Structure and composition of [(nacnac)MnCl]2 (nacnac = HC(C(Me)N(2.6-i-Pr2C6H3))2) products reduced by potassium-intercalated graphite in toluene and benzene

M. Yu Afonin; A. Yu Sedelnikova; A. Yu Konokhova; T. S. Sukhikh; S. N. Konchenko

doi:10.1134/S0022476621100139

Structure and composition of [(nacnac)MnCl]₂ (nacnac = HC(C(Me)N(2.6-i-Pr₂C₆H₃))₂) products reduced by potassium-intercalated graphite in toluene and benzene

Переведенное название: Строение и состав продуктов восстановления [(nacnac)MnCl]2 (nacnac = HC(C(Me)N(2.6-i-Pr2C6H3))2) в толуоле и бензоле интеркалированным калием графитом

M. Yu Afonin, A. Yu Sedelnikova, A. Yu Konokhova, T. S. Sukhikh, S. N. Konchenko

Результат исследования: Научные публикации в периодических изданиях › статья › рецензирование

Аннотация

Изучено восстановление [(nacnac)MnCl]2 (1) (nacnac = HC(C(Me)N(2.6- i -Pr2C6H3))2) интеркалированным калием графитом KC8 в толуоле и бензоле. Установлено, что в обоих случаях происходит восстановление Mn(II) до Mn(I) с образованием димера [(nacnac)Mn]2 (2) со связью Mn-Mn. Кроме него образуются продукты взаимодействия с растворителем: в первом случае - продукт мета-депротонирования толуола [(nacnac)Mn( m -C6H4CH3)] (3), во втором - восстановления бензола [{Mn(nacnac)}2(m-h4:h4-C6H6)]C6H6 (4). Строение комплексов 3 и 4 установлено методом рентгеноструктурного анализа монокристаллов. Набор кристаллических продуктов реакции и их соотношение определены с помощью количественного рентгенофазового анализа методом Ритвельда: в случае толуола - 2, 3 и [(nacnac)MnH]2 в отношении 1:1:4; в случае бензола - 2, 4×C6H6 и 1 в отношении 3:8.5:1, а также следовые количества кристаллической фазы неустановленного строения.

Переведенное название	Строение и состав продуктов восстановления [(nacnac)MnCl]2 (nacnac = HC(C(Me)N(2.6-i-Pr2C6H3))2) в толуоле и бензоле интеркалированным калием графитом
Язык оригинала	английский
Страницы (с-по)	1580-1587
Число страниц	8
Журнал	Journal of Structural Chemistry
Том	62
Номер выпуска	10
DOI	https://doi.org/10.1134/S0022476621100139
Состояние	Опубликовано - окт. 2021

Предметные области OECD FOS+WOS

2.05 ТЕХНОЛОГИЯ МАТЕРИАЛОВ
1.04 ХИМИЧЕСКИЕ НАУКИ

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10.1134/S0022476621100139

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@article{4adce68120284db3913cd25bb1ba85a2,

title = "Structure and composition of [(nacnac)MnCl]2 (nacnac = HC(C(Me)N(2.6-i-Pr2C6H3))2) products reduced by potassium-intercalated graphite in toluene and benzene",

abstract = "The reduction of [(nacnac)MnCl]2 (1) (nacnac = HC(C(Me)N(2.6-i-Pr2C6H3))2) by potassium intercalated graphite KC8 in toluene and benzene is studied. It is established that in both cases, Mn(II) reduces to Mn(I), giving [(nacnac)Mn]2 dimer (2) with the Mn–Mn bond. In addition, solvent interaction products form. In the first case, the product of toluene meta-deprotonation [(nacnac)Mn(m-C6H4CH3)] (3) forms; in the second, the product of benzene reduction [{Mn(nacnac)}2(μ–η4:η4-C6H6)] C6H6 (4) forms. The structures of complexes 3 and 4 are determined by single crystal X-ray diffraction (XRD). A set of crystalline reaction products and their ratio is determined by quantitative powder XRD using the Rietveld method: in the case of toluene, 2, 3, and [(nacnac)MnH]2 are in a 1:1:4 ratio; in the case of benzene, 2, 4·C6H6, and 1 are in a 3:8.5:1 ratio, and also trace amounts of a crystalline phase with an unknown structure.",

keywords = "crystal structure, manganese, powder X-ray diffraction analysis, π-arene ligand, σ-aryl ligand",

