Synthesis and characterization of new RuCoM (M = Co, Mo) mixed-metal linked tetrahedral clusters containing (−)-DIOP and reaction of [(μ 3-Se)RuCo 2(CO) 8] 2((−)-DIOP) with Na[Mo(CO) 3(η 5-C 5H 4COCH 3)]

• Published in: Polyhedron 2005-10, Vol.24 (15), p.2055-2061
• Main Authors: Zhu, Bao-Hua, Hu, Bin, Yin, Yuan-Qi, Sun, Jie
• Format: Article
• Language: English
• Subjects: (−)-DIOP; Crystal structure; Mixed-metal cluster; Ru and Co
• ISSN: 0277-5387
• DOI: 10.1016/j.poly.2005.06.008

Four mixed-metal Ru–Co linked tetrahedral clusters have been synthesized from reactions of diphosphine compound (−)-DIOP with [(μ 3-E)RuCo 2(CO) 9] and [(μ 3-E)RuCoMo(CO) 8(CpC(O)CH 3)] in n-hexane or THF at r.t., respectively. The metallic exchange reaction of [(μ 3-Se)RuCo 2(CO) 8] 2((−)-DIOP) with Na[Mo(CO) 3(η 5-C 5H 4COCH 3)] has also been investigated. The reactions of diphosphine compound (−)-DIOP [(2,2-dimethyl-1,3-dioxolane-4,5-diylbis-methylene)bisdiphenylphosphine] with [(μ 3-E)RuCo 2(CO) 9] (E = Se, S) and [(μ 3-E)RuCoMo(CO) 8(CpC(O)CH 3)] (E = Se, S) in n-hexane and THF at r.t. afford four mixed-metal linked tetrahedral clusters [(μ 3-E)RuCo 2(CO) 8] 2((−)-DIOP) (E = Se, 1; S, 2) and [(μ 3-E)RuCoMo(CO) 7(CpC(O)CH 3)] 2((−)-DIOP) (E = Se, 3; S, 4), respectively. The treatment of 1 with Na[Mo(CO) 3(η 5-C 5H 4COCH 3)] in THF at 60 °C produces a known cluster (μ 3-Se)RuCoMo(CO) 8(CpC(O)CH 3) and a new (−)-DIOP substituted tetrahedral cluster [(μ 3-Se)RuCoMo(CO) 6(CpC(O)CH 3)((−)-DIOP)] ( 5). The structure of cluster 1 has been determined by single-crystal X-ray diffraction. All clusters were characterized by C, H elemental analysis, IR and 1H NMR spectroscopy. The clusters 1, 2, 4, 5 also were characterized by 31P NMR spectroscopy.