高等学校化学学报

高等学校化学学报 ›› 2013, Vol. 34 ›› Issue (1): 30.doi: 10.7503/cjcu20120736

• 研究论文: 无机化学 • 上一篇    下一篇

含O,O'-二(对甲苯基)二硫代磷酸的双核铅配合物的晶体结构、谱学性质和抑菌活性

谢斌1, 王艳美2, 蔡述兰1, 何林芯1, 朱莎莎2, 王军1, 林肖2, 李玉龙1, 邹立科1   

  1. 1. 四川理工学院功能材料研究所, 绿色催化四川省高校重点实验室,;
    2. 材料与化学工程学院, 自贡 643000
  • 收稿日期:2012-08-10 发布日期:2012-12-31
  • 通讯作者: 谢斌,男,教授,主要从事有机合成、金属有机化学和配位化学研究.E-mail:xiebinqhg@sina.com.cn E-mail:xiebinqhg@sina.com.cn
  • 基金资助:

    绿色催化四川省高校重点实验室开放基金(批准号: LZJ1103); 四川省自贡市科技局项目(批准号: 2011G008)和四川理工学院研究生创新基金(批准号: y2011015, y2011019)资助.

Crystal Structure, Spectroscopic Properties and Antibacterial Activity of Binuclear Lead Complex with O, O'-Di(p-methylphenyl)dithiophosphate

WANG Yan-Mei1, CAI Shu-Lan2, HE Lin-Xin1, ZHU Sha-Sha1, WANG Jun2, LIN Xiao1, LI Yu-Long2, ZOU Li-Ke1   

  1. 1. Institute of Functional Materials, University Key Laboratory of Green Chemistry of Sichuan Institutes of Higher Education,;
    2. College of Materials & Chemical Engineering, Sichuan University of Science & Engineering, Zigong 643000, China
  • Received:2012-08-10 Published:2012-12-31

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摘要：

合成了双核铅配合物{Pb2[S2P(OC6H4Me-p)2]2 [μ-S2P(OC6H4Me-p)2]2}, 并用元素分析、 红外光谱、 紫外-可见光谱、 热重分析和X射线衍射对其进行了结构表征. 结果表明, 该晶体属于三斜晶系, P1空间群, 晶胞参数a=1.06393(6) nm, b=1.15005(6) nm, c=1.45006(5) nm, α=94.109(3)°, β=98.833(4)°, γ=109.242(5)°, V=1.64099(14) nm3, Dc=1.671 Mg·m-3, Z=1, F(000)=808, μ(Mo Kα)=5.523 mm-1, S=1.024, R1=0.0596, wR2=0.1464[I>2σ(I)]. 该配合物形成了具有椅式构型的八元环[Pb2S4P2], 每个Pb原子与1个螯合双齿配体(p-MeC6H4O)2PS2-的2个S原子和2个桥三齿配体μ-(p-MeC6H4O)2PS2-的3个S原子配位, Pb1—S的键长在0.2750~0.3257 nm范围内. 芳环对Pb原子有弱的π配位作用[Pb1…Cgi为0.3365(2) nm]. Pb原子处于Pb(S5ArE)(E代表孤对电子) 的畸变缺位五角双锥(Ψ-PB)环境中, 1个S原子和1个芳环位于Ψ-PB的轴向位置[键角S1—Pb1—Cgi为173.79(5)°], 4个S原子和Pb原子的一对立体化学活性的孤对电子占据Ψ-PB的赤道位置. 配合物热稳定性高, 在287.1℃开始分解. 与原料(p-MeC6H4O)2PS2NH2Et2比较, 配合物对葡萄球菌(Staphylococcus)、 大肠杆菌(E. Coli)和枯草杆菌(B. Subtilis)具有更好的抑菌活性.

关键词: O, O'-二烃基二硫代磷酸盐, 铅配合物, 晶体结构, 谱学性质, 抑菌活性

Abstract:

A new binuclear lead complex Pb2[S2P(OC6H4Me-p)2]2[μ-S2P(OC6H4Me-p)2]2 was synthesized and characterized, the antibacterial activities of the raw material (p-MeC6H4O)2PS2NH2Et2 and the complex were studied. The complex crystallized in triclinic, P1 space group with the cell parameters: a=1.06393(6) nm, b=1.15005(6) nm, c=1.45006(5) nm, α=94.109(3)°, β=98.833(4)°, γ=109.242(5)°, V=1.64099(14) nm3, Dc=1.671 Mg/m3, Z=1, F(000)=808, μ(Mo Kα)=5.523 mm-1, S=1.024, R1=0.0596, wR2=0.1464[I > 2σ(I)]. The crystal structure study shows that the complex contains two chelating anisobidentate and two bridging tridentate (p-MeC6H4O)2PS2- ligands. Each lead atom is in a distorted ψ-pentagonal bipyramidal geometry by five sulfur atoms from three (p-MeC6H4O)2PS2- ligands, an aryl group of one of bridging (p-MeC6H4O)2PS2- ligand, and a lone pair of stereochemically active electron originating from the lead atom, in which four sulfur atoms and a lone electron pair of lead locate in the equatorial positions, and a sulfur and an aryl group in the axial positions[the Pb1—S bond lengths rang from 0.2750 to 0.3257 nm, the distance of Pb1…Cgi is 0.3365(2) nm, and the S1—Pb1—Cgi angle is 173.79(5)°]. The two bridging (p-MeC6H4O)2PS2- ligands each bridges two lead atoms to form an chair conformation of eight-membered ring [Pb2S4P2]. The complex is stable up to over 281.7℃. The bioactivity test shows that both the raw material and complex can inhibit Staphylococcus, E. Coli, and B. Subtilis and the complex exhibited the higher antibacterial activity compared with the raw material.

Key words: O,O'-Dialkyldithiophosphate, Pb complex, Crystal structure, Spectroscopic property, Antibacterial activity

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