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A decanuclear silver chalcogenide cluster, [Ag 10 (Se){Se 2 P(O  i  Pr) 2 } 8 ] ( 2 ) was isolated from a hydride-encapsulated silver diisopropyl diselenophosphates, [Ag 7 (H){Se 2 P(O  i  Pr) 2 } 6 ], under thermal condition. The time-dependent NMR spectroscopy showed that 2 was generated at the first three hours and the hydrido silver cluster was completely consumed after thirty-six hours. This method illustrated as cluster-to-cluster transformations can be applied to prepare selenide-centered decanuclear bimetallic clusters, [Cu x Ag 10-x (Se){Se 2 P(O  i  Pr) 2 } 8 ] (x = 0-7, 3 ), via heating [Cu x Ag 7-x (H){Se 2 P(O  i  Pr) 2 } 6 ] (x = 1-6) at 60 °C. Compositions of 3 were accurately confirmed by the ESI mass spectrometry. While the crystal 2 revealed two un-identical [Ag 10 (Se){Se 2 P(O  i  Pr) 2 } 8 ] structures in the asymmetric unit, a co-crystal of [Cu 3 Ag 7 (Se){Se 2 P(O  i  Pr) 2 } 8 ] 0.6 [Cu 4 Ag 6 (Se){Se 2 P(O  i  Pr) 2 } 8 ] 0.4 ([ 3a ] 0.6 [ 3b ] 0.4 ) was eventually characterized by single-crystal X-ray diffraction. Even though compositions of 2 , [ 3a ] 0.6 [ 3b ] 0.4 and the previous published [Ag 10 (Se){Se 2 P(OEt) 2 } 8 ] ( 1 ) are quite similar (10 metals, 1 Se 2- , 8 ligands), their metal core arrangements are completely different. These results show that different synthetic methods by using different starting reagents can affect the structure of the resulting products, leading to polymorphism.

A New Synthetic Methodology in the Preparation of Bimetallic Chalcogenide Clusters via Cluster-to-Cluster Transformations