| 12184743 |
Grapperhaus CA, Poturovic S, Mashuta MS: Dichloromethane alkylates a trithiolato-ruthenium complex to yield a methylene-bridged thioether core. Inorg Chem. 2002 Aug 26;41(17):4309-11.
Synthesis and structural comparison to the thiolato-ruthenium precursor.. The previously reported triphosphino/trithiolato-ruthenium anion, [tris-(2-diphenylphosphinothia-phenolato) ruthenium (II)](-), [Ru (DPPBT)(3)](-), has been isolated as the PPN salt (PPN = bis (triphenylphosphoranylidene) ammonium), 1, from chlorobenzene/ether as light-orange crystalline plates, and the X-ray crystal structure has been determined. In dichloromethane, the cis positioned thiolates are alkylated by solvent yielding the methylene-bridged triphosphino/dithioether/thiolato complex [(bis-(2-diphenylphosphinothiaphenolato) methane)(2-diphenyl-phosphinothiap henolato) ruthenium (II)] chloride, [Ru ((DPPBT)(2) CH (2))(DPPBT)] Cl (2). Dichloromethane solutions of 1 layered with hexanes yield 2 as orange cubes. The ruthenium-sulfur bond distances in the alkylated, thioether product are slightly shorter than in the thiolate precursor. Within 2, the iron-thioether bond distances are comparable to the iron-thiolate distances. |
81(1,1,1,1) |