Structural and Oxidation State Alternatives in Platinum and Palladium Complexes of a Redox‐Active Amidinato Ligand

Reaction of [Pt(DMSO)2Cl2] or [Pd(MeCN)2Cl2] with the electron‐rich LH=N,N’‐bis(4‐dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2] (1) but dinuclear [Pd2L4] (2), a paddle‐wheel complex. The neutral compounds were characterized through experiments (crystal structures, electrochemistry, U...

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Veröffentlicht in:Chemistry : a European journal Jg. 27; H. 10; S. 3374 - 3381
Hauptverfasser: Ehret, Fabian, Filippou, Vasileios, Blickle, Svenja, Bubrin, Martina, Záliš, Stanislav, Kaim, Wolfgang
Format: Journal Article
Sprache:Englisch
Veröffentlicht: WEINHEIM Wiley 15.02.2021
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ISSN:0947-6539, 1521-3765, 1521-3765
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Abstract Reaction of [Pt(DMSO)2Cl2] or [Pd(MeCN)2Cl2] with the electron‐rich LH=N,N’‐bis(4‐dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2] (1) but dinuclear [Pd2L4] (2), a paddle‐wheel complex. The neutral compounds were characterized through experiments (crystal structures, electrochemistry, UV‐vis‐NIR spectroscopy, magnetic resonance) and TD‐DFT calculations as metal(II) species with noninnocent ligands L−. The reversibly accessible cations [PtL2]+ and [Pd2L4]+ were also studied, the latter as [Pd2L4][B{3,5‐(CF3)2C6H3}4] single crystals. Experimental and computational investigations were directed at the elucidation of the electronic structures, establishing the correct oxidation states within the alternatives [PtII(L−)2] or [Pt.(L )2], [PtII(L0.5−)2]+ or [PtIII(L−)2]+, [(PdII)2(μ‐L−)4] or [(Pd1.5)2(μ‐L0.75−)4], and [(Pd2.5)2(μ‐L−)4]+ or [(PdII)2(μ‐L0.75−)4]+. In each case, the first alternative was shown to be most appropriate. Remarkable results include the preference of platinum for mononuclear planar [PtL2] with an N‐Pt‐N bite angle of 62.8(2)° in contrast to [Pd2L4], and the dimetal (Pd24+→Pd25+) instead of ligand (L−→L ) oxidation of the dinuclear palladium compound. Qualitatively different structures and electron transfer behavior have been established for platinum and palladium complexes [PtL2]0/+ and [Pd2L4]0/+ with a redox‐active amidinato ligand L−/L..
AbstractList Reaction of [Pt(DMSO)(2)Cl-2] or [Pd(MeCN)(2)Cl-2] with the electron-rich LH = N,N'-bis(4-dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2] (1) but dinuclear [Pd2L4] (2), a paddle-wheel complex. The neutral compounds were characterized through experiments (crystal structures, electrochemistry, UV-vis-NIR spectroscopy, magnetic resonance) and TD-DFT calculations as metal(II) species with non-innocent ligands L-. The reversibly accessible cations [PtL2](+) and [Pd2L4](+) were also studied, the latter as [Pd2L4][B{3,5-(CF3)(2)C6H3}(4)] single crystals. Experimental and computational investigations were directed at the elucidation of the electronic structures, establishing the correct oxidation states within the alternatives [Pt-II(L-)(2)] or [Pt-center dot(L)(2)], [Pt-II(L0.5-)(2)](+) or [Pt-III(L-)(2)](+), [(Pd-II)(2)(mu-L-)(4)] or [(Pd-1.5)(2)(m-L0.75-)(4)], and [(Pd-2.5)(2)(mu-L-)(4)](+) or [(Pd-II)(2)(mu-L0.75-)(4)](+). In each case, the first alternative was shown to be most appropriate. Remarkable results include the preference of platinum for mononuclear planar [PtL2] with an N-Pt-N bite angle of 62.8(2)degrees in contrast to [Pd2L4], and the dimetal (Pd-2(4+) -> Pd-2(5+)) instead of ligand (L- -> L) oxidation of the dinuclear palladium compound.
