Preparation and structural characterization of two isomers of the rhenium phosphine complexes of stoichiometry Re2Cl5(PR3)3, where R = Me or Et

Abstract

by sublimation, giving colorless crystals having a melting point of 67 °C.Te[N(SIMe3)2]2 (2). The procedure for the preparation of 2 was identical with that of 1 except freshly sublimed TeCl4 was first dissolved in toluene before being added to an LiN(SiMe3)2/«-hexane solution at -78 °C. In a typical preparation using 1.10 g of LiN(SiMe3)2 (6.57 mmol) and 0.51 g of TeCl4 (1.89 mmol), a total of 0.43 g (0.97 mmol, 50% yield) of orange crystalline material having a melting point of [63][64][65] °C could be isolated by sublimation from the crude product. However, in order to obtain analytically pure product, the orange crystalline material had to be sublimed again twice (mp 69-71 °C). Anal. Found (calc

Electronic Structure of Anilinopyridinate-Supported Ru25+ Paddlewheel Compounds

“…Notably, Δ has been examined for a number of (δ,δ*) 1 and (δ,δ*) 3 complexes containing Mo 2 5+ , Tc 2 5+ , Re 2 5+ , and W 2 5+ bimetallic centers . Complexes bearing π-donating equatorial ligands, such as halides, exhibit δ → δ* transitions between 6500 and 7600 cm –1 . ,− Complexes with equatorial O -donor ligands (e.g., carboxylates) have Δ values of 14 500–18 200 cm –1 , , and those with N -donor ligands are similar (∼14 900 cm –1 ) . In comparison, the δ → δ* transitions for Ru 2 5+ carboxylate complexes have been observed at ∼1100 nm, yielding Δ ≈ 9000 cm –1 .…”

A Decade of Dinuclear Technetium Complexes with Multiple Metal–Metal Bonds

“…Single crystals of Tc 2 X 4 (PMe 3 ) 4 (X = Cl, Br) were grown in hexane. The compounds Tc 2 X 4 (PMe 3 ) 4 crystallize in the monoclinic space group C 2/ c and are isostructural with M 2 X 4 (PMe 3 ) 4 (M = Re, Mo, X = Cl, Br) 34. Both Tc 2 X 4 (PMe 3 ) 4 complexes exhibit the eclipsed conformation with D 2 d symmetry, the individual trans ‐TcX 2 (PMe 3 ) 2 units being nonplanar due to intramolecular repulsion (Figure 12).…”

“…31,32 The average Tc–P distances [2.4356(4) Å for X = Cl and 2.4434(8) Å for X = Br] are consistent with those found in monomeric trans ‐dihalo Tc II phosphine complexes 35. The Tc–X distances [2.3858(4) Å for X = Cl and 2.5207(5) Å for X = Br] are shorter than those in Tc II mononuclear complexes [Tc–Cl 2.424(2) Å in TcCl 2 (DPPE) 2 and Tc–Br 2.5925(7) Å in TcBr 2 (PMe 3 ) 4 ] 32,34. This phenomenon is primarily due to steric congestion in the monomer.…”

Pentachloro-1,3,6-tris(diethylphenylphosphino)dirhenium(II,III)

“…Although many dirhenium compounds with multiple metal± metal bonds and tertiary phosphine ligands (PR 3 ) of the type Re 2 Cl 5 (PR 3 ) 3 are known (Cotton & Walton, 1993), none containing diethylphenylphosphine ligands have been reported previously. Structures have been determined for 1,2,7-and 1,3,6-Re 2 Cl 5 (trimethylphosphine) 3 and 1,3,6-Re 2 Cl 5 (triethylphosphine) 3 (Cotton et al, 1990), 1,2,7-and 1,3,6-Re 2 Cl 5 (dimethylphenylphosphine) 3 (Cotton et al, 1998), 1,3,6-Re 2 Cl 5 (tri-n-propylphosphine) 3 (Cotton et al, 1999) and 1,3,6-Re 2 Cl 5 (dicyclohexylphosphine) 3 (Angaridis et al, 2002). The title compound, (I), was prepared from the quadruply bonded [Re 2 Cl 8 ] 2À ion in a solvent mixture containing a roomtemperature ionic liquid.…”