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本文报道Co-Ru簇的合成与表征的研究.由Et_4N[RuCl_4(CH_3CN)_2]和Co_2(CO)_8制备了Et_4N[Co_3Ru(CO)_(12)]·1/3THF,它与等摩尔的NOBF_4反应得到Co_3Ru(CO)_(11)(NO)(1)和Co_2Ru(CO)_(11)(5).簇合物1分别与乙炔、苯基乙炔和二苯基乙炔进一步反应得到(HC≡CH)Co_3Ru(CO)_9(NO)(2),(PhC≡CH)Co_3Ru(CO)_9(NO)(3)和(PhC≡CPh)Co_3Ru(CO)_9(NO)(4).在上述反应中还分离得到(HC≡CH)Co_2Ru(CO)_96),(PhC≡CH)Co_2Ru(CO)_9(7)和(PhC≡CPh)Co_2Ru(CO)_9(8).对所得族合物1,2,3,4进行了IR,UV,~1H NMR,m.p.,元素分析和单晶X射线衍射分析等性质表征.簇合物3的晶体属单斜晶系,Pa_1/n空间群,晶胞参数为:a=1.1438(9),b=1.3033(6),c=1.4345(9)nm.β=100.72(4)°.每个晶胞中有四个分子.
In this paper, the synthesis and characterization of Co-Ru clusters are reported. Et_4N [Co_3Ru (CO) _ (12)] · 1 / 3THF was prepared from Et_4N [RuCl_4 (CH_3CN) _2] and Co_2 (CO) _8, (CO) _ (11) (NO) (1) and Co_2Ru (CO) _ (11) (5) were obtained by the reaction of NOBF_4 with cluster reactor 1. The further reaction of cluster 1 with acetylene, phenylacetylene and diphenylacetylene gave (CO) _9 (NO) (2), (PhC≡CH) Co_3Ru (CO) _9 (NO) (3) and (PhC≡CPh) Co_3Ru (CO) _9 (NO) (HC≡CH) Co_2Ru (CO) _96), (PhC≡CH) Co_2Ru (CO) _9 (7) and (PhC≡CPh) Co_2Ru (CO) The complexes 1, 2, 3 and 4 were characterized by IR, UV, 1H NMR, elemental analysis and single crystal X-ray diffraction analysis.The crystal of cluster 3 was monoclinic, Pa_1 / n Space group with unit cell parameters of a = 1.1438 (9), b = 1.3033 (6), c = 1.4345 (9) nm.β = 100.72 (4) °. There are four molecules in each unit cell.