Triosmium carbonyl complexes with multiple 1,3,5-triaza-7-phosphaadamantane (PTA) ligands: Synthesis of a new water-soluble Os3 cluster

Autor: Joel L. Jackson, David M. Marolf, Nigel Gwini, Amanda C. Dugan, Brittney S.N. Nolan, Vladimir N. Nesterov, Kristen L. Brehm, Kayla N. Green, Hannah M. Johnston, Gregory L. Powell, James E. Johnstone, Soo Hun Yoon, Sarah D. Floris
Rok vydání: 2016
Předmět:
Zdroj: Polyhedron. 114:292-298
ISSN: 0277-5387
DOI: 10.1016/j.poly.2015.12.036
Popis: Microwave heating has been used to substitute carbonyl ligands for 1,3,5-triaza-7-phosphaadamantane (PTA) ligands on the Os3(CO)12 molecule. Os3(CO)11(PTA) (1) has been prepared in 66% yield by the reaction of Os3(CO)12 with MeCN, followed by reaction with one mole equivalent of PTA. Os3(CO)10(PTA)2 (2) has been prepared in 65% yield via a three-step reaction. First, Os3(CO)12 was heated in MeCN. Next, one mole equivalent of PTA was added to this reaction mixture. Finally, one mole equivalent of trimethylamine-N-oxide was added followed by another mole equivalent of PTA. Additionally, Os3(CO)9(PTA)3 (3) has been prepared in 85% yield by the reaction of Os3(CO)12 with 3.5 mol equivalents of PTA in 1,2-dichlorobenzene, and Os3(CO)8(PTA)4 (4) has been prepared in 36% yield by the reaction of Os3(CO)12 with 8 mol equivalents of PTA in a mixture of acetonitrile and 1,2-dichlorobenzene. The solubilities of clusters 1–4 in water at various pH levels have been studied, and 4 was found to be soluble in water with a neutral pH. X-ray diffraction has been used to determine the crystal structures of clusters 1 and 3. The X-ray crystal structure of a protonated form of 3, [Os3(CO)9(PTAH)3]Cl3 (5), has also been determined. All PTA ligands occupy equatorial coordination sites on the triangular Os3 units.
Databáze: OpenAIRE
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