Binuclear ruthenium η~6-arene complexes with tetradentate N,S-ligands containing the orthoaminothiophenol motif

Alberto Acosta-Ramirez; Edward D. Cross; Robert McDonaldMatthias Bierenstiel

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Binuclear ruthenium η~6-arene complexes with tetradentate N,S-ligands containing the orthoaminothiophenol motif

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A series of cationic binuclear (η~6-cymene-Ru)_2 complexes with N_2S_2-ligands were synthesized in 64 to 85 yield by reaction of Ru(η~6-cymene)Cl_2_2 with bis-S,S'-(ortho-aminothiophenol)-xylenes as BF_4~? and PF_6~? salts. The compounds were studied using NMR, HRMS, UV-vis and IR spectroscopy, EA and inductively coupled plasma (ICP) MS. It was determined that the hinged binuclear Ru complexes were anti and syn diastereomers obtained in 2: 1 ratio for ortho- and meta-xylylene bridged ligands and in a 1: 1 ratio for the para-xylylene bridged ligand. An anion effect was found for the presence of NaBF4 with the meta-xylylene bridged system yielding the targeted binuclear Ru complex and a mononuclear Ru complex. This mononuclear S,S'-coordinated η~6-cymene Ru chloride structure lacked amine-metal coordination and was obtained in a 1: 3 ratio of anti: syn diastereomers which were insoluble in CH_2Cl_2 and soluble in DMSO and DMF. X-ray crystallographic analysis was obtained for the N_2S_2 ligand, 1,2-bis{(2-aminophenyl)thiomethyl} benzene, showing a C_S symmetry with amine groups facing outwards with a tilt of 28.95° from the ortho-aminothiophenol pendant ring. The interatomic sulfur-sulfur distance (S-S') is 4.6405 ? within the crystal structure while accommodating a potential metal bite angle from 1.0 ? to 5.9 ? when allowing rotation of the methylene phenyl bond.

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《Dalton transactions: An international journal of inorganic chemistry》 |2014年第8期|3104-3113|共10页
作者
Alberto Acosta-Ramirez; Edward D. Cross; Robert McDonaldMatthias Bierenstiel;
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作者单位

X-Ray Crystallography Laboratory, Department of Chemistry, University of Alberta, Edmonton, Alberta T6G 2G2, Canada;

Cape Breton University, Department of Chemistry, 1250 Grand Lake Road, Sydney, Nova Scotia B1P 6L2, Canada;

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正文语种英语
中图分类化学;无机化学;
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Binuclear; ruthenium; motif;

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Binuclear ruthenium η~6-arene complexes with tetradentate N,S-ligands containing the orthoaminothiophenol motif

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