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Synthesis and crystal structures of dimeric W(Mo)/Cu/S and polymeric W/Cu/S neutral clusters with flexible 1,4-bis(3,5-dimethylpyrazol-1-yl)butane as a linker ligand

Lookup NU author(s): Professor William Clegg, Dr Ross Harrington, Dr Luca Russo

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Abstract

Reactions of [MES3](2) (M = W, Mo; E = S, O) with CuCl and bbd [1,4-bis(3,5-dimethylpyrazol-1-yl)butane] in DMF affords two new double nest-shape clusters, [WOS3Cu3Cl(mu-bbd)](2) (1) and [MoOS3Cu3Cl(mu-bbd)](2) (2) and a novel one-dimensional polymeric complex [WS4Cu2(mu-bbd)](n) (4). The complexes have been characterized by elemental analysis, IR and UV-Vis spectroscopy, and single-crystal X-ray diffraction. In the core structure of the isostructural dimeric [MOS3Cu3Cl(mu-bbd)](2) clusters, the copper atoms have a distorted trigonal planar geometry, with CuS2N and CuS2Cl core environments. The [MOS3Cu3] fragments are interconnected by a pair of flexible mu-bbd ligands via their nitrogen donor atoms to form a centrosymmetric macrocyclic twin-nest-shaped cluster in which the two fragments are also linked by direct secondary Cu center dot center dot center dot Cl interactions. Complex 4 represents the first example of a polymeric heterothiometallic cluster, interconnected by bbd ligands, to be structurally characterized by X-ray crystallography. In the repeat unit of 4, the skeleton of the cluster core [CuS2WS2Cu] has an essentially linear Cu center dot center dot center dot W center dot center dot center dot Cu arrangement. The W atom retains the tetrahedral geometry of the parent [WS4](2) anion. These cluster cores are linked by bbd bridges having alternately two different conformations to construct a zigzag structure. Complexes [MoS4Cu3Cl(bbd)(0.5)](2) (3) and [WS4Cu4(NCS)(2)(bbd)(2)](n) (5) have been synthesized and characterized by elemental analysis, IR and UV-Vis spectroscopy, but we have been unable to grow suitable crystals of 3 and 5 for X-ray analysis. (C) 2011 Elsevier B. V. All rights reserved.

Publication metadata

Author(s): Beheshti A, Clegg W, Fard SAM, Harrington RW, Nobakht V, Russo L

Publication type: Article

Publication status: Published

Journal: Inorganica Chimica Acta

Year: 2011

Volume: 376

Issue: 1

Pages: 310-316

Print publication date: 30/06/2011

ISSN (print): 0020-1693

ISSN (electronic): 1873-3255

Publisher: Elsevier BV

URL: http://dx.doi.org/10.1016/j.ica.2011.06.034

DOI: 10.1016/j.ica.2011.06.034

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