Angewandte Chemie International Edition · 2019 · 56 citations · 45 references
Natural SciencesChemistryMaterials ScienceMaterials ChemistryNanomaterialsSolid-state ChemistryCluster ChemistryCluster CompoundsCoordination ChemistryCrystal ChemistryNanomaterials SynthesisTransition Metal ChemistryCluster SynthesisMetal HydridesNanocluster ChemistrySingle-crystal DiffractionSingle-crystal Neutron DiffractionSingle-crystal X-ray DiffractionStructural Characterization Of ClustersTransition Metal Clusters
Abstract The structurally precise Cu‐rich hydride nanoclusters [PdCu 14 H 2 (dtc/dtp) 6 (C≡CPh) 6 ] (dtc: di‐butyldithiocarbamate ( 1 ); dtp: di‐isopropyl dithiophosphate ( 2 )) were synthesized from the reaction of polyhydrido copper clusters [Cu 28 H 15 (S 2 CN n Bu 2 ) 12 ] + or [Cu 20 H 11 {S 2 P(O i Pr) 2 } 9 ] with phenyl acetylene in the presence of Pd(PPh 3 ) 2 Cl 2 . Their structures and compositions were determined by single‐crystal X‐ray diffraction and the results supported by ESI‐mass spectrometry. Hydride positions in 1 were confirmed by single‐crystal neutron diffraction. Each hydride is connected to one Pd 0 and four Cu I atoms in slightly distorted trigonalbipyramidal geometry. The anatomies of clusters 1 and 2 are very similar and DFT calculations allow rationalizing the interactions between the encapsulated [PdH 2 ] 2− unit and its Cu 14 bicapped icosahedral cage. As a result, Pd has the highest coordination number (14) so far recorded.
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