双二茂铁甲氨基异丙醇的合成与晶体结构

双二茂铁甲醇与BF3在CH2Cl2中与BF3作用形成的双二茂铁甲基碳正离子, 无需从溶液中分离出来, 便可直接与异丙醇胺反应得到双二茂铁甲氨基异丙醇,且产率较高。由乙醇重结晶得到的单晶经X射线衍射法测试表明, 该化合物晶体属三斜晶系, P空间群, 化学式为2C24H27Fe2NO]CH3CH2OH, Mr = 960.40。晶胞参数: a = 10.6825(7), b = 14.463(1), c = 15.794(1) , ?= 69.593(1), b = 75.535(1), g = 81.302(1)? V = 2208.9(3) 3, Z = 2, Dc = 1.444 g/cm3, m(MoKa) = 1.332 mm-1, F(000) = 1004, 对于I > 2(I)的4742个衍射点, 最终的R = 0.0525、wR = 0.0704。晶体结构由2分子双二茂铁甲氨基异丙醇和1分子乙醇通过氢键缔合组成。

Synthesis and Structure Characterization of Diferrocenylmethylaminoisopropanols

The reaction of diferrocenylmethanol with the ethereal solution of boron trifluoride resulted in the formation of -diferrocenylmethyl carbocation in dichloride methane. Without separation from the reaction mixture, the reaction of the ion and isopropanolamine synthesizes the diferrocenylmethylaminoisopropanol directly. The single crystals of diferrocenylmethylaminoisopropanol were gained through the recrystallization of ethanol. The crystal and molecular structures of the compound were determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 10.6825(7), b = 14.4629(1), c = 15.7935(1) ? = 69.593(1), = 75.535(10), = 81.3020(10)? 2C24H27Fe2NO]CH3CH2OH, Mr = 960.40, Z = 2, V = 2208.9(3) ?, Dc = 1.444 g/cm3, (MoK? = 1.332mm-1 and F(000) = 1004. For 4742 observed reflections with I > 2(I), the final R = 0.0525 and Rw = 0.0704, indicating the crystal structure is composed of two diferrocenylmethylaminoisopropanol molecules and one ethanol molecule united through hydrogen bonds.