Rad, Nazli E., Junk, Peter C., Deacon, Glen B., Taidakov, Ilya V., and Wang, Jun (2020) Synthesis and structural characterisation of lithium, zinc, and aluminium pyrazolate complexes. Australian Journal of Chemistry, 73 (6). pp. 520-528.

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Abstract

The reaction of nBuLi with 3,5-dimethylpyrazole (Me(2)pzH) in Et2O or tmeda/hexane (tmeda=N,N,N ',N '-tetramethylethane-1,2-diamine) and with 3,5-dimethyl-4-nitropyrazolate (Me(2)pzHNO(2)) in THF results in the formation of three structurally diverse lithium pyrazolates: namely an Et2O-solvated tetrameric complex [Li-4(Me(2)pz)(4)(OEt2)(4)], bridged entirely with mu-eta(2):eta(1)-pyrazolate bonding, a hexanuclear complex [Li-6(Me(2)pz)(6)(tmeda)(2)] with four different coordination modes (mu-eta(1):eta(1), mu-eta(2):eta(1), mu(3)-eta(1):eta(2):eta(1) and mu(3)-eta(2):eta(2):eta(1)), and a new polymeric compound [Li-2(Me(2)pzNO(2))(2)(thf)(2)](n), with [Li-2(Me(2)pzNO(2))(2)(thf)(2)] groups linked by -NO2 coordination. A mononuclear zinc complex [Zn(tBu(2)pz)(2)(tBu(2)pzH)(2)].1/2THF (tBu(2)pzH=3,5-di-tert-butylpyrazole) was prepared by reaction of tBu(2)pzH with ZnEt2, unidentate tBu(2)pz groups being stabilised by N-HN hydrogen bonding. Treatment of 3,5-diphenylpyrazole (Ph(2)pzH) with trimethylaluminium (mole ratio 3:1) in THF led to the formation of dinuclear [AlMe2(mu-Ph(2)pz)](2).1/2THF.

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