New Chemistry Unit, Jawaharlal Nehru Centre for Advanced Scientific Research, Jakkur, Bangalore, 560064, India.
Dalton Trans. 2014 Feb 7;43(5):2153-60. doi: 10.1039/c3dt52484a.
Two new organic hybrid materials [H4V10O28][CuCl(H2O)2(1,10-phenanthroline)]2·4H2O (V10O28-CuCl-phen) and [H4V10O28][Cu(H2O)3(1,10-phenanthroline)]2·4H2O (V10O28-CuO-phen) were synthesized at room temperature. The effect of the presence and absence of AlCl3 on the single crystal growth of the two compounds was studied. The compounds were characterized using single crystal X-ray diffraction (XRD), scanning electron microscopy, energy dispersive spectroscopy, infra-red spectroscopy and thermogravimetric analysis. XRD studies on selected single crystals suggest that the compounds consist of supramolecular 3D layer structures constructed from a tetra-protonated [V10O28] unit and the organometallic complex Cu(1,10-phen) with Cl and 2H2O molecules in the presence of AlCl3 in V10O28-CuCl-phen and with 3H2O molecules in V10O28-CuO-phen which was confirmed by TGA studies. Both compounds crystallize in the triclinic space group P1[combining macron]: a = 8.3886(3) Å, b = 10.4266(4) Å, c = 13.5860(5) Å, α = 92.440(2)°, β = 92.315(2)°, γ = 98.160(2)° for V10O28-CuCl-phen and a = 8.3733(5) Å, b = 10.4132(6) Å, c = 13.5904(8) Å, α = 92.295(4)°, β = 92.331(2)°, γ = 98.086(4)° for V10O28-CuO-phen. Magnetic measurements suggest that Cu exists in magnetic +2 oxidation state in V10O28-CuCl-phen and non-magnetic +1 oxidation state in V10O28-CuO-phen.
两种新的有机杂化材料[H4V10O28][CuCl(H2O)2(1,10-菲咯啉)]2·4H2O(V10O28-CuCl-phen)和[H4V10O28][Cu(H2O)3(1,10-菲咯啉)]2·4H2O(V10O28-CuO-phen)在室温下合成。研究了 AlCl3 的存在和不存在对两种化合物单晶生长的影响。利用单晶 X 射线衍射(XRD)、扫描电子显微镜、能谱、红外光谱和热重分析对化合物进行了表征。对选定单晶的 XRD 研究表明，在 V10O28-CuCl-phen 中，化合物由四质子化[V10O28]单元和有机金属配合物 Cu(1,10-菲咯啉)与 Cl 和 2H2O 分子组成的超分子 3D 层结构组成，而在 V10O28-CuO-phen 中，化合物由 3H2O 分子组成，这一结果得到了 TGA 研究的证实。这两种化合物都结晶在三斜空间群 P1[combining macron]中：a = 8.3886(3)Å, b = 10.4266(4)Å, c = 13.5860(5)Å, α = 92.440(2)°，β = 92.315(2)°，γ = 98.160(2)°，V10O28-CuCl-phen 的 a = 8.3733(5)Å, b = 10.4132(6)Å, c = 13.5904(8)Å, α = 92.295(4)°，β = 92.331(2)°，γ = 98.086(4)°，V10O28-CuO-phen。磁性测量表明，Cu 在 V10O28-CuCl-phen 中存在磁+2 氧化态，在 V10O28-CuO-phen 中存在非磁+1 氧化态。
