Reaction of CpRu(PPh 3 ) 2 Cl with six-member cyclothioethers. Structures of the [CpRu(PPh 3 ) x L]Y complexes (L = pentamethylene sulfide, x = 2, Y = BF 4 − ; L = 1,3-dithiane; 1,3,5-trithiane, x = 2, Y = CF 3 SO 3 − ; L = 1,4-dithiane, x = 1, Y = BF 4 − )
作者： Mark Green , M. Draganjac , Yanjing Jiang , Paul M. Nave , A.W. Cordes
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摘要: The synthesis of a series ruthenium complexes with cyclothioether ligands is reported. compounds were characterized by X-ray diffraction techniques. molecular structures [CpRu(PPh3)2(pms)]BF4 (1), [CpRu(PPh3)2(1,3-dithiane)]OTfl (2), [CpRu(PPh3)2(1,3,5-trithiane)]OTfl (3), and [CpRu(PPh3)(1,4-dithiane)]BF4 (4) show chelation occurs only when the sulfur atoms are separated at least two C atoms, creating ligand bite size large enough to chelate. Cell parameters: 1, space group P21/c, = 14.601(4), b 19.102(10), c 14.751(7) A, β 98.28(3)○; 2, 12.859(7), 15.576(3), 22.126(11) 102.22(4)○; 3, 12.7320(20), 15.571(5), 22.287(4) 101.812(14)○; 4, Pbca, 11.2010(10), 16.321(7), 28.966(4) A. Compounds 2 3 isomorphous. Ru–S bond lengths range from 2.341(3), 2.365(3) A in compound 4 2.382(4) 2. Upon (compound 4), subsequent loss PPh3, Ru–P shortens 2.327(3) This may be due reduced steric hindrance about Ru atom. No evidence for C–S lengthening observed.
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