Reaction of [Pt(DMSO) 2 Cl 2 ] or [Pd(MeCN) 2 Cl 2 ] with the electron‐rich LH=N,N’‐bis(4‐dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL 2 ] ( 1 ) but dinuclear [Pd 2 L 4 ] ( 2 ), a paddle‐wheel complex. The neutral compounds were characterized through experiments (crystal structures, electrochemistry, UV‐vis‐NIR spectroscopy, magnetic resonance) and TD‐DFT calculations as metal(II) species with noninnocent ligands L − . The reversibly accessible cations [PtL 2 ] + and [Pd 2 L 4 ] + were also studied, the latter as [Pd 2 L 4 ][B{3,5‐(CF 3 ) 2 C 6 H 3 } 4 ] single crystals. Experimental and computational investigations were directed at the elucidation of the electronic structures, establishing the correct oxidation states within the alternatives [Pt II (L − ) 2 ] or [Pt . (L ) 2 ], [Pt II (L 0.5− ) 2 ] + or [Pt III (L − ) 2 ] + , [(Pd II ) 2 (μ‐L − ) 4 ] or [(Pd 1.5 ) 2 (μ‐L 0.75− ) 4 ], and [(Pd 2.5 ) 2 (μ‐L − ) 4 ] + or [(Pd II ) 2 (μ‐L 0.75− ) 4 ] + . In each case, the first alternative was shown to be most appropriate. Remarkable results include the preference of platinum for mononuclear planar [PtL 2 ] with an N ‐Pt‐N bite angle of 62.8(2)° in contrast to [Pd 2 L 4 ], and the dimetal (Pd 2 4+ →Pd 2 5+ ) instead of ligand (L − →L ) oxidation of the dinuclear palladium compound.
Reaction of [Pt(DMSO)2 Cl2 ] or [Pd(MeCN)2 Cl2 ] with the electron-rich LH=N,N'-bis(4-dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2 ] (1) but dinuclear [Pd2 L4 ] (2), a paddle-wheel complex. The neutral compounds were characterized through experiments (crystal structures, electrochemistry, UV-vis-NIR spectroscopy, magnetic resonance) and TD-DFT calculations as metal(II) species with noninnocent ligands L- . The reversibly accessible cations [PtL2 ]+ and [Pd2 L4 ]+ were also studied, the latter as [Pd2 L4 ][B{3,5-(CF3 )2 C6 H3 }4 ] single crystals. Experimental and computational investigations were directed at the elucidation of the electronic structures, establishing the correct oxidation states within the alternatives [PtII (L- )2 ] or [Pt. (L )2 ], [PtII (L0.5- )2 ]+ or [PtIII (L- )2 ]+ , [(PdII )2 (μ-L- )4 ] or [(Pd1.5 )2 (μ-L0.75- )4 ], and [(Pd2.5 )2 (μ-L- )4 ]+ or [(PdII )2 (μ-L0.75- )4 ]+ . In each case, the first alternative was shown to be most appropriate. Remarkable results include the preference of platinum for mononuclear planar [PtL2 ] with an N-Pt-N bite angle of 62.8(2)° in contrast to [Pd2 L4 ], and the dimetal (Pd2 4+ →Pd2 5+ ) instead of ligand (L- →L ) oxidation of the dinuclear palladium compound.Reaction of [Pt(DMSO)2 Cl2 ] or [Pd(MeCN)2 Cl2 ] with the electron-rich LH=N,N'-bis(4-dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2 ] (1) but dinuclear [Pd2 L4 ] (2), a paddle-wheel complex. The neutral compounds were characterized through experiments (crystal structures, electrochemistry, UV-vis-NIR spectroscopy, magnetic resonance) and TD-DFT calculations as metal(II) species with noninnocent ligands L- . The reversibly accessible cations [PtL2 ]+ and [Pd2 L4 ]+ were also studied, the latter as [Pd2 L4 ][B{3,5-(CF3 )2 C6 H3 }4 ] single crystals. Experimental and computational investigations were directed at the elucidation of the electronic structures, establishing the correct oxidation states within the alternatives [PtII (L- )2 ] or [Pt. (L )2 ], [PtII (L0.5- )2 ]+ or [PtIII (L- )2 ]+ , [(PdII )2 (μ-L- )4 ] or [(Pd1.5 )2 (μ-L0.75- )4 ], and [(Pd2.5 )2 (μ-L- )4 ]+ or [(PdII )2 (μ-L0.75- )4 ]+ . In each case, the first alternative was shown to be most appropriate. Remarkable results include the preference of platinum for mononuclear planar [PtL2 ] with an N-Pt-N bite angle of 62.8(2)° in contrast to [Pd2 L4 ], and the dimetal (Pd2 4+ →Pd2 5+ ) instead of ligand (L- →L ) oxidation of the dinuclear palladium compound.
