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首页> 外文期刊>Crystal growth & design >Engineering Three-Dimensional Chains of Porous Nanoballs from a 1,2,4-Triazole-carboxylate Supramolecular Synthon
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Engineering Three-Dimensional Chains of Porous Nanoballs from a 1,2,4-Triazole-carboxylate Supramolecular Synthon

机译：1,2,4-三唑-羧酸盐超分子合成子的多孔纳米球的工程三维链

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摘要

Glycine ethyl ester was recruited in an amine exchange process based on a transamination to afford ethyl 4H-,2,4-triazol-4-yl-acetate (L1). The acid hydrolysis of this molecule leads to quantitative isolation of 4H-1,2,4-triazol-4-yl acetic acid (L2). This versatile synthon crystallizes in a noncentrosymmetric orthorhombic space group (Fdd2) with Z = 16. This crystal structure is the first one for a 1,2,4-triazole ligand constructed from an amino acid derivative. The strong intermolecular hydrogen bonding O-H center dot center dot center dot N (2.570(3) angstrom) connects molecules into infinite one-dimensional chains running parallel to the b axis, and the structure is further extended by numerous but moderate strength hydrogen bonds (C-H center dot center dot center dot O). Prominent features of L2 are the presence of diverse potential coordinating groups such as carboxylic acid and triazole on the same framework as well as the inherent flexibility of the ligand backbone. Reaction of L1 or L2 with aq. Cu(BF4)(2) in aq. DMF gives dark blue crystals which crystallize in a noncentrosymmetric, cubic space group (1 (4) over bar 3m) and which were formulated as [Cu-3(mu(3)-O)(L2)(3). (H2O)(3)]BF4 center dot H2O (C1). The self-assembly of C3-symmetric, mu(3)-oxo bridged triangular tricopper secondary building blocks (SBB) formed an unique architecture which encompasses voluminous nanoball voids of 1 nm. The total solvent accessible volume is 4477.5 angstrom(3) which accounts for 48% of the cell volume. The crystal network stability was studied by thermogravimetric analysis (TGA) differential thermal analysis (DTA) and scanning electron microscopy (SEM) analyses. Sorption properties and gas storage capacities were measured by BET. CI shows no preference for N-2(g), but a reversible H-2(g) uptake of 21 cm(3)/g was observed, Morphology analysis by SEM on single crystals of CI shows "ultrawells" of square shape irregularly located on the surface, whose origin is due to desolvation or crystal defects. Mercury porosimetry measurements reveal pore size distribution with a diameter ranging from 350 nm to 2.3 mu m.
机译：在基于氨基转移的胺交换过程中募集甘氨酸乙酯，得到4H-，2,4-三唑-4-基乙酸乙酯（L1）。该分子的酸水解导致4H-1,2,4-三唑-4-基乙酸（L2）的定量分离。这种通用的合成子在Z = 16的非中心对称的正交晶体空间基团（Fdd2）中结晶。该晶体结构是由氨基酸衍生物构成的1,2,4-三唑配体的第一个晶体。强大的分子间氢键OH中心点中心点中心点N（2.570（3）埃）将分子连接到与b轴平行的无限一维链中，并且该结构进一步被众多但强度适中的氢键（CH中心点中心点中心点O）。 L 2的突出特征是在同一骨架上存在多种潜在的配位基团，例如羧酸和三唑，以及配体主链的固有柔性。 L1或L2与水溶液反应。水溶液中的Cu（BF4）（2） DMF产生深蓝色晶体，该晶体在非中心对称的立方空间群中（在条形3m上为1（4）结晶），配制成[Cu-3（mu（3）-O）（L2）（3）。 （H2O）（3）] BF4中心点H2O（C1）。 C3对称，mu（3）-氧桥三角tricopper二级构件（SBB）的自组装形成了一个独特的体系结构，其中包含1 nm的大量纳米球空隙。总溶剂可及体积为4477.5埃（3），占电池体积的48％。通过热重分析（TGA），差热分析（​​DTA）和扫描电子显微镜（SEM）分析研究了晶体网络的稳定性。吸附性能和储气量通过BET测量。 CI没有显示出对N-2（g）的偏爱，但是观察到21 cm（3）/ g的可逆H-2（g）吸收，通过SEM对CI的单晶进行的形态分析表明，不规则正方形的“超阱”位于表面上，其起源是由于去溶剂化或晶体缺陷。汞孔隙率法测量显示孔径分布范围为350 nm至2.3μm。

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