双取代二茂铁为配体的配合物研究——Ⅲ.1,1’-双(二苯基膦)二茂铁氯化钯配合物的合成、表征、电化学性质和晶体结构  

STUDY ON BIMETALLIC COMPLEXES OF 1,1'-BISUBSTITUTED FERROCENES Ⅲ.PREPARATION,CHARACTERIZATION,ELECTROCHEMISTRY AND CRYSTAL STRUCTURE OF Pd(dppf)Cl_(2)

作　　者：席振峰 杨瑞娜 候益民 金斗满 罗保生[2] 

机构地区：[1]河南化学研究所,郑州450003 [2]武汉大学分析测试中心,武汉430072

出　　处：《无机化学学报》1991年第4期379-383,共5页Chinese Journal of Inorganic Chemistry

基　　金：国家自然科学基金资助项目

摘　　要：合成了以1,1′-双(二苯基膦)二茂铁(dppf)为双齿配体的双核配合物Pd(dppf)Cl_2,并通过红外、元素分析、热重分析.电子光谱对其进行了表征.该配合物及dppf的循环伏安研究结果给出两条可逆性较好的单电子氧化还原曲线.dppf形成配合物后,茂基氧化峰电位值显著增加.Pd(dppf)Cl_2的X-射线晶体结构表明,该配合物属单斜晶系,P2_1/n空间群.晶胞参数a=12.281(2)(?),b=16.497(2)(?).c=16.896(3)(?),β=93.6(2.6)°,Z=4,D_(?)=1.423g/cm^3.与Pd(dppe)Cl_2的晶体结构进行了比较讨论,进一步研究了配体dppf和dppe的配位性能的差别.Pd(dppf)Cl2 was prepared and characterized by means of IR spectra, electronic spectra and TG. Well-defined, one-electron reversible rcdox waves were observed on cyclic voltammetry for the oxidation of dppf and the complex. Upon complexation to Pd, the Ep,a of fcrroccnyl group increased considerably. The crystal structure determined by the single crystal X-ray diffraction shows that the crystal is monoclinic with four formula units in a cell of dimensions: a= 12.281(2) A, b= 16.497(2) A, c= 16.896(3) A, β = 93.6(2.6)° ; space group P21 / n, De= 1.423g/ cm3. Discussions compared with the crystal structure of Pd(dppe)Cl2cnablc further study on the differences of coordination ability of ligands dppf and dppe.

关 键 词：二氯-1 1’-二(二苯基膦)二茂铁合钯(Ⅱ) 双取代二茂铁 双核配合物 双齿膦配体 合成 结构 循环伏安 

分 类 号：O614.823[理学—无机化学]