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

UR - http://www.scopus.com/inward/record.url?scp=85119128899&partnerID=8YFLogxK

UR - https://www.mendeley.com/catalogue/f31bbb1d-878a-31be-aa3b-92c29c641b70/

U2 - 10.1134/S0022476621100139

DO - 10.1134/S0022476621100139

M3 - Article

AN - SCOPUS:85119128899

VL - 62

SP - 1580

EP - 1587

JO - Journal of Structural Chemistry

JF - Journal of Structural Chemistry

SN - 0022-4766

IS - 10

ER -