Reaction of [Pt(DMSO) Cl ] or [Pd(MeCN) Cl ] with the electron-rich LH=N,N'-bis(4-dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL ] (1) but dinuclear [Pd L ] (2), a paddle-wheel complex. The neutral compounds were characterized through experiments (crystal structures, electrochemistry, UV-vis-NIR spectroscopy, magnetic resonance) and TD-DFT calculations as metal(II) species with noninnocent ligands L . The reversibly accessible cations [PtL ] and [Pd L ] were also studied, the latter as [Pd L ][B{3,5-(CF ) C H } ] single crystals. Experimental and computational investigations were directed at the elucidation of the electronic structures, establishing the correct oxidation states within the alternatives [Pt (L ) ] or [Pt (L ) ], [Pt (L ) ] or [Pt (L ) ] , [(Pd ) (μ-L ) ] or [(Pd ) (μ-L ) ], and [(Pd ) (μ-L ) ] or [(Pd ) (μ-L ) ] . In each case, the first alternative was shown to be most appropriate. Remarkable results include the preference of platinum for mononuclear planar [PtL ] with an N-Pt-N bite angle of 62.8(2)° in contrast to [Pd L ], and the dimetal (Pd →Pd ) instead of ligand (L →L ) oxidation of the dinuclear palladium compound.
Reaction of [Pt(DMSO)2Cl2] or [Pd(MeCN)2Cl2] with the electron‐rich LH=N,N’‐bis(4‐dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2] (1) but dinuclear [Pd2L4] (2), a paddle‐wheel complex. The neutral compounds were characterized through experiments (crystal structures, electrochemistry, UV‐vis‐NIR spectroscopy, magnetic resonance) and TD‐DFT calculations as metal(II) species with noninnocent ligands L−. The reversibly accessible cations [PtL2]+ and [Pd2L4]+ were also studied, the latter as [Pd2L4][B{3,5‐(CF3)2C6H3}4] single crystals. Experimental and computational investigations were directed at the elucidation of the electronic structures, establishing the correct oxidation states within the alternatives [PtII(L−)2] or [Pt.(L )2], [PtII(L0.5−)2]+ or [PtIII(L−)2]+, [(PdII)2(μ‐L−)4] or [(Pd1.5)2(μ‐L0.75−)4], and [(Pd2.5)2(μ‐L−)4]+ or [(PdII)2(μ‐L0.75−)4]+. In each case, the first alternative was shown to be most appropriate. Remarkable results include the preference of platinum for mononuclear planar [PtL2] with an N‐Pt‐N bite angle of 62.8(2)° in contrast to [Pd2L4], and the dimetal (Pd2 4+→Pd2 5+) instead of ligand (L−→L ) oxidation of the dinuclear palladium compound. Qualitatively different structures and electron transfer behavior have been established for platinum and palladium complexes [PtL2]0/+ and [Pd2L4]0/+ with a redox‐active amidinato ligand L− /L..
Reaction of [Pt(DMSO)2Cl2] or [Pd(MeCN)2Cl2] with the electron‐rich LH=N,N’‐bis(4‐dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2] (1) but dinuclear [Pd2L4] (2), a paddle‐wheel complex. The neutral compounds were characterized through experiments (crystal structures, electrochemistry, UV‐vis‐NIR spectroscopy, magnetic resonance) and TD‐DFT calculations as metal(II) species with noninnocent ligands L−. The reversibly accessible cations [PtL2]+ and [Pd2L4]+ were also studied, the latter as [Pd2L4][B{3,5‐(CF3)2C6H3}4] single crystals. Experimental and computational investigations were directed at the elucidation of the electronic structures, establishing the correct oxidation states within the alternatives [PtII(L−)2] or [Pt.(L )2], [PtII(L0.5−)2]+ or [PtIII(L−)2]+, [(PdII)2(μ‐L−)4] or [(Pd1.5)2(μ‐L0.75−)4], and [(Pd2.5)2(μ‐L−)4]+ or [(PdII)2(μ‐L0.75−)4]+. In each case, the first alternative was shown to be most appropriate. Remarkable results include the preference of platinum for mononuclear planar [PtL2] with an N‐Pt‐N bite angle of 62.8(2)° in contrast to [Pd2L4], and the dimetal (Pd24+→Pd25+) instead of ligand (L−→L ) oxidation of the dinuclear palladium compound.
Reaction of [Pt(DMSO)2Cl2] or [Pd(MeCN)2Cl2] with the electron‐rich LH=N,N’‐bis(4‐dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2] (1) but dinuclear [Pd2L4] (2), a paddle‐wheel complex. The neutral compounds were characterized through experiments (crystal structures, electrochemistry, UV‐vis‐NIR spectroscopy, magnetic resonance) and TD‐DFT calculations as metal(II) species with noninnocent ligands L−. The reversibly accessible cations [PtL2]+ and [Pd2L4]+ were also studied, the latter as [Pd2L4][B{3,5‐(CF3)2C6H3}4] single crystals. Experimental and computational investigations were directed at the elucidation of the electronic structures, establishing the correct oxidation states within the alternatives [PtII(L−)2] or [Pt.(L )2], [PtII(L0.5−)2]+ or [PtIII(L−)2]+, [(PdII)2(μ‐L−)4] or [(Pd1.5)2(μ‐L0.75−)4], and [(Pd2.5)2(μ‐L−)4]+ or [(PdII)2(μ‐L0.75−)4]+. In each case, the first alternative was shown to be most appropriate. Remarkable results include the preference of platinum for mononuclear planar [PtL2] with an N‐Pt‐N bite angle of 62.8(2)° in contrast to [Pd2L4], and the dimetal (Pd24+→Pd25+) instead of ligand (L−→L ) oxidation of the dinuclear palladium compound. Qualitatively different structures and electron transfer behavior have been established for platinum and palladium complexes [PtL2]0/+ and [Pd2L4]0/+ with a redox‐active amidinato ligand L−/L..
