)<sub>2</sub>(η<sup>1</sup>-C<sub>4</sub>H<...
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| Format: | Article |
| Language: | English |
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MDPI AG
2020-04-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/25/9/2035 |
| _version_ | 1797569538223505408 |
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| author | Hsiao-Fen Wang Kuang-Hway Yih Gene-Hsiang Lee |
| author_facet | Hsiao-Fen Wang Kuang-Hway Yih Gene-Hsiang Lee |
| author_sort | Hsiao-Fen Wang |
| collection | DOAJ |
| description | In a refluxing chloroform solution, the η<sup>1</sup>-pyrimidinyl {pyrimidinyl = C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>} palladium complex [Pd(PPh<sub>3</sub>)<sub>2</sub>(η<sup>1</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)(Br)], <b>1</b> exhibited intermolecular displacement of two triphenylphosphine ligands to form the doubly bridged η<sup>2</sup>-pyrimidinyl Dipalladium complex [Pd(PPh<sub>3</sub>)(Br)]<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>, <b>3</b>. The treatment of <b>1</b> with Hdppa {Hdppa = <i>N</i>,<i>N</i>-bisdiphenyl phosphinoamine} in refluxing dichloromethane yielded the doubly bridged Hdppa dipalladium complex [Pd(Br)]<sub>2</sub>(μ,η<sup>2</sup>-Hdppa)<sub>2</sub>, <b>4</b>. Complex <b>1</b> reacted with the bidentate ligand, NH<sub>4</sub>S<sub>2</sub>CNC<sub>4</sub>H<sub>8</sub> and, NaS<sub>2</sub>COEt, and the tridentate ligand, KTp {Tp = tris(pyrazoyl-1-yl)borate}, to form the η<sup>2</sup>-dithio η<sup>1</sup>-pyrimidinyl complex [Pd(PPh<sub>3</sub>)(η<sup>1</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)(η<sup>2</sup>-SS)], (<b>5</b>: SS = S<sub>2</sub>CNC<sub>4</sub>H<sub>8</sub>; <b>6</b>: SS = S<sub>2</sub>COEt) and η<sup>2</sup>-Tp η<sup>1</sup>-pyrimidinyl complex [Pd(PPh<sub>3</sub>)(η<sup>1</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)(η<sup>2</sup>-Tp)], <b>7</b>, respectively. Treatment of <b>1</b> with AgBF<sub>4</sub> in acetonitrile at room temperature resulted in the formation of the doubly bridged η<sup>2</sup>-pyrimidinyl dipalladium complex [{Pd(PPh<sub>3</sub>)(CH<sub>3</sub>CN)}<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>][BF<sub>4</sub>]<sub>2</sub>, <b>8</b>. All of the complexes were identified using spectroscopic methods, and complexes <b>3</b>, <b>4</b>, and <b>8</b> were determined using single-crystal X-ray diffraction analyses. |
| first_indexed | 2024-03-10T20:11:58Z |
| format | Article |
| id | doaj.art-fa2c41bdcb8041759e9283dd90a07912 |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-10T20:11:58Z |
| publishDate | 2020-04-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-fa2c41bdcb8041759e9283dd90a079122023-11-19T22:52:33ZengMDPI AGMolecules1420-30492020-04-01259203510.3390/molecules25092035Syntheses, Reactivities, Characterization, and Crystal Structures of Dipalladium Complexes Containing the 1,3-pyrimidinyl Ligand: Structures of [Pd(PPh<sub>3</sub>)(Br)]<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>, [Pd(Br)]<sub>2</sub>(μ,η<sup>2</sup>-Hdppa)<sub>2</sub>, and [{Pd(PPh<sub>3</sub>)(CH<sub>3</sub>CN)}<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>][BF<sub>4</sub>]<sub>2</sub>Hsiao-Fen Wang0Kuang-Hway Yih1Gene-Hsiang Lee2Department of Hair Styling and Design, Hungkuang University, No. 1018, Sec. 6, Taiwan Boulevard, Shalu Dist., Taichung 43306, TaiwanDepartment of Applied Cosmetology, Hungkuang University, No. 1018, Sec. 6, Taiwan Boulevard, Shalu Dist., Taichung 43306, TaiwanInstrumentation Center, College of Science, National Taiwan University, Taipei 10617, TaiwanIn a refluxing chloroform solution, the η<sup>1</sup>-pyrimidinyl {pyrimidinyl = C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>} palladium complex [Pd(PPh<sub>3</sub>)<sub>2</sub>(η<sup>1</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)(Br)], <b>1</b> exhibited intermolecular displacement of two triphenylphosphine ligands to form the doubly bridged η<sup>2</sup>-pyrimidinyl Dipalladium complex [Pd(PPh<sub>3</sub>)(Br)]<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>, <b>3</b>. The treatment of <b>1</b> with Hdppa {Hdppa = <i>N</i>,<i>N</i>-bisdiphenyl phosphinoamine} in refluxing dichloromethane yielded the doubly bridged Hdppa dipalladium complex [Pd(Br)]<sub>2</sub>(μ,η<sup>2</sup>-Hdppa)<sub>2</sub>, <b>4</b>. Complex <b>1</b> reacted with the bidentate ligand, NH<sub>4</sub>S<sub>2</sub>CNC<sub>4</sub>H<sub>8</sub> and, NaS<sub>2</sub>COEt, and the tridentate ligand, KTp {Tp = tris(pyrazoyl-1-yl)borate}, to form the η<sup>2</sup>-dithio η<sup>1</sup>-pyrimidinyl complex [Pd(PPh<sub>3</sub>)(η<sup>1</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)(η<sup>2</sup>-SS)], (<b>5</b>: SS = S<sub>2</sub>CNC<sub>4</sub>H<sub>8</sub>; <b>6</b>: SS = S<sub>2</sub>COEt) and η<sup>2</sup>-Tp η<sup>1</sup>-pyrimidinyl complex [Pd(PPh<sub>3</sub>)(η<sup>1</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)(η<sup>2</sup>-Tp)], <b>7</b>, respectively. Treatment of <b>1</b> with AgBF<sub>4</sub> in acetonitrile at room temperature resulted in the formation of the doubly bridged η<sup>2</sup>-pyrimidinyl dipalladium complex [{Pd(PPh<sub>3</sub>)(CH<sub>3</sub>CN)}<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>][BF<sub>4</sub>]<sub>2</sub>, <b>8</b>. All of the complexes were identified using spectroscopic methods, and complexes <b>3</b>, <b>4</b>, and <b>8</b> were determined using single-crystal X-ray diffraction analyses.https://www.mdpi.com/1420-3049/25/9/2035dipalladiumpyrimidinyltris(pyrazoyl-1-yl)boratepyrrolidinyldithiocarbamatedoubly bridgedcrystal structures |
| spellingShingle | Hsiao-Fen Wang Kuang-Hway Yih Gene-Hsiang Lee Syntheses, Reactivities, Characterization, and Crystal Structures of Dipalladium Complexes Containing the 1,3-pyrimidinyl Ligand: Structures of [Pd(PPh<sub>3</sub>)(Br)]<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>, [Pd(Br)]<sub>2</sub>(μ,η<sup>2</sup>-Hdppa)<sub>2</sub>, and [{Pd(PPh<sub>3</sub>)(CH<sub>3</sub>CN)}<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>][BF<sub>4</sub>]<sub>2</sub> Molecules dipalladium pyrimidinyl tris(pyrazoyl-1-yl)borate pyrrolidinyldithiocarbamate doubly bridged crystal structures |
| title | Syntheses, Reactivities, Characterization, and Crystal Structures of Dipalladium Complexes Containing the 1,3-pyrimidinyl Ligand: Structures of [Pd(PPh<sub>3</sub>)(Br)]<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>, [Pd(Br)]<sub>2</sub>(μ,η<sup>2</sup>-Hdppa)<sub>2</sub>, and [{Pd(PPh<sub>3</sub>)(CH<sub>3</sub>CN)}<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>][BF<sub>4</sub>]<sub>2</sub> |
| title_full | Syntheses, Reactivities, Characterization, and Crystal Structures of Dipalladium Complexes Containing the 1,3-pyrimidinyl Ligand: Structures of [Pd(PPh<sub>3</sub>)(Br)]<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>, [Pd(Br)]<sub>2</sub>(μ,η<sup>2</sup>-Hdppa)<sub>2</sub>, and [{Pd(PPh<sub>3</sub>)(CH<sub>3</sub>CN)}<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>][BF<sub>4</sub>]<sub>2</sub> |
| title_fullStr | Syntheses, Reactivities, Characterization, and Crystal Structures of Dipalladium Complexes Containing the 1,3-pyrimidinyl Ligand: Structures of [Pd(PPh<sub>3</sub>)(Br)]<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>, [Pd(Br)]<sub>2</sub>(μ,η<sup>2</sup>-Hdppa)<sub>2</sub>, and [{Pd(PPh<sub>3</sub>)(CH<sub>3</sub>CN)}<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>][BF<sub>4</sub>]<sub>2</sub> |
| title_full_unstemmed | Syntheses, Reactivities, Characterization, and Crystal Structures of Dipalladium Complexes Containing the 1,3-pyrimidinyl Ligand: Structures of [Pd(PPh<sub>3</sub>)(Br)]<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>, [Pd(Br)]<sub>2</sub>(μ,η<sup>2</sup>-Hdppa)<sub>2</sub>, and [{Pd(PPh<sub>3</sub>)(CH<sub>3</sub>CN)}<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>][BF<sub>4</sub>]<sub>2</sub> |
| title_short | Syntheses, Reactivities, Characterization, and Crystal Structures of Dipalladium Complexes Containing the 1,3-pyrimidinyl Ligand: Structures of [Pd(PPh<sub>3</sub>)(Br)]<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>, [Pd(Br)]<sub>2</sub>(μ,η<sup>2</sup>-Hdppa)<sub>2</sub>, and [{Pd(PPh<sub>3</sub>)(CH<sub>3</sub>CN)}<sub>2</sub>(μ,η<sup>2</sup>-C<sub>4</sub>H<sub>3</sub>N<sub>2</sub>)<sub>2</sub>][BF<sub>4</sub>]<sub>2</sub> |
| title_sort | syntheses reactivities characterization and crystal structures of dipalladium complexes containing the 1 3 pyrimidinyl ligand structures of pd pph sub 3 sub br sub 2 sub μ η sup 2 sup c sub 4 sub h sub 3 sub n sub 2 sub sub 2 sub pd br sub 2 sub μ η sup 2 sup hdppa sub 2 sub and pd pph sub 3 sub ch sub 3 sub cn sub 2 sub μ η sup 2 sup c sub 4 sub h sub 3 sub n sub 2 sub sub 2 sub bf sub 4 sub sub 2 sub |
| topic | dipalladium pyrimidinyl tris(pyrazoyl-1-yl)borate pyrrolidinyldithiocarbamate doubly bridged crystal structures |
| url | https://www.mdpi.com/1420-3049/25/9/2035 |
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