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Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate)
The investigation of the coordination chemistry of heterometallic transition-metal complexes of palladium (Pd) and rhenium (Re) led to the isolation and crystallographic characterization of tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether d...
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Formato: | Online Artículo Texto |
Lenguaje: | English |
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International Union of Crystallography
2021
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Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8491523/ https://www.ncbi.nlm.nih.gov/pubmed/34667629 http://dx.doi.org/10.1107/S2056989021009270 |
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author | Shapovalov, Sergey Tikhonova, Olga Skabitsky, Ivan |
author_facet | Shapovalov, Sergey Tikhonova, Olga Skabitsky, Ivan |
author_sort | Shapovalov, Sergey |
collection | PubMed |
description | The investigation of the coordination chemistry of heterometallic transition-metal complexes of palladium (Pd) and rhenium (Re) led to the isolation and crystallographic characterization of tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate, [Pd(C(5)H(8)N(2))(4)][Re(4)(CO)(16)]·2C(4)H(10)O or [Pd(IMe)(4)][Re(4)(CO)(16)]·2C(4)H(10)O, (1), and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium, [Pd(4)Re(2)(C(18)H(15)P)(4)(CO)(10)] or Pd(4)Re(2)(PPh(3))(4)(μ-CO)(8)(CO)(2), (2), from the reaction of Pd(PPh(3))(4) with 1,3-dimethylimidazolium-2-carboxylate and Re(2)(CO)(10) in a toluene–acetonitrile mixture. In complex 1 the Re—Re bond lengths [2.9767 (3)–3.0133 (2) Å] are close to double the covalent Re radii (1.51 Å). The palladium–rhenium carbonyl cluster 2 has not been structurally characterized previously; the Pd—Re bond lengths [2.7582 (2)–2.7796 (2) Å] are about 0.1 Å shorter than the sum of the covalent Pd and Re radii (1.39 + 1.51 = 2.90 Å). One carbene ligand and a diethyl ether molecule are disordered over two positions with occupancy ratios of 0.5:0.5 and 0.625 (15):0.375 (15) in 1. An unidentified solvent is present in compound 2. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s). The SQUEEZE routine [Spek (2015 ▸). Acta Cryst. C71, 9–18] in PLATON was used to remove the contribution of the electron density in the solvent region from the intensity data and the solvent-free model was employed for the final refinement. The cavity with a volume of ca 311 Å(3) contains approximately 98 electrons. |
format | Online Article Text |
id | pubmed-8491523 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2021 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-84915232021-10-18 Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate) Shapovalov, Sergey Tikhonova, Olga Skabitsky, Ivan Acta Crystallogr E Crystallogr Commun Research Communications The investigation of the coordination chemistry of heterometallic transition-metal complexes of palladium (Pd) and rhenium (Re) led to the isolation and crystallographic characterization of tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate, [Pd(C(5)H(8)N(2))(4)][Re(4)(CO)(16)]·2C(4)H(10)O or [Pd(IMe)(4)][Re(4)(CO)(16)]·2C(4)H(10)O, (1), and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium, [Pd(4)Re(2)(C(18)H(15)P)(4)(CO)(10)] or Pd(4)Re(2)(PPh(3))(4)(μ-CO)(8)(CO)(2), (2), from the reaction of Pd(PPh(3))(4) with 1,3-dimethylimidazolium-2-carboxylate and Re(2)(CO)(10) in a toluene–acetonitrile mixture. In complex 1 the Re—Re bond lengths [2.9767 (3)–3.0133 (2) Å] are close to double the covalent Re radii (1.51 Å). The palladium–rhenium carbonyl cluster 2 has not been structurally characterized previously; the Pd—Re bond lengths [2.7582 (2)–2.7796 (2) Å] are about 0.1 Å shorter than the sum of the covalent Pd and Re radii (1.39 + 1.51 = 2.90 Å). One carbene ligand and a diethyl ether molecule are disordered over two positions with occupancy ratios of 0.5:0.5 and 0.625 (15):0.375 (15) in 1. An unidentified solvent is present in compound 2. The given chemical formula and other crystal data do not take into account the unknown solvent molecule(s). The SQUEEZE routine [Spek (2015 ▸). Acta Cryst. C71, 9–18] in PLATON was used to remove the contribution of the electron density in the solvent region from the intensity data and the solvent-free model was employed for the final refinement. The cavity with a volume of ca 311 Å(3) contains approximately 98 electrons. International Union of Crystallography 2021-09-14 /pmc/articles/PMC8491523/ /pubmed/34667629 http://dx.doi.org/10.1107/S2056989021009270 Text en © Shapovalov et al. 2021 https://creativecommons.org/licenses/by/4.0/This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited. |
spellingShingle | Research Communications Shapovalov, Sergey Tikhonova, Olga Skabitsky, Ivan Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate) |
title | Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate) |
title_full | Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate) |
title_fullStr | Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate) |
title_full_unstemmed | Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate) |
title_short | Crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(II) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate) |
title_sort | crystal structure of the new palladium complexes tetrakis(1,3-dimethylimidazolium-2-ylidene)palladium(ii) hexadecacarbonyltetrarhenium diethyl ether disolvate and octa-μ-carbonyl-dicarbonyltetrakis(triphenylphosphane)palladiumdirhenium (unknown solvate) |
topic | Research Communications |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8491523/ https://www.ncbi.nlm.nih.gov/pubmed/34667629 http://dx.doi.org/10.1107/S2056989021009270 |
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