Synthesis and Crystal Structure of an Azide Bridged Binuclear Zinc(II) Complex Including the Reduced Derivative of Nitronyl Nitroxide, [Zn(Him2Py)(N_3)_2]_2

The title compound [Zn(Him2Py)(N3)2]2 (Zn2C26H38N18O2, Mr = 765.48) has been prepared and structurally characterized by X-ray diffraction methods. It crystallizes in monoclinic, space group P21/n with a = 10.989(3), b = 11.519(3), c = 13.812(4) ? b = 101.700(5), V = 1711.9(9) ?, Z = 2, Dc = 1.485 g/cm3, m(MoKa) = 1.456 mm～1, F(000) = 792, the final R = 0.0401 and wR = 0.0861 for 2054 observed reflections with I>2s(I). The imino nitroxide 2-(3- methyl-2-pyridyl)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazolyl-1-oxyl (im2Py) was reduced to obtain 2-(3-methyl -2-pyridyl)-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazole-1-ydroxy (Him2Py) coordinating to the zinc (II) ion, around which the coordination geometry is a square-based pyramid with a terminal nitrogen atom located at the apical position. The four basal sites are occupied by two m1,1 nitrogen atoms from two different bridging azide ions and two nitrogen atoms from Him2Py. The units of [Zn(Him2Py)(N3)2]2 were connected as two dimension planes by intermolecular hydrogen bonds.

假木豆中一新偶氮化合物

为了研究假木豆的化学成分,采用硅胶、大孔树脂柱色谱和重结晶的方法对乙醇提取物进行分离纯化,通过理化性质和波谱技术鉴定化合物结构。分离鉴定了13个化合物,分别是偶氮-2,2′-双[Z-(2,3-二羟基-4-甲基-5-甲氧基)苯基乙烯](1)、β-谷甾醇(2)、N-(2′-羟基-二十四酰基)-2-氨基-1,3,4-三羟基-十八-8E-烯(3)、羽扇豆醇(4)、环桉烯醇(5)、胡萝卜苷(6)、白桦脂酸(7)、白桦脂醇(8)、二十六烷酸甘油酯(9)、26-羟基-二十六烷酸甘油酯(10)、脱镁叶绿素甲酯(11)、金合欢素-7-O-α-L-鼠李糖基(1→6)-β-D-葡萄糖苷(12)和刺槐苷(13),其中化合物1为新化合物。所有化合物均是首次从该属植物中分离得到。经活性筛选研究发现,与维生素E(VE)相比较,在2μg·mL-1浓度下,化合物1具有较好的谷氨酸诱导PC12细胞的损伤保护活性。