CN105001246B - 8‑氨基喹啉席夫碱叠氮锌金属配合物及其制备方法 - Google Patents
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Abstract
本发明公开了8‑氨基喹啉席夫碱叠氮锌金属配合物及其制备方法。将8‑氨基喹啉、水杨醛和三乙胺均溶于有机溶剂中,搅拌下回流、冷却;再在上述溶液中加入溶有六水合高氯酸锌和叠氮化钠的有机溶液,常温搅拌7天,过滤,滤液自然挥发,三十天后得到灰色针状晶体;过滤,乙醚洗涤滤饼,得到分子式为C32H24N10O3Zn2的配合物单晶。该配合物通过氢键和π…π芳香环堆积构成三维超分子结构。
Description
技术领域
本发明属于有机合成领域,涉及一种8-氨基喹啉席夫碱叠氮锌金属配合物单晶以及制备方法。
背景技术
金属有机配合物以其结构的多样性和独特的理化性质,引发了人们广泛关注,成为新型材料的重要成员。其中,过渡金属和稀土金属有机配合物的中心离子具有价电子数多变和空的d轨道或空的f-轨道的引入,给光、电、磁功能材料带来了新的研究空间和新的变化,并赋予某些独特的优点,如:有机金属配合物的偶极矩和极化率在基态时较大,而其激发态能量较低,从而使其对于光电响应速度有显著的提高;电子在金属和配体之间、配体内部的相互作用,能诱导分子内的电荷分布发生畸变;金属为中心粒子,与有机配体可以构筑形状各异的零维、一维、二维和三维结构,这些独特的分子结构可能具有光电磁性能,是纯粹的有机或无机分子无法独立完成的。为此,选择有机配体与过渡金属离子配位形成金属有机配合物是功能化材料的潜在来源。
发明内容
本发明的第一个目的是提供一种8-氨基喹啉席夫碱叠氮锌金属配合物。该配合物通过氢键和π…π芳香环堆积构成三维超分子结构。
本发明所涉及的8-氨基喹啉席夫碱叠氮锌金属配合物的化学式为(L1)2·Zn2·(N3)2·H2O,其中L1为8-氨基喹啉席夫碱阴离子:
本发明的第二个目的是提供一种8-氨基喹啉席夫碱叠氮锌金属配合物的制备方法。
为达到上述目的,本发明8-氨基喹啉席夫碱叠氮锌金属配合物的制备方法是:将8-氨基喹啉、水杨醛和三乙胺均溶于有机溶剂中,搅拌下回流,冷却;再在上述溶液中加入溶有六水合高氯酸锌和叠氮化钠的有机溶液,常温搅拌7天,过滤,滤液自然挥发,三十天后得到灰色针状晶体;过滤,乙醚洗涤滤饼,得目标配合物。
所述的回流时间为2~4小时。8-氨基喹啉、水杨醛、三乙胺、六水合高氯酸锌、叠氮化钠的摩尔比为1∶1∶1~1.5∶1∶1~1.5;上述有机溶剂为甲醇、乙醇、丙酮。
本发明选择8-氨基喹啉席夫碱、叠氮酸根为配体,锌为中心离子,进行自组装,得到具有三维超分子结构的金属-有机配合物单晶。它们的二级结构单元为:晶体属于三斜晶系,空间群为P-1,晶胞参数为:α=97.091(2)°,β=106.120(10)°,γ=91.787(2)°。该配合物的不对称单元中含2个Zn2+,2个L1配体、2个N3 -和1个游离的H2O。Zn2为5配位,两个配位N原子分别来自于两个N3 -1,且其中一个N3 -1的同一N原子还以头-头形式与Zn1配位,从而联接两个Zn原子,同时参与配位的另两个N原子和一个O原子来自于同一个L1配体,且该O原子还与Zn1配位,该配位模式属畸变的四方锥;Zn1也为5配位,除与上述一个N、一个O配位外,参与配位的其余两个N原子和一个氧原子来自另一个L1配体,也构成了畸变的四方锥;同时,该结构单元中还存在一个游离水分子。分子间弱的氢键和π…π芳香环堆积构成三维超分子结构。本发明制备方法简单,原料易得,且该配合物具有三维超分子结构。
附图说明
图1是本发明8-氨基喹啉席夫碱叠氮锌金属配合物的晶体结构图;
图2是本发明8-氨基喹啉席夫碱叠氮锌金属配合物的堆积结构图。
具体实施方式
本发明8-氨基喹啉席夫碱叠氮锌金属配合物的化学式为(L1)2·Zn2·(N3)2·H2O,其中的L1为8-氨基喹啉席夫碱阴离子。
下面结合具体实施实例进一步阐述本发明。
