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通过(μ-cy-C_6H_(11)S)(μ-n-C_5H_(11)S)Fe_2(CO)_6同PPh_3在苯中,80℃下反应5小时,制得了三苯膦单取代产物(μ-cy-C_6H_(11)S)(μ-n-C_5H_(11)S)Fe_2(CO)_5PPh_3(1),并用X衍射技术测得其单晶结构.晶体属正交晶系,空间群为.Pbca,α=12.940(2)A,b=23.170(7)A,c=23.294(2)A,D_=1.25g·cm~(-3) Z=8.采用直接法(RANTAN)测得其初结构,以SHELX-76程序经全矩阵最小二乘法分块修正,最后偏离因子R=0.043,R_w=0.058.单晶X射线分析表明,三苯膦取代反应发生在配合物Fe—Fe键的反位上;两个硫桥以不等性方式同两个铁原子相连;硫桥上的取代基cy-C_6H_(11)及n-C_5H_(11)同处于e,e键,且弯向Fe_2原子一边.重要的键长有Fe(1)—Fe(2)=2.527(1)A,Fe(1)—S=2.287(1)及2.281(1)A,Fe(1)—p=2.271(1)A,Fe(2)—S=2.267(1)及2.275(1)A.五个Fe—C键长在1.757(7)～1.810(6)A范围内。
The reaction of triphenyl phosphine with a single reaction of (μ-cy-C_6H_ (11) S) (μ-n-C_5H_ (11) S) Fe_2 (CO) _6 with PPh_3 in benzene at 80 ℃ for 5 hours The crystal structure of the crystal belongs to the orthorhombic system with space group (μ-n-C_5H_ (11) S) Fe_2 (CO) _5PPh_3 (1) (2) A, b = 23.170 (7) A, c = 23.294 (2) A, D_ = 1.25g · cm -3 Z = 8. Using RANTAN The initial structure of SHELX-76 program was corrected by the full matrix least square method, the final deviation factor R = 0.043, R_w = 0.058. Single crystal X-ray analysis showed that the triphenylphosphine substitution reaction occurred in the complex Fe-Fe The two sulfur bridges are connected with two iron atoms in an unequal manner. The substituents cy-C_6H_ (11) and n-C_5H_ (11) on the sulfur bridge are located at the e and e bonds, Fe (1) -Fe (2) = 2.527 (1) A, Fe (1) -S = 2.287 (1) and 2.281 (1) A, Fe = 2.271 (1) A, Fe (2) -S = 2.267 (1) and 2.275 (1) A. The five Fe-C bonds are in the 1.757 (7) ~1.810 (6) A range.