Synthesis and Structural Characterization of the Ruthenium Complexes Based on ortho-Carborane-1,2-diselenolate Ligand and Terminal Alkynone

• Published in: Russian journal of inorganic chemistry Vol. 67; no. 11; pp. 1739 - 1744
• Main Authors: Hu, J. R., Wang, J. H.
• Format: Journal Article
• Language: English
• Published: Moscow Pleiades Publishing 01.11.2022; Springer Nature B.V
• Subjects: Argon; Butyllithium; Carborane; Chemical analysis; Chemistry; Chemistry and Materials Science; Coordination Compounds; Infrared spectroscopy; Inorganic Chemistry; NMR spectroscopy; Ruthenium compounds; Selenium; Structural analysis; Toluene; chalcogenide element; synthesis; carborane; terminal alkynone; ruthenium complexes
• ISSN: 0036-0236; 1531-8613
• DOI: 10.1134/S0036023622600654

One-pot reaction of ortho -carborane, n -butyl lithium, selenium, and [( p -cymene)RuCl 2 ] 2 under argon leads to 16-electron complex ( p -cymene)Ru(Se 2 C 2 B 10 H 10 ) ( 1 ), and [( p -cymene)RuCl 2 ] 2 reacts with Li 2 (Se 2 C 2 B 10 H 10 ) in the presence of excess sulfur to generate dinuclear complex ( p -cymene)Ru(µ-S 2 )Ru(Se 2 C 2 B 10 H 10 ) 2 ( 2 ). Treatment of 1 and 2 with HC≡CCOCH 3 affords addition complexes ( p -cymene)Ru(Se 2 C 2 B 10 H 10 )(HC=C−COCH 3 ) ( 3 ) and ( p -cymene)Ru(µ-S 2 )Ru(Se 2 C 2 B 10 H 10 ) 2 (R 1 C=CR 2 ) (R 1 = H, R 2 = COCH 3 ( 4 ); R 1 = COCH 3 , R 2 = H ( 5 )), respectively. In boiling toluene, 4 and 5 could be interconverted. These complexes were characterized by elemental analysis, mass, IR and NMR spectroscopy. X-ray structural analyses was performed on 3 . Complex 3 crystallizes in monoclinic system, space group P 2 1 / n with a = 11.522(4) Å, b = 10.564(4) Å, c = 20.048(7) Å, α = 90°, β = 92.750(5)°, γ = 90°, C 16 H 28 B 10 ORuSe 2 , FW = 603.47, V = 2437.5(15) Å 3 , Dc = 1.644 g/cm 3 , Z = 4, F (000) = 1176, µ(Mo K α ) = 3.636 mm –1 , R = 0.0434 and ω R = 0.1020 for 3847 observed reflections ( I > 2σ( I )).