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首页> 外文期刊>Crystal growth & design >Structural diversity of lanthanum-organic frameworks based on 1,4-phenylenebis(methylene)diphosphonic acid
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Structural diversity of lanthanum-organic frameworks based on 1,4-phenylenebis(methylene)diphosphonic acid

机译：基于1,4-亚苯基双（亚甲基）二膦酸的镧-有机骨架的结构多样性

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摘要

The preparation of five different compounds, [La_2(H _2pmd)_3(H_2O)_(12)] (1: 1D), [La _2(H_2pmd)(pmd)(H_2O)_2] (2: 3D), [La(H_3pmd)(H_2pmd)(H_2O)] (3: 3D), [La _2(H_2pmd)_3(H_2O)_2] (4: 3D), and [La_2(H_2pmd)(pmd)(H_2O)_4] (5: 3D), as crystalline materials from the reaction of 1,4-phenylenebis(methylene) diphosphonic acid (H4pmd) with lanthanum chloride is reported. Two different, fast, and economically viable synthetic approaches were employed with their various parameters being probed and, when possible, optimized to increase yields and purity: microwave-assisted synthesis (MWAS, in ca. 1 min) and a bench procedure using standard ambient conditions (one-pot, ca. 10 min). Compounds 1 and 2 were isolated as phase-pure crystalline materials. Compounds 3 and 4 were characterized by single-crystal X-ray diffraction from mixtures, and compound 5 was identified by powder X-ray diffraction studies (also from a physical mixture with 2). Structural details for all compounds were investigated by using in tandem X-ray diffraction (single-crystal and powder), electron microscopy (SEM and EDS), and FT-IR spectroscopy. Topological studies were also performed for all 3D networks. The conversion of compound 1 (1D) into 3D networks was investigated using hydrothermal, microwave, and one-pot methods: 1 was totally converted into phase-pure 2 via the hydrothermal method and one-pot method.
机译：制备五种不同的化合物[La_2（H _2pmd）_3（H_2O）_（12）（1：1D），[La _2（H_2pmd）（pmd）（H_2O）_2]（2：3D），[La （H_3pmd）（H_2pmd）（H_2O）]（3：3D），[La _2（H_2pmd）_3（H_2O）_2]（4：3D）和[La_2（H_2pmd）（pmd）（H_2O）_4]（5 ：3D），据报道是1，4-亚苯基双（亚甲基）二膦酸（H4pmd）与氯化镧反应的结晶物质。使用了两种不同的，快速且经济可行的合成方法，对它们的各种参数进行了探索，并在可能的情况下进行了优化，以提高收率和纯度：微波辅助合成（MWAS，约1分钟）和使用标准环境的实验步骤条件（一锅，约10分钟）。分离化合物1和2为纯相结晶材料。化合物3和4通过混合物的单晶X射线衍射进行表征，化合物5通过粉末X射线衍射研究（也从具有2的物理混合物）进行鉴定。通过串联X射线衍射（单晶和粉末），电子显微镜（SEM和EDS）和FT-IR光谱研究了所有化合物的结构细节。还对所有3D网络进行了拓扑研究。使用水热，微波和一锅法研究了化合物1（1D）向3D网络的转化：通过水热法和一锅法将1完全转化为纯相2。

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