间硝基苯甲酸/8-羟基喹啉(1/1)共晶体结构解析与Rietveld精修  

Structure analysis and Rietveld refinement of a cocrystal of m-nitrobenzoic acid/8-hydroxyquinoline (1/1)

作　　者：居威材 陶亚秋[1] 沈晓冬[1] 潘志刚[1] 

机构地区：[1]南京工业大学材料科学与工程学院,江苏南京210009

出　　处：《南京工业大学学报（自然科学版）》2017年第3期126-131,共6页Journal of Nanjing Tech University(Natural Science Edition)

基　　金：长江学者和创新团队发展计划(IRT1146);江苏高校优势学科建设工程

摘　　要：通过溶液冷却结晶法制备出间硝基苯甲酸/8-羟基喹啉(1/1)共晶体。利用粉末X线衍射技术及傅里叶红外光谱技术采集该共晶体的粉末衍射数据及红外光谱数据。对该共晶体粉末衍射数据进行指标化及晶体结构解析,并参照红外分析结果对该共晶体的晶体结构进行了Rietveld精修,最终测定了间硝基苯甲酸/8-羟基喹啉(1/1)共晶体的晶体结构。该共晶体的一个不对称单元中包含一个间硝基苯甲酸分子(去质子化的)和一个8-羟基喹啉分子(质子化的)。8-羟基喹啉上的酚羟基和芳香N原子与间硝基苯甲酸上的羧基通过O—H…O氢键、N—H…O氢键形成二聚体,沿b轴方向相互平行的二聚体之间存在着π…π堆砌作用。An organic cocrystal of m-nitrobenzoic acid/8-hydroxyquinoline( 1/1) was obtained through crystallization. Powder X-ray diffraction data and infrared spectroscopy data were collected and the indexing and crystallographic structural analyses of the cocrystal were carried out followed by Rietveld refinement. Proton transfer from m-nitrobenzoic acid to 8-hydroxyquinoline was revealed via fourier transform infrared spectroscopy. The asymmetric unit of the crystal structure had one deprotonated mnitrobenzoic acid and one protonized 8-hydroxyquinoline.The phenol group and the aromatic N atom in 8-hydroxyquinoline were involved in hydrogen bonding with carboxylic group in m-nitrobenzoic acid,resulting in a dimmer of m-nitrobenzoic acid/8-hydroxyquinoline.The π…π stacking interactions between the dimmers along the b-axis were observed. The hydrogen bonding and π…π stacking interactions were analyzed and their role in crystal packing was investigated.

关 键 词：共晶体 粉末X线衍射 RIETVELD精修 质子转移 氢键 

分 类 号：O722.4[理学—晶体学] O723.1