Author Záliš, Stanislav
Filippou, Vasileios
Ehret, Fabian
Bubrin, Martina
Blickle, Svenja
Kaim, Wolfgang
AuthorAffiliation 2 J. Heyrovský Institute of Physical Chemistry, v.v.i. Academy of Sciences of the Czech Republic Dolejškova 3 18223 Prague Czech Republic
1 Institut für Anorganische Chemie Universität Stuttgart Pfaffenwaldring 55 70550 Stuttgart Germany
AuthorAffiliation_xml – name: 1 Institut für Anorganische Chemie Universität Stuttgart Pfaffenwaldring 55 70550 Stuttgart Germany
– name: 2 J. Heyrovský Institute of Physical Chemistry, v.v.i. Academy of Sciences of the Czech Republic Dolejškova 3 18223 Prague Czech Republic
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  organization: Universität Stuttgart
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  givenname: Svenja
  surname: Blickle
  fullname: Blickle, Svenja
  organization: Universität Stuttgart
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  organization: Universität Stuttgart
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  givenname: Stanislav
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  surname: Kaim
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BackLink https://www.ncbi.nlm.nih.gov/pubmed/32959415$$D View this record in MEDLINE/PubMed
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ISSN 0947-6539
1521-3765
IngestDate Tue Sep 30 16:49:13 EDT 2025
Sun Nov 09 09:15:17 EST 2025
Tue Oct 07 07:14:02 EDT 2025
Thu Apr 03 07:13:29 EDT 2025
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Fri Dec 05 22:45:40 EST 2025
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Sat Nov 29 07:11:34 EST 2025
Wed Jan 22 16:29:57 EST 2025
IsDoiOpenAccess true
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Issue 10
Keywords oxidation states
ORDER
ELECTRON
MONONUCLEAR
electron transfer
APPROXIMATION
spin distribution
spectroelectrochemistry
REACTIVITY
radical ligands
METAL
Language English
License 2020 Wiley-VCH GmbH.
This is an open access article under the terms of the http://creativecommons.org/licenses/by/4.0/ License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited.
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Snippet Reaction of [Pt(DMSO)2Cl2] or [Pd(MeCN)2Cl2] with the electron‐rich LH=N,N’‐bis(4‐dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2] (1) but...
Reaction of [Pt(DMSO) 2 Cl 2 ] or [Pd(MeCN) 2 Cl 2 ] with the electron‐rich LH=N,N’‐bis(4‐dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL 2 ] ( 1 )...
Reaction of [Pt(DMSO)(2)Cl-2] or [Pd(MeCN)(2)Cl-2] with the electron-rich LH = N,N'-bis(4-dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2] (1) but...
Reaction of [Pt(DMSO) Cl ] or [Pd(MeCN) Cl ] with the electron-rich LH=N,N'-bis(4-dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL ] (1) but...
Reaction of [Pt(DMSO)2 Cl2 ] or [Pd(MeCN)2 Cl2 ] with the electron-rich LH=N,N'-bis(4-dimethylaminophenyl)ethanimidamide yielded mononuclear [PtL2 ] (1) but...
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SubjectTerms Cations
Chemistry
Chemistry, Multidisciplinary
Computer applications
Crystal structure
Crystals
Electrochemistry
electron transfer
Ligands
Magnetic resonance
Oxidation
oxidation states
Palladium
Palladium compounds
Physical Sciences
Platinum
radical ligands
Science & Technology
Single crystals
spectroelectrochemistry
Spectroscopy
spin distribution
Valence
Title Structural and Oxidation State Alternatives in Platinum and Palladium Complexes of a Redox‐Active Amidinato Ligand
URI https://onlinelibrary.wiley.com/doi/abs/10.1002%2Fchem.202003636
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https://www.ncbi.nlm.nih.gov/pubmed/32959415
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https://www.proquest.com/docview/2444881606
https://pubmed.ncbi.nlm.nih.gov/PMC7986709
Volume 27
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