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Formation of Spirocyclic Imidophosphinato Complexes: Crystal Structures of and

DOI: 10.1039/DT9910001285

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

Update date:2022-08-04

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Authors:

Rietzel, MathiasRietzel, Mathias

Roesky, Herbert W.Roesky, Herbert W.

Katti, Kattesh V.Katti, Kattesh V.

Noltemeyer, MathiasNoltemeyer, Mathias

Symons, Martyn C. R.Symons, Martyn C. R.

Abu-Raqabah, AtiehAbu-Raqabah, Atieh

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Article abstract of DOI:10.1039/DT9910001285

Treatment of tetrahydrofuran (thf) solutions of 1b with ButOH, LiOBut 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deg and Z = 4.The structure was refined to R = 0.033, R' = 0.044.The nitrogen atoms in 1b adjacent to the metal have been replaced by oxygen atoms during alcoholysis.The V atom has a square-pyramidal geometry.The d1 electronic state was confirmed by ESR measurements.Reaction of MoOCl4 and Cl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).

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Product name:bis(N-diphenylphosphoryl-P,P-diphenylphosphinimidato-κ(2)O,O')-oxovanadium(IV)

Cas No:135436-25-8

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