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

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.

[1]  R. McDonald,et al.  Organometallic rhenium(III) chalcogenide clusters: coordination of N-heterocyclic carbenes. , 2015, Chemical communications.

[2]  G. Sheldrick.  Crystal structure refinement with SHELXL , 2015, Acta crystallographica. Section C, Structural chemistry.

[3]  R. McDonald,et al.  Azide alkyne cycloaddition facilitated by hexanuclear rhenium chalcogenide cluster complexes. , 2013, Dalton transactions.

[4]  R. McDonald,et al.  Preparation of a family of hexanuclear rhenium cluster complexes containing 5-(phenyl)tetrazol-2-yl ligands and alkylation of 5-substituted tetrazolate ligands. , 2012, Inorganic chemistry.

[5]  Sung‐Jin Kim,et al.  Octahedral cyanohydroxo cluster complex trans-[Re6Se8(CN)4(OH)2]4−: Synthesis, crystal structure, and properties , 2011 .

[6]  O. Efremova,et al.  Selective functionalisation of Re6 cluster anionic units: from hexa-hydroxo [Re6Q8(OH)6]4- (Q = S, Se) to neutral trans-[Re6Q8L4L'2] hybrid building blocks. , 2009, Dalton transactions.

[7]  L. F. Szczepura,et al.  Synthesis and electrochemical study of the first tetrazolate hexanuclear rhenium cluster complex. , 2007, Chemical communications.

[8]  Peter J. Orto,et al.  Alcohol addition to acetonitrile activated by the [Re6(mu3-Se)8]2+ cluster core. , 2007, Inorganic chemistry.

[9]  N. Kitamura,et al.  Emission and metal- and ligand-centered-redox characteristics of the hexarhenium(III) clusters trans- and cis-[Re6(mu 3-S)8Cl4(L)2]2-, where L is a pyridine derivative or pyrazine. , 2000, Inorganic chemistry.

[10]  Zhiping Zheng,et al.  Synthesis and Structures of Solvated Monoclusters and Bridged Di- and Triclusters Based on the Cubic Building Block [Re(6)(&mgr;(3)-Se)(8)](2+). , 1999, Inorganic chemistry.

[11]  Zhiping Zheng,et al.  Cluster Condensation by Thermolysis: Synthesis of a Rhomb-Linked Re12Se16 Dicluster and Factors Relevant to the Formation of the Re24Se32 Tetracluster , 1997 .

[12]  Colin Eaborn,et al.  Comprehensive Coordination Chemistry , 1988 .

[13]  E. Lindner,et al.  SO3-Einschiebungsreaktionen bei Organopentacarbonyl-rhenium(I)-Verbindungen , 1971 .