含羰基钌配合物Ru(CO)_2[S_2P(O-i-C_3H_7)_2]_2的合成与晶体结构  

Synthesis and Crystal Structure of Ruthenium Complex Containing Carbonyl Ru(CO)_2[S_2P(O-i-C_3H_7)_2]_2

作　　者：于富强[1] 刘树堂[1] 吴秉芳[1] 金祥林[2] 

机构地区：[1]内蒙古大学化学化工学院,呼和浩特010021 [2]北京大学化学与分子工程学院,北京100871

出　　处：《内蒙古大学学报（自然科学版）》2004年第2期168-171,共4页Journal of Inner Mongolia University：Natural Science Edition

基　　金：国家自然科学基金资助项目(29861001)

摘　　要：用Ru3(CO)12和双(硫代磷酸二异丙基酯)二硫化物(C3H7-i-O)2P(S)-S-S-P(S)(O-i-C3H7)2反应得到一个新的含羰基钌配位化合物Ru(CO)2[S2P(O-i-C3H7)2]2,对其进行了元素分析和IR(υco)、1HNMR、31PNMR及MS谱学表征,并测定了分子的晶体结构,属于单斜晶系,C2/c空间群,晶胞参数:a=2.4608(1)nm,b=0.91372(6)nm,c=1.21461(5)nm,α=90°,β=109.609°,γ=90°,Z=4,V=2.5726(2)nm3,Dc=1.509g/cm-3,μ=1.082mm-1,F(000)=1192,(Δρ)max=377e·nm-3,(Δρ)mix=-602e·nm-3,R=0.0269,wR2=0.0522.晶体结构分析表明,该配合物的分子骨架RuS4C2近似为八面体结构,由两个螯合配体S2P(O-i-C3H7)2提供的4个硫原子和2个端羰基CO配体与中心原子钌成键,分子内含有两个等价的平面四元环RuSPS组件.A new ruthenium carbonyl complex Ru(CO)_2[S_2P(O-i-C_3H_7)_2]_2 was synthesized by reaction of Ru_3(CO)_(12) with (C_3H_7-i-O)_2P(S)-S-S-P(S)(O-i-C_3H_7)_2.This complex was characterized by elementary analysis,IR(υ_(co)),~1H NMR,^(31)P NMR and MS spectroscopy,and its crystal structure was determined by X-ray single crystal diffraction method.The crystal belongs to monoclinic,space group C 2/c,with crystal parameters as follows:a=2.4608(1) nm,b=0.91372(6) nm,c=1.21461(5) nm,α=90°,β=109.609°,γ=90°,Z=4,V=2.5726(2) nm^3,Dc=1.509 g/cm^(-3),μ=1.082 mm^(-1),F(000)=1192, (Δρ)_(max)=377 e·nm^(-3),(Δρ)_(mix)=-602 e·nm^(-3),R=0.0269,(wR_2=0.0522).The structural analysis shows that the molecular framework,Ru S_4C_2,is approximately octahedral,where the four sulfur atoms from two chelate ligands(C_3H_7-i-O)_2PS_2 and two carbonyls as terminal ligands link with a ruthenium atom.The molecular contains two equivalent four member plane rings of RuSPS.

关 键 词：羰基钌配合物 合成 晶体结构 

分 类 号：O641.812[理学—物理化学]