An organocuprate(III) complex, [Cu(TMSPS3)(CH2CN)]- (2), was identified along with a sequential derivative, [Cu(TMSPS3)(CN)]- (3), and an intermediate, [Cu(TMSPS3)(HN=PPh3)] (4), formed in a relative transformation. Apical ligands among these complexes all strongly associate with a robust trigonal copper(III) platform. The nature of the ligand binding was spectroscopically and computationally investigated through a series of copper(III) complexes. The bonding along the principal C3 axis is adaptable, and σ interaction dominates the axial ligand coordination, where the cyanomethyl group exhibits the strongest bonding. Complex 2 is a scarce example of a thermostable aliphatic organocuprate(III) compound, which sheds some light on the organocopper(III) chemistry widely involved in many copper-mediated catalyses.
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