New Interventions by silicone grease in synthesis

Junk, Peter Courtney; Werner, Daniel; Rad, N. E.; Guo, Zhifang; Deacon, Glen B.

doi:10.1002/zaac.202200222

Zeitschrift anorg allge chemie

2022

DOI: 10.1002/zaac.202200222

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New Interventions by silicone grease in synthesis

Peter Courtney Junk

Daniel Werner

N. E. Rad

et al.

Abstract: In redox‐transmetallation protolysis (RTP) reactions in tetrahydrofuran (thf) between excess scandium or cerium metal, Hg(C6F5)2 and 3,5‐dimethylpyrazole (Me2pzH) in silicone greased Schlenk flasks, formation of the 3,5‐dimethyl‐1‐pyrazolyl(dimethyl)siloxide (Me2pzSiMe2O) ligand was observed. Thus the former reaction gave [Sc2(Me2pz)4(Me2pzSiMe2O)2] 1 in good yield, whilst the latter gave a mixture of [Ce4O(Me2pz)9(Me2pzSiMe2O)2] 2 a, [Ce4O(Me2pz)11] 2 b, both mixed oxidation state species, and the CeIV comple… Show more

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Synthesis and Structures of Oxide ‐Centred Alkali Metal (K, Li)/Lanthanoid (Ln3 or 4) 3,5‐Dimethylpyrazolate Cages ‐ Herbert Schumann Revisited

Werner,

Guo,

Deacon

et al. 2024

Chemistry An Asian Journal

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Reaction of lanthanoid tris(3,5‐dimethylpyrazolate) compounds, [Ln(Me2pz)3(thf)]2 (Ln = La 1a, Ce, Pr, Dy 1b, Yb, Lu) with potassium or lithium bistrimethylsilylamide and with or without added 3,5‐dimethylpyrazole, or of lanthanoid tris(bistrimethylsilyl)amide complexes with potassium bistrimethylsilylamide and 3,5‐dimethylpyrazole have yielded a variety of oxide centred Ln3 or Ln4/(K or Li)1‐3 multinuclear cages, namely, [La4O(Me2pz)11K(thf)2] (2a), [La4O(Me2pz)11Li(Me2pzH)]⋅0.5Hexane (2b), [La4O(Me2pz)10(Me2pzH)] (2c) (from heating 1a in toluene), [Ce3O(Me2pz)9K2(dme)2] (3a), [Ce3O(Me2pz)9Li2(thf)2]⋅0.5Hexane (3b) and [Ce(Me2pz)5Li2(thf)3] (3c), which crystallized together, [Ce3O(Me2pz)10K3(thf)3] (3d), [Pr3O(Me2pz)10K3(thf)3] (4), [Dy3O(Me2pz)9K2(thf)2]·THF (5), [Yb3O(Me2pz)9K2(thf)2]·THF (6), and [Lu3O(Me2pz)9K2(thf)2]⋅THF (7). Crystals of {[K8(Me2pz)8(thf)2]⋅THF}∞ (8) were also obtained from the preparation of 7. From reaction of [Ce(Me2pz)3(thf)]2 with potassium tert‐butoxide in toluene, the cerium(IV) heterobimetallic polymer [Ce2(Me2pz)6(OtBu)4K2]∞ (9) was isolated. In the Ln3O and the Ln4O cages, the Ln atoms have triangular and distorted tetrahedral arrangements about the central oxygen, respectively. All metals are bound to the cages by a variety of pyrazolate binding modes, with up to five different exhibited in some structures, and a new coordination mode, μ4‐1κ(N):2κ(N′):η5:η5, was observed in two complexes.

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Synthesis and Structures of Oxide ‐Centred Alkali Metal (K, Li)/Lanthanoid (Ln3 or 4) 3,5‐Dimethylpyrazolate Cages ‐ Herbert Schumann Revisited

Werner,

Guo,

Deacon

et al. 2024

Chemistry An Asian Journal

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show abstract

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New Interventions by silicone grease in synthesis

Cited by 1 publication

References 40 publications

Synthesis and Structures of Oxide ‐Centred Alkali Metal (K, Li)/Lanthanoid (Ln3 or 4) 3,5‐Dimethylpyrazolate Cages ‐ Herbert Schumann Revisited

Synthesis and Structures of Oxide ‐Centred Alkali Metal (K, Li)/Lanthanoid (Ln3 or 4) 3,5‐Dimethylpyrazolate Cages ‐ Herbert Schumann Revisited

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