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

Two structures, [Cu15H2((S2CNBu2)-Bu- n )(6)(C VCPh)(6)][CuCl2] (1) and [AgH2Cu14{S2P((OPr)-Pr- i )(2)}(6)(C VCPh)(6)][PF6] (2), are characterized by X-ray crystallography with high-quality singlecrystals. The position of interstitial hydrides can be accuratelylocated. In addition, the refinement of the hydrides with anisotropicdisplacement parameters (ADPs) was successful. The distances betweenthe central atom and copper atoms, as well as the distances withinthe metal cages surrounding the hydrides, are analyzed and comparedwith similar MH2@Cu-14 (M = Cu, Ag, Pd) compounds.This work provides a thoughtful and accurate assessment of the considerationsand challenges associated with anisotropic refinement for H atoms,particularly in X-ray data collection.