A structural study of ligand exchange on chalcogen‐passivated copper nanoclusters is far less developed. Herein, we report the synthesis of polyhydrido copper nanoclusters [Cu20H11{Se2P(O
iBu)2}9] (2) passivated by Se‐donor ligands via ligand replacement reaction on [Cu20H11{S2P(O
iPr)2}9] (1) with NH4[Se2P(O
iBu)2]. In parallel to the synthesis of 2, cluster [Cu20H11{S2P(CH2CH2Ph)2}9] (4) was produced by the ligand exchange reaction on a new derivative of 1, that is [Cu20H11{S2P(O
nPr)2}9] (3). Solid state structures of both clusters 2 and 4 were unequivocally established by single‐crystal X‐ray diffraction studies and cluster 4 epitomizes exceptional case to preserve both the shape and size of the nanocluster during the course of ligand exchange. Structurally precise cluster 2 is the second example where the copper hydride nanocluster is stabilized by Se‐donor ligands. The anatomy of 2 can be visualized as a twisted cuboctahedral Cu13 core, two triangular faces of which are capped by a Cu6 cupola and a single Cu atom along the C3 rotational axis.
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