A series of hybrid hetero bimetallic metal–organic frameworks, as solid metal–organic precursors, have been prepared via a conventional hydrothermal method. Herein, we report a facile approach for the synthesis of novel crystalline organic–inorganic hybrid compounds of diaquabis(acetylacetonato)[nickel(II)/zinc(II)] in the presence of varying mole ratios of Ni(II)/Zn(II) mixed metal ions. C10H18O6Ni0.7Zn0.3 (N0.7Z0.3AA.2H2O) as an instance of the series has been investigated through detailed characterization. The crystal is composed of N0.7Z0.3AA units and two coordinated water molecules to form a monoclinic structure with space group P21/c. All the solid‐state structures have the metals in octahedral environments forming six‐membered chelate rings. The unit cell dimensions were obtained using single‐crystal X‐ray diffraction. Thermogravimetric analysis reveals that the hybrid compounds can be considered as suitable precursors for the synthesis of oxides via metal–organic chemical vapour deposition. At room temperature, all crystals clearly exhibit paramagnetic behaviour. Besides varying molar ratios of hybrid, the transition point of magnetic behaviour occurs at Ni critical concentration of around 10% in the hybrid. In addition, the magnetic susceptibility increases with increasing Ni content in the compounds.
We have synthesized novel metal organic hybrid mixed compounds of bis (acetylacetonato κ-O, O') [zinc(ii)/copper(ii)]. Taking C10H14O4Zn0.7Cu0.3 (Z0.7C0.3AA) as an example, the crystals are composed of Z0.7C0.3AA units and uncoordinated water molecules. Single-crystal X-ray diffraction results show that the complex Z0.7C0.3AA crystallizes in the monoclinic system, space group P21/n. The unit cell dimensions are a = 10.329(4) Å, b = 4.6947(18) Å, and c = 11.369(4) Å; the angles are α = 90°, β = 91.881(6)°, and γ = 90°, the volume is 551.0(4) Å(3), and Z = 2. In this process, the M(ii) ions of Zn and Cu mix and occupy the centers of symmetrical structural units, which are coordinated to two ligands. The measured bond lengths and angles of O-M-O vary with the ratio of metal species over the entire series of the complexes synthesized. The chemistry of the as-synthesized compounds has been characterized using infrared spectroscopy, mass spectroscopy, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy analysis, and the morphology of the products has been characterized using scanning electron microscopy. The thermal decomposition of the Z0.7C0.3AA composites measured by thermogravimetric analysis suggests that these complexes are volatile. The thermal characteristics of these complexes make them attractive precursors for metal organic chemical vapor deposition.
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