author = "Afonin, {M. Yu} and Sedelnikova, {A. Yu} and Konokhova, {A. Yu} and Sukhikh, {T. S.} and Konchenko, {S. N.}",

note = "Funding Information: The work was supported by the Russian Science Foundation (Grant No. 19-73-00183) and the Ministry of Science and Higher Education of the Russian Federation (Projects Nos. 121031700321-3, 121031700313-8). Publisher Copyright: {\textcopyright} 2021, Pleiades Publishing, Ltd.",

year = "2021",

month = oct,

doi = "10.1134/S0022476621100139",

language = "English",

volume = "62",

pages = "1580--1587",

journal = "Journal of Structural Chemistry",

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publisher = "Springer GmbH & Co, Auslieferungs-Gesellschaf",

number = "10",

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Structure and composition of [(nacnac)MnCl]₂ (nacnac = HC(C(Me)N(2.6-i-Pr₂C₆H₃))₂) products reduced by potassium-intercalated graphite in toluene and benzene. / Afonin, M. Yu; Sedelnikova, A. Yu; Konokhova, A. Yu и др.

В: Journal of Structural Chemistry, Том 62, № 10, 10.2021, стр. 1580-1587.

Результат исследования: Научные публикации в периодических изданиях › статья › рецензирование

TY - JOUR

T1 - Structure and composition of [(nacnac)MnCl]2 (nacnac = HC(C(Me)N(2.6-i-Pr2C6H3))2) products reduced by potassium-intercalated graphite in toluene and benzene

AU - Afonin, M. Yu

AU - Sedelnikova, A. Yu

AU - Konokhova, A. Yu

AU - Sukhikh, T. S.

AU - Konchenko, S. N.

N1 - Funding Information: The work was supported by the Russian Science Foundation (Grant No. 19-73-00183) and the Ministry of Science and Higher Education of the Russian Federation (Projects Nos. 121031700321-3, 121031700313-8). Publisher Copyright: © 2021, Pleiades Publishing, Ltd.

PY - 2021/10

Y1 - 2021/10

N2 - The reduction of [(nacnac)MnCl]2 (1) (nacnac = HC(C(Me)N(2.6-i-Pr2C6H3))2) by potassium intercalated graphite KC8 in toluene and benzene is studied. It is established that in both cases, Mn(II) reduces to Mn(I), giving [(nacnac)Mn]2 dimer (2) with the Mn–Mn bond. In addition, solvent interaction products form. In the first case, the product of toluene meta-deprotonation [(nacnac)Mn(m-C6H4CH3)] (3) forms; in the second, the product of benzene reduction [{Mn(nacnac)}2(μ–η4:η4-C6H6)] C6H6 (4) forms. The structures of complexes 3 and 4 are determined by single crystal X-ray diffraction (XRD). A set of crystalline reaction products and their ratio is determined by quantitative powder XRD using the Rietveld method: in the case of toluene, 2, 3, and [(nacnac)MnH]2 are in a 1:1:4 ratio; in the case of benzene, 2, 4·C6H6, and 1 are in a 3:8.5:1 ratio, and also trace amounts of a crystalline phase with an unknown structure.

AB - The reduction of [(nacnac)MnCl]2 (1) (nacnac = HC(C(Me)N(2.6-i-Pr2C6H3))2) by potassium intercalated graphite KC8 in toluene and benzene is studied. It is established that in both cases, Mn(II) reduces to Mn(I), giving [(nacnac)Mn]2 dimer (2) with the Mn–Mn bond. In addition, solvent interaction products form. In the first case, the product of toluene meta-deprotonation [(nacnac)Mn(m-C6H4CH3)] (3) forms; in the second, the product of benzene reduction [{Mn(nacnac)}2(μ–η4:η4-C6H6)] C6H6 (4) forms. The structures of complexes 3 and 4 are determined by single crystal X-ray diffraction (XRD). A set of crystalline reaction products and their ratio is determined by quantitative powder XRD using the Rietveld method: in the case of toluene, 2, 3, and [(nacnac)MnH]2 are in a 1:1:4 ratio; in the case of benzene, 2, 4·C6H6, and 1 are in a 3:8.5:1 ratio, and also trace amounts of a crystalline phase with an unknown structure.

KW - crystal structure

KW - manganese

KW - powder X-ray diffraction analysis

KW - π-arene ligand

KW - σ-aryl ligand

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DO - 10.1134/S0022476621100139

M3 - Article

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SP - 1580

EP - 1587

JO - Journal of Structural Chemistry

JF - Journal of Structural Chemistry

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