Crystal structure of a Pd4 carbonyl triphenylphosphane cluster [Pd4(CO)5(PPh3)4]·2C4H8O, comparing solvates
Attempts to synthesize Au–Pd heterometallic compounds from homonuclear palladium or gold complexes, [Pd(PtBu2)2] and [Au(PPh3)Cl] in a tetrahydrofuran (THF) solution under a CO atmosphere resulted in a homonuclear Pd cluster, namely pentakis(μ-carbonyl-κ2C:C)tetrakis(triphenylphosphane-κP)tetrapalla...
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| Format: | Article |
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International Union of Crystallography
2016-02-01
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| Series: | Acta Crystallographica Section E: Crystallographic Communications |
| Subjects: | |
| Online Access: | http://scripts.iucr.org/cgi-bin/paper?S205698901502441X |
| _version_ | 1819291070897324032 |
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| author | Koen Robeyns Christopher Willocq Bernard Tinant Michel Devillers Sophie Hermans |
| author_facet | Koen Robeyns Christopher Willocq Bernard Tinant Michel Devillers Sophie Hermans |
| author_sort | Koen Robeyns |
| collection | DOAJ |
| description | Attempts to synthesize Au–Pd heterometallic compounds from homonuclear palladium or gold complexes, [Pd(PtBu2)2] and [Au(PPh3)Cl] in a tetrahydrofuran (THF) solution under a CO atmosphere resulted in a homonuclear Pd cluster, namely pentakis(μ-carbonyl-κ2C:C)tetrakis(triphenylphosphane-κP)tetrapalladium(5 Pd—Pd) tetrahydrofuran disolvate, [Pd4(CO)5(C18H15P)4]·2C4H8O. The complex molecule lies on a twofold rotation axis. The crystal structure is described in relation to the CH2Cl2 solvate previously determined by our group [Willocq et al. (2011). Inorg. Chim. Acta, 373, 233–242], and in particular to the desolvated structure [Feltham et al. (1985). Inorg. Chem. 24, 1503–1510]. It is assumed that the title compound transforms into the latter structure, upon gradual loss of solvent molecules. In the title compound, the symmetry-unique THF solvent molecule is linked to the complex molecule by a weak C—H...O hydrogen bond. Contributions of disordered solvent molecules to the diffraction intensities, most likely associated with methanol, were removed with the SQUEEZE [Spek (2015). Acta Cryst. C71, 9–18] algorithm. |
| first_indexed | 2024-12-24T03:32:48Z |
| format | Article |
| id | doaj.art-c4eade3530e54062858d602cc3ef812a |
| institution | Directory Open Access Journal |
| issn | 2056-9890 |
| language | English |
| last_indexed | 2024-12-24T03:32:48Z |
| publishDate | 2016-02-01 |
| publisher | International Union of Crystallography |
| record_format | Article |
| series | Acta Crystallographica Section E: Crystallographic Communications |
| spelling | doaj.art-c4eade3530e54062858d602cc3ef812a2022-12-21T17:17:09ZengInternational Union of CrystallographyActa Crystallographica Section E: Crystallographic Communications2056-98902016-02-0172212012310.1107/S205698901502441Xlh5801Crystal structure of a Pd4 carbonyl triphenylphosphane cluster [Pd4(CO)5(PPh3)4]·2C4H8O, comparing solvatesKoen Robeyns0Christopher Willocq1Bernard Tinant2Michel Devillers3Sophie Hermans4Institute of Condensed Matter and Nanosciences (IMCN), Université Catholique de Louvain, 1 Place Louis Pasteur, B 1348 Louvain-la-Neuve, BelgiumInstitute of Condensed Matter and Nanosciences (IMCN), Université Catholique de Louvain, 1 Place Louis Pasteur, B 1348 Louvain-la-Neuve, BelgiumInstitute of Condensed Matter and Nanosciences (IMCN), Université Catholique de Louvain, 1 Place Louis Pasteur, B 1348 Louvain-la-Neuve, BelgiumInstitute of Condensed Matter and Nanosciences (IMCN), Université Catholique de Louvain, 1 Place Louis Pasteur, B 1348 Louvain-la-Neuve, BelgiumInstitute of Condensed Matter and Nanosciences (IMCN), Université Catholique de Louvain, 1 Place Louis Pasteur, B 1348 Louvain-la-Neuve, BelgiumAttempts to synthesize Au–Pd heterometallic compounds from homonuclear palladium or gold complexes, [Pd(PtBu2)2] and [Au(PPh3)Cl] in a tetrahydrofuran (THF) solution under a CO atmosphere resulted in a homonuclear Pd cluster, namely pentakis(μ-carbonyl-κ2C:C)tetrakis(triphenylphosphane-κP)tetrapalladium(5 Pd—Pd) tetrahydrofuran disolvate, [Pd4(CO)5(C18H15P)4]·2C4H8O. The complex molecule lies on a twofold rotation axis. The crystal structure is described in relation to the CH2Cl2 solvate previously determined by our group [Willocq et al. (2011). Inorg. Chim. Acta, 373, 233–242], and in particular to the desolvated structure [Feltham et al. (1985). Inorg. Chem. 24, 1503–1510]. It is assumed that the title compound transforms into the latter structure, upon gradual loss of solvent molecules. In the title compound, the symmetry-unique THF solvent molecule is linked to the complex molecule by a weak C—H...O hydrogen bond. Contributions of disordered solvent molecules to the diffraction intensities, most likely associated with methanol, were removed with the SQUEEZE [Spek (2015). Acta Cryst. C71, 9–18] algorithm.http://scripts.iucr.org/cgi-bin/paper?S205698901502441Xstructure transformationhomonuclear clusterpalladiumgoldcrystal structure |
| spellingShingle | Koen Robeyns Christopher Willocq Bernard Tinant Michel Devillers Sophie Hermans Crystal structure of a Pd4 carbonyl triphenylphosphane cluster [Pd4(CO)5(PPh3)4]·2C4H8O, comparing solvates Acta Crystallographica Section E: Crystallographic Communications structure transformation homonuclear cluster palladium gold crystal structure |
| title | Crystal structure of a Pd4 carbonyl triphenylphosphane cluster [Pd4(CO)5(PPh3)4]·2C4H8O, comparing solvates |
| title_full | Crystal structure of a Pd4 carbonyl triphenylphosphane cluster [Pd4(CO)5(PPh3)4]·2C4H8O, comparing solvates |
| title_fullStr | Crystal structure of a Pd4 carbonyl triphenylphosphane cluster [Pd4(CO)5(PPh3)4]·2C4H8O, comparing solvates |
| title_full_unstemmed | Crystal structure of a Pd4 carbonyl triphenylphosphane cluster [Pd4(CO)5(PPh3)4]·2C4H8O, comparing solvates |
| title_short | Crystal structure of a Pd4 carbonyl triphenylphosphane cluster [Pd4(CO)5(PPh3)4]·2C4H8O, comparing solvates |
| title_sort | crystal structure of a pd4 carbonyl triphenylphosphane cluster pd4 co 5 pph3 4 ·2c4h8o comparing solvates |
| topic | structure transformation homonuclear cluster palladium gold crystal structure |
| url | http://scripts.iucr.org/cgi-bin/paper?S205698901502441X |
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