Bimetallic dioxidovanadium(V) complex containing a malonohydrazide derivative ligand: Synthesis, characterization, and crystal structure

S. D. Kurbah
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Abstract

In this paper, we report the synthesis and characterization of the dioxidovanadium(V) complex derived from a malonohydrazide ligand (N'1,N'3-bis(2-hydroxybenzylidene) malonohydrazide). The newly synthesized complex was characterized by infrared spectroscopy (IR), nuclear magnetic resonance (NMR), and the structure of the complex was also established by a single crystal X-ray diffraction study. The bimetallic complex crystallizes in the triclinic space group P-1 with the following parameters a = 10.8273(5) Å, b = 11.4677(6) Å, c = 15.0366(8) Å, α = 81.591(4)°, β = 83.018(4)°, γ = 76.326(4)°, V = 1787.23(16) Å3, Z = 2, T = 292.5(2) K, μ(MoKα) = 0.600 mm-1, Dcalc = 1.463 g/cm3, 11730 reflections measured (6.236° ≤ 2Θ ≤ 58.062°), 7981 unique (Rint = 0.0231, Rsigma = 0.0506) which were used in all calculations. The final R1 was 0.0496 (I > 2σ(I)) and wR2 was 0.1255 (all data). The ligand was coordinated to the metal ions in a tridentate fashion through the donor O/N/O atoms. The metal ions adopted a square pyramidal geometry with slight distortion. Reaction of the complex with hydrogen peroxide was also carried out, and it was found that the complex reacts with hydrogen peroxide to form a peroxo complex.
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含丙二酰肼衍生物配体的双金属二氧化钒配合物:合成、表征和晶体结构
本文报道了丙二酰肼配体(N' 1,n '3-二(2-羟基苄基)丙二酰肼)衍生的二氧化钒配合物的合成和表征。通过红外光谱(IR)、核磁共振(NMR)对新合成的配合物进行了表征,并通过单晶x射线衍射研究确定了配合物的结构。双金属配合物在三斜空间群P-1中结晶,参数为a = 10.8273(5) Å, b = 11.4677(6) Å, c = 15.0366(8) Å, α = 81.591(4)°,β = 83.018(4)°,γ = 76.326(4)°,V = 1787.23(16) Å3, Z = 2, T = 292.5(2) K, μ(mok - α) = 0.600 mm-1, Dcalc = 1.463 g/cm3,测量反射11730个(6.236°≤2Θ≤58.062°),唯一7981个(Rint = 0.0231, Rsigma = 0.0506)。最终R1为0.0496 (I > 2σ(I)), wR2为0.1255(所有数据)。配体通过给体O/N/O原子与金属离子以三叉配位方式配位。金属离子呈棱锥形,有轻微的畸变。还进行了配合物与过氧化氢的反应,发现配合物与过氧化氢反应形成过氧配合物。
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