Synthesis, structure and EPR spectroscopy of a vanadium(IV)–amide metallacyclic complex
1999; Elsevier BV; Volume: 285; Issue: 1 Linguagem: Inglês
10.1016/s0020-1693(98)00261-8
ISSN1873-3255
AutoresCharles R. Cornman, Edward P. Zovinka, Yvette D. Boyajian, Marilyn M. Olmstead, B.C. Noll,
Tópico(s)Metal-Catalyzed Oxygenation Mechanisms
ResumoThe crystal structures and EPR spectra for two dinuclear, metallacyclic VIV complexes are reported. The coordinating ligands include a rare example of vanadium(IV) coordinated to the carbonyl oxygen of an amide moiety. In the solid state, the cavity of these complexes encircles two molecules of methylene chloride which interact only weakly with the metallacycle. EPR spectra are typical of mononuclear VIV ion indicating that the spins are not interacting. Crystal data: for 1, C21H20Cl8N4O3V, M = 710.95, triclinic, space group P1, a = 10.543(2), b = 11.999(3), c = 13.654(2) Å, α = 64.170(14), β = 70.084(12), γ = 87.19(2)°, U = 1451.6(5) Å3, Z = 2, Dc = 1.627 g cm−3, T = 123(2) K, no. of unique reflections = 3797, no. of parameters = 355, R1 = 0.0882, wR2 = 0.1892 (all data). Crystal data for 2: C40.5H45Cl13N8O6V, M = 71302.63, triclinic, space group P1, a = 11.933(5), b = 12.020(3), c = 12.047(4) Å, α = 63.24(2), β = 65.46(3), γ = 80.06(3)°, U = 1403.4(9) Å3, Z = 2, Dc = 1.54 g cm−3, T = 130 K, no. of unique reflections = 3663, no. of parameters = 224, R1 = 0.1271, Rw = 0.1384 (F > 4.0σ(F)).
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