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通过(μ-i-C_3H_7S)(μ-PhCH_2S)Fe_2(CO)_6和三苯膦在甲苯中回流反应6h,制得了三苯膦双取代配合物(μ-i-C_3H_7S)(μ-PhCH_2S)Fe_2(CO)_4(PPh_3)_2(1),并用 X 射线衍射技术测得其单晶结构.晶体属三斜晶系,空间群为 PI.晶胞参数:a=10.268(4),b=20.289(1),c=22.799(5)■α=94.73(1)°,β=102.98(2)°,γ=89.93(1)°;V=4610.5(?)~3,Z=4,D_o=1.36g/cm~3.晶体结构用直接法(MULTAN 82)测定,采用块矩阵最小二乘法进行最终结构精化,最后偏离因子 R=0.059,R_w=0.068.单晶 X 射线分析表明,配合物1的簇核是由两个铁原子和两个硫原子组成的蝴蝶式结构;两个三苯膦配体处于铁—铁弯键的反位;异丙基和苄基分别以 e 键与硫相连.
(Μ-i-C_3H_7S) (μ-PhCH_2S) was prepared by the reaction of μ-i-C_3H_7S (μ-PhCH_2S) Fe_2 (CO) _6 with triphenylphosphine in toluene for 6h. Its crystal structure belongs to triclinic system and the space group is PI. Cell parameters: a = 10.268 (4), b = Α = 94.73 (1) °, β = 102.98 (2) °, γ = 89.93 (1) °; V = 4610.5 (?) To 3, Z = 4, D_o = 1.36g / cm ~ 3. The crystal structure was determined by the direct method (MULTAN 82), the final structure was refined by the least square method of block matrix, the final deviation factor R = 0.059, R_w = 0.068. Single crystal X-ray analysis showed that the coordination The cluster core of object 1 is a butterfly structure consisting of two iron atoms and two sulfur atoms; two triphenylphosphine ligands are in the opposite position of the iron-iron bend bond; the isopropyl and benzyl groups are respectively linked by e and Sulfur connected.