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化学学报
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化学学报 ›› 1988, Vol. 46 ›› Issue (10): 984-990. 上一篇    下一篇

研究论文

双三苯膦铁硫原子簇配合物(μ-i-C3H7S)(μ-PhCH2S)-Fe2(CO)4(PPh3)2的合成及晶体结构

宋礼成;胡青眉;王如骥;王宏根   

  1. 南开大学化学系;南开大学测试计算中心
  • 发布日期:1988-10-15

Synthesis and crystal structure of bis-PPh3-substituted Fe-S cluster complex (μ-i-C3H7S)-(μ-PhCh2S)Fe2 (CO)4(PPh3)2

SONG LICHENG;HU QINGMEI;WANG RUJI;WANG HONGGEN   

  • Published:1988-10-15

PDF

471

被引次数

9

通过(μ-i-C3H7S)(μ-PhCH2S)Fe2(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-C3H7S)(μ-PhCH2S)Fe2(CO)4(PPh3)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)埃; a=94.73(1)°, β=102.98(2)°, γ=89.93(1)°;V=4610.5埃^3, Z=4, Dc=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, Rw=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6键与硫相连.

关键词: 晶体结构, 铁络合物, 羰基络合物, 三苯基膦, 簇状化合物, 硫络合物

Reaction of (m-Me2CHS)(m-PhCH2S)Fe2(CO)6 with excess PPh3 in boiling toluene for 6 h gave (m-Me2CHS)(m-PhCH2S)Fe2(CO)4(PPh3)2 (I). The crystal of I is triclinic, P1, with a 10.268(4), b 20.289(1), c 22.799(5) ? a 94.73(1), b 102.98(2), g 89.93(1)? Z = 4, R = 0.059 and Rw = 0.068. The cluster core of I consists of 2 Fe and 2 S atoms and has a butterfly structure. Two PPh3 ligands bonded to 2 Fe atoms are at the positions trans to Fe-Fe bent bond; Me2CH and PhCH2 groups are attached to different S atoms by equatorial bonds.

Key words: CRYSTAL STRUCTURE, IRON COMPLEX, CARBONYL COMPLEX, TRIPHENYLPHOSPHINE, CLUSTER COMPOUND, SULFIDE COMPLEX

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