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Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10]
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Zeitschriftentitel: | Zeitschrift für Naturforschung B |
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Personen und Körperschaften: | , , , , |
In: | Zeitschrift für Naturforschung B, 39, 1984, 7, S. 843-849 |
Format: | E-Article |
Sprache: | Englisch |
veröffentlicht: |
Walter de Gruyter GmbH
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Schlagwörter: |
author_facet |
Krebs, B. Henkel, G. Dartmann, M. Preetz, W. Bruns, M. Krebs, B. Henkel, G. Dartmann, M. Preetz, W. Bruns, M. |
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author |
Krebs, B. Henkel, G. Dartmann, M. Preetz, W. Bruns, M. |
spellingShingle |
Krebs, B. Henkel, G. Dartmann, M. Preetz, W. Bruns, M. Zeitschrift für Naturforschung B Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] General Chemistry |
author_sort |
krebs, b. |
spelling |
Krebs, B. Henkel, G. Dartmann, M. Preetz, W. Bruns, M. 1865-7117 0932-0776 Walter de Gruyter GmbH General Chemistry http://dx.doi.org/10.1515/znb-1984-0701 <jats:p>On heating of [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N][OsCl<jats:sub>6</jats:sub>] for a short time at 240 °C , Cl<jats:sub>2</jats:sub> is lost and [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N]<jats:sub>2</jats:sub>[Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>] is formed quantitatively. Both complexes are connected by a temperature dependent redox equilibrium so that by treatment at 120 °C with Cl<jats:sub>2</jats:sub> gas the hexachloroosmate(V) is recovered from the decachlorodiosmate(IV). The crystal structures of salts of both an ions were determined from single crystal X -ray diffraction analyses. [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N][OsCl<jats:sub>6</jats:sub>] is monoclinic, space group P2<jats:sub> 1</jats:sub> with a = 7 .020 (1), b = 10 .163 (2), c = 11.609 (2) Å , β = 103.91(1)° (at - 133 °C ). The strongly pseudocentrosymmetric structure shows a reversible phase transition at ca. 85 °C. The Os -Cl bond length (mean value 2.303 Å) in the regular [OsCl<jats:sub>6</jats:sub>]-octahedra is significantly smaller than in [OsCl<jats:sub>6</jats:sub>]<jats:sup>2−</jats:sup> , in accordance with vibrational spectra. [(n -C<jats:sub>4</jats:sub>H<jats:sub>9</jats:sub>)<jats:sub>4</jats:sub>N]<jats:sub>2</jats:sub> [Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>] crystallizes in the orthorhombic space group Pbca with a = 15 .496 (2), b = 15 .965 (3), c = 19 .431(3) Å and contains centrosymmetric [Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>]<jats:sup>2−</jats:sup> ions with approximate D<jats:sub>2h</jats:sub> symmetry. Within the edge-sharing [OsCl<jats:sub>6</jats:sub>] octahedra the mean terminal and bridging Os -Cl bond lengths are 2.307 and 2.411 Å , respectively.</jats:p> Reaktionen und Strukturen von [(C<sub>2</sub>H<sub>5</sub>)<sub>4</sub>N][OsCl<sub>6</sub>] und [(n-C<sub>4</sub>H<sub>9</sub>)<sub>4</sub>N]<sub>2</sub>[Os<sub>2</sub>Cl<sub>10</sub>] / Reactions and Structures of [(C<sub>2</sub>H<sub>5</sub>)<sub>4</sub>N][OsCl<sub>6</sub>] and [(n-C<sub>4</sub>H<sub>9</sub>)<sub>4</sub>N]<sub>2</sub>[Os<sub>2</sub>Cl<sub>10</sub>] Zeitschrift für Naturforschung B |
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10.1515/znb-1984-0701 |
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DE-L229 DE-D275 DE-Bn3 DE-Brt1 DE-Zwi2 DE-D161 DE-Gla1 DE-Zi4 DE-15 DE-Pl11 DE-Rs1 DE-105 DE-14 DE-Ch1 |
imprint |
Walter de Gruyter GmbH, 1984 |
imprint_str_mv |
Walter de Gruyter GmbH, 1984 |
issn |
1865-7117 0932-0776 |
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1865-7117 0932-0776 |
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Walter de Gruyter GmbH (CrossRef) |
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1984 |
publisher |
Walter de Gruyter GmbH |
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Zeitschrift für Naturforschung B |
source_id |
49 |
title |
Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_unstemmed |
Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_full |
Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_fullStr |
Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_full_unstemmed |
Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_short |
Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_sort |
