Synthesis, structural characterization, photoluminescence and thermal properties of [(Ph3P)2Cu(μ-SeC{O}R)2Cu(PPh3)]

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Abstract
A number of neutral unsymmetrical dimers [(Ph3P)2Cu(μ-SeC{O}R)2Cu(PPh3)] (R = C6H5 (1), C6H4-Me-4 (2), C6H4-OMe-4 (3), C6H4-Cl-4 (4), C6H4-F-4 (5) and CH3 (6)) were synthesized in moderate yield, and characterized by analytical and spectroscopic techniques including 31P NMR. Variable temperature 31P NMR experiments appear to indicate that the molecular structure is retained in solution. X-Ray structure determination of 2 and 6 confirmed the molecular geometry of the unsymmetrical dimer. In 2 the two 4-MeO-C6H4CO groups have anti stereochemistry with respect to the Cu2Se2 ring while MeCO groups have syn configuration in 6. A weak C–H⋯OC intramolecular hydrogen bond present between the two selenoacetato ligands appears to dictate the syn geometry in 6. This hydrogen bonding is also responsible for the non-planarity of the Cu2Se2 ring. These compounds are photoemissive in CH2Cl2 solution. Thermogravimetry and pyrolysis experiments in nitrogen atmosphere show that 1–6 are good single source precursors to copper selenide bulk materials. Preliminary experiments show that these compounds are good single source molecular precursors for cubic phase Cu2−xSe nanoparticles with an average size of 75 ± 15 nm.

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