We have synthesized a number of Cu I complexes of thiophenolato ligands with different alkyl substituents in the ortho positions in a single-step procedure starting from a readily available copper(I) precursor to evaluate the coordination preferences of the metal atom. In most cases similar reaction conditions led to the formation of two complexes: a mononuclear complex and a polynuclear cluster, as evident from Xray crystallography. One dinuclear complex formed has the unique geometry of an L 2 Cu 2 (µ-L) 2 core that has not previously been observed for related systems. The steric bulk around the metal atom has a clear effect on the coordination sphere of the complex obtained. Ligands with no ortho sub-
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