reaktionen und strukturen von [(c<sub>2</sub>h<sub>5</sub>)<sub>4</sub>n][oscl<sub>6</sub>] und [(n-c<sub>4</sub>h<sub>9</sub>)<sub>4</sub>n]<sub>2</sub>[os<sub>2</sub>cl<sub>10</sub>] / reactions and structures of [(c<sub>2</sub>h<sub>5</sub>)<sub>4</sub>n][oscl<sub>6</sub>] and [(n-c<sub>4</sub>h<sub>9</sub>)<sub>4</sub>n]<sub>2</sub>[os<sub>2</sub>cl<sub>10</sub>] |
topic |
General Chemistry |
url |
http://dx.doi.org/10.1515/znb-1984-0701 |
publishDate |
1984 |
physical |
843-849 |
description |
<jats:p>On heating of [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N][OsCl<jats:sub>6</jats:sub>] for a short time at 240 °C , Cl<jats:sub>2</jats:sub> is lost and [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N]<jats:sub>2</jats:sub>[Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>] is formed quantitatively. Both complexes are connected by a temperature dependent redox equilibrium so that by treatment at 120 °C with Cl<jats:sub>2</jats:sub> gas the hexachloroosmate(V) is recovered from the decachlorodiosmate(IV). The crystal structures of salts of both an ions were determined from single crystal X -ray diffraction analyses. [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N][OsCl<jats:sub>6</jats:sub>] is monoclinic, space group P2<jats:sub> 1</jats:sub> with a = 7 .020 (1), b = 10 .163 (2), c = 11.609 (2) Å , β = 103.91(1)° (at - 133 °C ). The strongly pseudocentrosymmetric structure shows a reversible phase transition at ca. 85 °C. The Os -Cl bond length (mean value 2.303 Å) in the regular [OsCl<jats:sub>6</jats:sub>]-octahedra is significantly smaller than in [OsCl<jats:sub>6</jats:sub>]<jats:sup>2−</jats:sup> , in accordance with vibrational spectra. [(n -C<jats:sub>4</jats:sub>H<jats:sub>9</jats:sub>)<jats:sub>4</jats:sub>N]<jats:sub>2</jats:sub> [Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>] crystallizes in the orthorhombic space group Pbca with a = 15 .496 (2), b = 15 .965 (3), c = 19 .431(3) Å and contains centrosymmetric [Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>]<jats:sup>2−</jats:sup> ions with approximate D<jats:sub>2h</jats:sub> symmetry. Within the edge-sharing [OsCl<jats:sub>6</jats:sub>] octahedra the mean terminal and bridging Os -Cl bond lengths are 2.307 and 2.411 Å , respectively.</jats:p> |
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author | Krebs, B., Henkel, G., Dartmann, M., Preetz, W., Bruns, M. |
author_facet | Krebs, B., Henkel, G., Dartmann, M., Preetz, W., Bruns, M., Krebs, B., Henkel, G., Dartmann, M., Preetz, W., Bruns, M. |
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description | <jats:p>On heating of [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N][OsCl<jats:sub>6</jats:sub>] for a short time at 240 °C , Cl<jats:sub>2</jats:sub> is lost and [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N]<jats:sub>2</jats:sub>[Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>] is formed quantitatively. Both complexes are connected by a temperature dependent redox equilibrium so that by treatment at 120 °C with Cl<jats:sub>2</jats:sub> gas the hexachloroosmate(V) is recovered from the decachlorodiosmate(IV). The crystal structures of salts of both an ions were determined from single crystal X -ray diffraction analyses. [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N][OsCl<jats:sub>6</jats:sub>] is monoclinic, space group P2<jats:sub> 1</jats:sub> with a = 7 .020 (1), b = 10 .163 (2), c = 11.609 (2) Å , β = 103.91(1)° (at - 133 °C ). The strongly pseudocentrosymmetric structure shows a reversible phase transition at ca. 85 °C. The Os -Cl bond length (mean value 2.303 Å) in the regular [OsCl<jats:sub>6</jats:sub>]-octahedra is significantly smaller than in [OsCl<jats:sub>6</jats:sub>]<jats:sup>2−</jats:sup> , in accordance with vibrational spectra. [(n -C<jats:sub>4</jats:sub>H<jats:sub>9</jats:sub>)<jats:sub>4</jats:sub>N]<jats:sub>2</jats:sub> [Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>] crystallizes in the orthorhombic space group Pbca with a = 15 .496 (2), b = 15 .965 (3), c = 19 .431(3) Å and contains centrosymmetric [Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>]<jats:sup>2−</jats:sup> ions with approximate D<jats:sub>2h</jats:sub> symmetry. Within the edge-sharing [OsCl<jats:sub>6</jats:sub>] octahedra the mean terminal and bridging Os -Cl bond lengths are 2.307 and 2.411 Å , respectively.</jats:p> |
