Crystal structure of octa-μ₃-selenido-(p-toluenesulfonato-κO)pentakis(triethylphosphane-κP)-octahedro-hexarhenium(III)p-toluenesulfonate dichloromethane disolvate

Abstract

The title compound, [Re6Se8{O3SC6H4(CH3)}{P(C2H5)3}5](CH3C6H4SO3)·2CH2Cl2, contains the face-capped hexa­nuclear [Re6(μ3-Se)8]2+ cluster core. The [Re6Se8]2+ cluster core displays a non-crystallographic center of symmetry and is bonded through the ReIII atoms to five tri­ethyl­phosphane ligands and one p-toluene­sulfonate ligand. One p-toluene­sulfonate counter-ion and two di­chloro­methane solvent mol­ecules are also present in the asymmetric unit. One of the ethyl chains of one triethylphos­phane ligand and one of the CH2Cl2 solvent molecules are disordered over two sets of sites (occupancy ratios 0.65:0.35 and 0.5:0.5, respectively). The Re—O(sulfon­ate) bond length of 2.123 (5) Å is similar to other Re—O bond lengths of hexa­nuclear rhenium chalcogenide clusters containing other O-donor ligands such as dimethyl sulfoxide (DMSO), di­methyl­formamide (DMF) and hydroxide.

Rhenium Selenide Clusters Containing Alkynyl Ligands: Unexpected Reactivity of σ-Bound Phenylacetylide

“…[Re 6 Se 8 (PEt 3 ) 5 I]I and cis-and trans-[Re 6 Se 8 (PEt 3 ) 4 I 2 ] were synthesized from previously published procedures, 50,51 and the synthesis of [Re 6 Se 8 (PEt 3 ) 4 (OTs) 2 ] was modeled after the preparation of [Re 6 Se 8 (PEt 3 ) 5 (OTs)](OTs). 52 Phenylacetylene, dimethyl sulfate, dry THF, and the lithium phenylacetylide solution (1.0 M in THF) were purchased from Sigma-Aldrich. Triethylamine was dried using a 2% weight per volume amount of 4 Å molecular sieves; all other materials were purchased and used as received.…”