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首页> 外文期刊>Crystal growth & design >Production and Characterization of a New Copper(II) Propanoate-Isonicotinamide Adduct Obtained via Slow Evaporation and using Supercritical CO2 as an Antisolvent
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Production and Characterization of a New Copper(II) Propanoate-Isonicotinamide Adduct Obtained via Slow Evaporation and using Supercritical CO2 as an Antisolvent

机译：通过缓慢蒸发和使用超临界二氧化碳作为防溶剂获得的新铜（II）丙酸乙酯 - 异滴烟酰胺加合物的生产和表征

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摘要

A new adduct of isonicotinamide (INA) with copper(II) propanoate [Cu(C-3)(2)] was prepared [Cu-2(C-3)(4)(INA)(4)] using two different methods. This type of compound shows high fungicidal activity. Solvent evaporation from ethanol rendered crystals suitable for single-crystal X-ray diffraction. Furthermore, a new semicontinuous method capable of simultaneous crystallization and micronization of the adduct using supercritical CO2 , the supercritical antisolvent technique (SAS), was also assessed. Crystals were characterized using powder X-ray diffraction, infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis coupled with mass spectrometry, scanning electron microscopy, and microelemental analysis. In the adduct, two copper(II) ions are coordinated through two bridging and two chelating carboxylates to the propanoate anions forming approximately a plane. Each metal ion is then coordinated with the pyridine nitrogen of two different INA molecules that behave as monodentate ligands. The amide groups of the INA form H-bonds with other amide and carboxylate groups forming a molecular crystal with a three-dimensional H-bond arrangement of the binuclear units. With the SAS technique, crystals 100-fold smaller than those obtained by slow evaporation were obtained, proving SAS as a suitable method for mixed-ligand complexes preparation with reduced particle size and therefore expected bioavailability enhancement.
机译：使用两种不同的方法制备[Cu-2（C-3）（4）（4）]制备具有铜（II）丙烷[Cu（C-3）（4）（Ina）（4）]的新加合物。这种类型的化合物显示出高杀菌活性。从适合单晶X射线衍射的乙醇渲染晶体的溶剂蒸发。此外，还评估了一种能够同时结晶和使用超临界CO2结晶和微粉化加合物的新的半连续方法，超临界抗临时技术（SAS）。使用粉末X射线衍射，红外光谱，差示扫描量热法，热重分析，与质谱，扫描电子显微镜和微精检耦合。在加合物中，通过两个桥接和两个螯合羧酸盐与丙烷阴离子的两种桥接和两种螯合羧酸酯协调，形成大致平面。然后将每个金属离子与两种不同的Ina分子的吡啶氮配位，该分子表现为单常液配体。 INA的酰胺基团与其他酰胺和羧酸盐基团形成，形成分子晶体，其具有双核单元的三维H键布置。利用SAS技术，获得了小于通过缓慢蒸发获得的晶体100倍，作为混合配体复合物制剂的合适方法，其具有降低的粒度，因此预期的生物利用度增强。

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