Formation of Spirocyclic Imidophosphinato Complexes: Crystal Structures of and

DOI: 10.1039/DT9910001285

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 1285 - 1290 (1991)

Update date:2022-08-04

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Authors:

Rietzel, Mathias

Roesky, Herbert W.

Katti, Kattesh V.

Noltemeyer, Mathias

Symons, Martyn C. R.

Abu-Raqabah, Atieh

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Article abstract of DOI:10.1039/DT9910001285

Treatment of tetrahydrofuran (thf) solutions of 1b with Bu^tOH, LiOBu^t or NaOSiPh3 affords in small yields the spirocyclic vanadyl complex 2. This complex is formed in nearly quantitative yield from and Na.It crystallizes in the monoclinic space group P2₁/c with a = 1572.0(8), b = 1056.3(5), c = 2685.0(13) pm, β = 94.30(2) deg and Z = 4.The structure was refined to R = 0.033, R' = 0.044.The nitrogen atoms in 1b adjacent to the metal have been replaced by oxygen atoms during alcoholysis.The V atom has a square-pyramidal geometry.The d¹ electronic state was confirmed by ESR measurements.Reaction of MoOCl4 and Cl yields the already known 1a and the spirocyclic molybdenum compound 3.The 1:1 MeCN adduct of 3 crystallizes in the acentric space group P1 with a = 1087.1(5), b = 1156.4(6), c = 1166.5(6) pm, α = 82.86(2), β = 68.26(2), γ = 64.15(2) deg and Z =1.The Mo atom has a distorted-octahedral geometry with short Mo-N bond lengths (average 177.8 pm).

Full text of DOI:10.1039/DT9910001285

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