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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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Autores principales: Shapovalov, Sergey, Tikhonova, Olga, Skabitsky, Ivan
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2021
Materias:
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.
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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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AT tikhonovaolga crystalstructureofthenewpalladiumcomplexestetrakis13dimethylimidazolium2ylidenepalladiumiihexadecacarbonyltetrarheniumdiethyletherdisolvateandoctamcarbonyldicarbonyltetrakistriphenylphosphanepalladiumdirheniumunknownsolvate
AT skabitskyivan crystalstructureofthenewpalladiumcomplexestetrakis13dimethylimidazolium2ylidenepalladiumiihexadecacarbonyltetrarheniumdiethyletherdisolvateandoctamcarbonyldicarbonyltetrakistriphenylphosphanepalladiumdirheniumunknownsolvate