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Synthesis of Unprecedented 4d/4f-Polypnictogens.

ABSTRACT: A series of 4d/4f-polyarsenides, -polyarsines and -polystibines was obtained by reduction of the Mo-pnictide precursor complexes [{Cp^t Mo(CO)₂ }₂ (μ,η^2:2 -E₂ )] (E=As, Sb; Cp^t =tBu substituted cyclopentadienyl) with two different divalent samarocenes [Cp*₂ Sm] and [(Cp^Me4nPr )₂ Sm]. For the reductive conversion of the Mo-stibide only one product was isolated, featuring a planar tetrastibacyclobutadiene moiety as an unprecedented ligand for organometallic compounds. For the corresponding Mo-arsenide a tetraarsacyclobutadiene and a second species with a side-on coordinated As₂ ^2- anion was isolated. The latter can be considered as reaction intermediate for the formation of the tetraarsacyclobutadiene.

SUBMITTER: Reinfandt N

PROVIDER: S-EPMC7986065 | biostudies-literature | 2021 Feb

REPOSITORIES: biostudies-literature

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Synthesis of Unprecedented 4d/4f-Polypnictogens.

Reinfandt Niklas N Schoo Christoph C Dütsch Luis L Köppe Ralf R Konchenko Sergey N SN Scheer Manfred M Roesky Peter W PW

Chemistry (Weinheim an der Bergstrasse, Germany) 20210114 12

A series of 4d/4f-polyarsenides, -polyarsines and -polystibines was obtained by reduction of the Mo-pnictide precursor complexes [{Cpt Mo(CO)2 }2 (μ,η2:2 -E2 )] (E=As, Sb; Cpt =tBu substituted cyclopentadienyl) with two different divalent samarocenes [Cp*2 Sm] and [(CpMe4nPr )2 Sm]. For the reductive conversion of the Mo-stibide only one product was isolated, featuring a planar tetrastibacyclobutad ...[more]

PMID: 33010187

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Project description:The reaction between the 2-(1-(2,6-di(pyrazol-1-yl)-4-methylpyridyl)-4,5-(4,5-bis(propylthio)-tetrathiafulvalenyl)-1H-benzimidazol-2-yl)-pyridine ligand (L), 1 equivalent of Ln(hfac)3·2H2O/Dy(tta)3·2H2O (hfac- = 1,1,1,5,5,5-hexafluoroacetylacetonate, tta- = 2-thenoyltrifluoroacetonate) and M(hfac)2·2H2O leads to the formation of heteroleptic 3d-4f dinuclear complexes of formula [MLn(hfac)5(L)]n (M(II) = Cd, Zn, Co, Mn, Ni and Ln(III) = Dy, Yb, Nd) and [ZnDy(tta)2(hfac)3(L)]·(CH2Cl2). Their X-ray structures reveal that the two coordination sites are occupied by one Ln(III) ion and one M(II) transition metal respectively. The M(II) ions are coordinated to the benzoimidazolylpyridine (bzip) moiety in a N2O4 coordination sphere, while the Ln(III) ions are coordinated to the 2,6-di(pyrazol-1-yl)-4-pyridine (dpp) moiety in a N3O6 surrounding. When Dy(III) ion is used a field-induced Single-Molecule Magnet (SMM) behavior is detected with a magnetic relaxation time slightly dependent to the nature of the vicinal divalent transition metal. On the other hand, when the Yb(III) is used, intense, moderated or quenched 2F5/2 → 2F7/2 NIR luminescence is observed when the Yb(III) ion is respectively associated with the Zn(II), Mn(II) and Ni(II)/Co(II) ion. The emission intensity can be modulated in function of the metal-to-ligand charge transfer and d-d transition intensities. The replacement of the divalent transition metal by a trivalent lanthanide leads to the formation of heteroleptic 4f-4f' dinuclear complexes of formula [Ln2-xLn'x(hfac)6(L)]·a(CH2Cl2)·b(C6H14) and [Dy1.11Nd0.89(tta)3(hfac)3(L)]. The coordination selectivity is based on the radius. Among the 4f-4f' series, the Dy(III) derivatives displayed such ion in N2O6 eight-coordinated sphere allowing the observation of SMM behavior. The three compounds [Dy1.21Nd0.79(hfac)6(L)]·2(CH2Cl2)·(C6H14), [Yb1.04Nd0.96(hfac)6(L)] and [YbPr(hfac)6(L)] displayed respectively Nd(III), modarated Yb(III) and intense Yb(III) NIR emissions.

Dataset Information

Synthesis of Unprecedented 4d/4f-Polypnictogens.

Publications

Synthesis of Unprecedented 4d/4f-Polypnictogens.

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