实施例1:将0.10mmol 8-氨基喹啉(14.4mg)、0.10mmol水杨醛(12.2mg)和0.10mmol三乙胺(10.1mg)均溶于30ml甲醇溶剂中,搅拌下回流2小时。冷却后,向上述溶液中缓慢加入溶有0.10mmolZn(ClO4)2.6H2O(37.2mg)、0.10mmolNaN3(6.5mg)的10ml甲醇溶液,常温搅拌7天、过滤;滤液置于50ml烧杯中,用薄膜封口,并扎小孔,自然挥发。三十天后得到灰色针状晶体,过滤,乙醚洗涤滤饼,得目标配合物。基于8-氨基喹啉计算的产率为31%。
实施例2:将0.10mmol 8-氨基喹啉(14.4mg)、0.10mmol水杨醛(12.2mg)和0.11mmol三乙胺(11.1mg)均溶于30ml乙醇溶剂中,搅拌下回流3小时。冷却后,向上述溶液中缓慢加入溶有0.10mmolZn(ClO4)2·6H2O(37.2mg)、0.12mmolNaN3(7.8mg)的10ml乙醇溶液,常温搅拌7天、过滤;滤液置于50ml烧杯中,用薄膜封口,并扎小孔,自然挥发。三十天后得到灰色针状晶体,过滤,乙醚洗涤滤饼,得目标配合物。基于8-氨基喹啉计算的产率为38%。
实施例3:将0.10mmol 8-氨基喹啉(14.4mg)、0.10mmol水杨醛(12.2mg)和0.12mmol三乙胺(12.1mg)均溶于30ml丙酮溶剂中,搅拌下回流4小时,冷却后,向上述溶液中缓慢加入溶有0.10mmolZn(ClO4)2.6H2O(37.2mg)、0.13mmolNaN3(8.5mg)的10ml丙酮溶液,常温搅拌7天、过滤;滤液置于50ml烧杯中,用薄膜封口,并扎小孔,自然挥发。三十天后得到灰色针状晶体,过滤,乙醚洗涤滤饼,得目标配合物。基于8-氨基喹啉计算的产率为36%。
实施例4:将0.10mmol 8-氨基喹啉(14.4mg)、0.10mmol水杨醛(12.2mg)和0.15mmol三乙胺(15.2mg)均溶于30ml甲醇溶剂中,搅拌下回流4小时,冷却后,向上述溶液中缓慢加入溶有0.10mmolZn(ClO4)2.6H2O(37.2mg)、0.15mmolNaN3(9.7mg)的10ml甲醇溶液,常温搅拌7天、过滤;滤液置于50ml烧杯中,用薄膜封口,并扎小孔,自然挥发。三十天后得到灰色针状晶体,过滤,乙醚洗涤滤饼,得目标配合物。基于8-氨基喹啉计算的产率为52%。
本发明8-氨基喹啉席夫碱叠氮锌金属配合物的结构测定:
晶体结构采用Bruker Smart Apex II CCD单晶衍射仪测定,以石墨单色化的Mokα射线( )为入射辐射,ω-2θ扫描方式收集室温X-射线单晶衍射数据,最小二乘法精修晶胞参数,SHELXL-97直接法解得晶体结构,全矩阵最小平方二乘法对所有非氢原子位置及各向异性热温度因子进行精修。所有的H原子位置由几何加氢方式确定。详细的晶体测定数据见表1,结构见图1和2。
表1本发明8-氨基喹啉席夫碱叠氮锌金属配合物的晶体学数据
Claims (3)
1.8-氨基喹啉席夫碱叠氮锌金属配合物单晶,其特征在于该单晶结构采用带有石墨单色器的SMART CCD area detector衍射仪,X-射线源为MoKα、以ω-2θ扫描方式收集衍射点,经过最小二乘法修正得到晶胞参数,衍射数据用SAINT程序还原处理,晶体结构解析使用SHELXL-97软件包,并用重原子法解得单晶数据:
2.一种如权利要求1所述的配合物单晶制备方法,其特征在于:以8-氨基喹啉、水杨醛、三乙胺、六水合高氯酸锌、叠氮化钠的摩尔比为1∶1∶1~1.5∶1∶1~1.5计,将8-氨基喹啉、水杨醛和三乙胺均溶于有机溶剂中,搅拌下回流2~4小时,冷却;再在上述溶液中加入溶有六水合高氯酸锌和叠氮化钠的相应的有机溶剂,常温搅拌7天,过滤,滤液自然挥发,三十天后得到灰色针状晶体;过滤,乙醚洗涤滤饼,得目标配合物。
3.如权利要求2所述的配合物单晶制备方法,其特征在于:所述的有机溶剂为甲醇、乙醇、丙酮。
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