Synthesis and Crystal Structures of Dinuclear Dioxidovanadium(V) and Tetranuclear Oxidovanadium(IV) Complexes with 2,6-Bis(hydroxymethyl)-4-methylphenol

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  • MIKURIYA Masahiro
    Department of Applied Chemistry for Environment and Research Center for Coordination Molecule-based Devices, School of Science and Technology, Kwansei Gakuin University
  • FUKUTANI Masami
    Department of Applied Chemistry for Environment and Research Center for Coordination Molecule-based Devices, School of Science and Technology, Kwansei Gakuin University
  • YOSHIOKA Daisuke
    Department of Applied Chemistry for Environment and Research Center for Coordination Molecule-based Devices, School of Science and Technology, Kwansei Gakuin University

抄録

μ-Alkoxido-bridged dinuclear dioxidovanadium(V) and tetranuclear oxidovanadium(IV) complexes with 2,6-bis(hydroxymethyl)-4-methylphenol (H3bhmp), [Et3NH]2[(VO2)2(Hbhmp)2] (1) and [Et3NH]2[(VO)4(Hbhmp)2(MeO)2(SO4)2] (2) were synthesized. The crystal structures were determined by the single-crystal X-ray diffraction method at 293 K. Compound 1 crystallizes in the triclinic space group P1 with a = 8.5059(15)Å, b = 9.8815(17)Å, c = 11.3339(19)Å, α = 82.916(3)°, β = 83.819(3)°, γ = 65.595(3)°, V = 859.2(3)Å3, Dx = 1.358 g/cm3, Dm (floatation) = 1.358 g/cm3, and Z = 1. However, compound 2 crystallizes in the triclinic space group P1 with a = 10.731(14)Å, b = 11.373(15)Å, c = 11.558(15)Å, α = 104.28(3)°, β = 112.76(2)°, γ = 108.23(2)°, V = 1121(3)Å3, Dx = 1.568 g/cm3, Dm (floatation) = 1.554 g/cm3, and Z = 1. The R1 [I > 2σ(I)] and wR2 (all data) values are 0.0409 and 0.1166 for 1 and 0.0514 and 0.1454 for 2, respectively. Compound 1 consists of triethylammonium cations and the di-μ-alkoxido-bridged dinuclear dioxidovanadium(V) complex anion [(VO2)2(Hbhmp)2]2-, whereas compound 2 consists of triethylammonium cations and the di-μ-sulfato-di-μ-methoxido-di-μ-alkoxido-di-μ-phenoxido-bridged tetranuclear oxidovanadium(IV) complex anion [(VO)4(Hbhmp)2(MeO)2(SO4)2]2- with a parallelogram array of four vanadium atoms.

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