doi_str_mv | 10.1515/znb-1984-0701 |
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id | ai-49-aHR0cDovL2R4LmRvaS5vcmcvMTAuMTUxNS96bmItMTk4NC0wNzAx |
imprint | Walter de Gruyter GmbH, 1984 |
imprint_str_mv | Walter de Gruyter GmbH, 1984 |
institution | DE-L229, DE-D275, DE-Bn3, DE-Brt1, DE-Zwi2, DE-D161, DE-Gla1, DE-Zi4, DE-15, DE-Pl11, DE-Rs1, DE-105, DE-14, DE-Ch1 |
issn | 1865-7117, 0932-0776 |
issn_str_mv | 1865-7117, 0932-0776 |
language | English |
last_indexed | 2024-03-01T15:02:58.015Z |
match_str | krebs1984reaktionenundstrukturenvonc2h54noscl6undnc4h94n2os2cl10reactionsandstructuresofc2h54noscl6andnc4h94n2os2cl10 |
mega_collection | Walter de Gruyter GmbH (CrossRef) |
physical | 843-849 |
publishDate | 1984 |
publishDateSort | 1984 |
publisher | Walter de Gruyter GmbH |
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series | Zeitschrift für Naturforschung B |
source_id | 49 |
spelling | Krebs, B. Henkel, G. Dartmann, M. Preetz, W. Bruns, M. 1865-7117 0932-0776 Walter de Gruyter GmbH General Chemistry http://dx.doi.org/10.1515/znb-1984-0701 <jats:p>On heating of [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N][OsCl<jats:sub>6</jats:sub>] for a short time at 240 °C , Cl<jats:sub>2</jats:sub> is lost and [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N]<jats:sub>2</jats:sub>[Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>] is formed quantitatively. Both complexes are connected by a temperature dependent redox equilibrium so that by treatment at 120 °C with Cl<jats:sub>2</jats:sub> gas the hexachloroosmate(V) is recovered from the decachlorodiosmate(IV). The crystal structures of salts of both an ions were determined from single crystal X -ray diffraction analyses. [(C<jats:sub>2</jats:sub>H<jats:sub>5</jats:sub>)<jats:sub>4</jats:sub>N][OsCl<jats:sub>6</jats:sub>] is monoclinic, space group P2<jats:sub> 1</jats:sub> with a = 7 .020 (1), b = 10 .163 (2), c = 11.609 (2) Å , β = 103.91(1)° (at - 133 °C ). The strongly pseudocentrosymmetric structure shows a reversible phase transition at ca. 85 °C. The Os -Cl bond length (mean value 2.303 Å) in the regular [OsCl<jats:sub>6</jats:sub>]-octahedra is significantly smaller than in [OsCl<jats:sub>6</jats:sub>]<jats:sup>2−</jats:sup> , in accordance with vibrational spectra. [(n -C<jats:sub>4</jats:sub>H<jats:sub>9</jats:sub>)<jats:sub>4</jats:sub>N]<jats:sub>2</jats:sub> [Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>] crystallizes in the orthorhombic space group Pbca with a = 15 .496 (2), b = 15 .965 (3), c = 19 .431(3) Å and contains centrosymmetric [Os<jats:sub>2</jats:sub>Cl<jats:sub>10</jats:sub>]<jats:sup>2−</jats:sup> ions with approximate D<jats:sub>2h</jats:sub> symmetry. Within the edge-sharing [OsCl<jats:sub>6</jats:sub>] octahedra the mean terminal and bridging Os -Cl bond lengths are 2.307 and 2.411 Å , respectively.</jats:p> Reaktionen und Strukturen von [(C<sub>2</sub>H<sub>5</sub>)<sub>4</sub>N][OsCl<sub>6</sub>] und [(n-C<sub>4</sub>H<sub>9</sub>)<sub>4</sub>N]<sub>2</sub>[Os<sub>2</sub>Cl<sub>10</sub>] / Reactions and Structures of [(C<sub>2</sub>H<sub>5</sub>)<sub>4</sub>N][OsCl<sub>6</sub>] and [(n-C<sub>4</sub>H<sub>9</sub>)<sub>4</sub>N]<sub>2</sub>[Os<sub>2</sub>Cl<sub>10</sub>] Zeitschrift für Naturforschung B |
spellingShingle | Krebs, B., Henkel, G., Dartmann, M., Preetz, W., Bruns, M., Zeitschrift für Naturforschung B, Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10], General Chemistry |
title | Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_full | Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_fullStr | Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_full_unstemmed | Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_short | Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
title_sort | reaktionen und strukturen von [(c<sub>2</sub>h<sub>5</sub>)<sub>4</sub>n][oscl<sub>6</sub>] und [(n-c<sub>4</sub>h<sub>9</sub>)<sub>4</sub>n]<sub>2</sub>[os<sub>2</sub>cl<sub>10</sub>] / reactions and structures of [(c<sub>2</sub>h<sub>5</sub>)<sub>4</sub>n][oscl<sub>6</sub>] and [(n-c<sub>4</sub>h<sub>9</sub>)<sub>4</sub>n]<sub>2</sub>[os<sub>2</sub>cl<sub>10</sub>] |
title_unstemmed | Reaktionen und Strukturen von [(C2H5)4N][OsCl6] und [(n-C4H9)4N]2[Os2Cl10] / Reactions and Structures of [(C2H5)4N][OsCl6] and [(n-C4H9)4N]2[Os2Cl10] |
topic | General Chemistry |
url | http://dx.doi.org/10.1515/znb-1984-0701 |