Locating Interstitial Hydrides in MH2@Cu14 (M = Cu, Ag) Clusters by Single-Crystal X‑ray Diffraction

Two structures, [Cu15H2(S2CNnBu2)6(CCPh)6][CuCl2] (1) and [AgH2Cu14{S2P(OiPr)2}6(CCPh)6][PF6] (2), are characterized by X-ray crystallography with high-quality single crystals. The position of interstitial hydrides can be accurately located. In addition, the refinement of the hydrides with anisotropic displacement parameters (ADPs) was successful. The distances between the central atom and copper atoms, as well as the distances within the metal cages surrounding the hydrides, are analyzed and compared with similar MH2@Cu14 (M = Cu, Ag, Pd) compounds. This work provides a thoughtful and accurate assessment of the considerations and challenges associated with anisotropic refinement for H atoms, particularly in X-ray data collection.