Since moisture may frequently be present in many solvents, it is important to know the reactivity of a catalyst against water for catalytic reactions. In order to explore the stability and understand the transformation process of diphosphino‐boryl‐based PBP pincer platform, [PdCl{B(NCH2PtBu2)2−o‐C6H4}] (1) was treated with PdCl2, HB(NCH2PPh2)2−o‐C6H4 was reacted with [PdCl2(cod)] (cod=cyclo‐octa‐1,5‐diene) and [Pd2(dba)3] (dba=dibenzylideneacetone), respectively, in the presence of water. Some novel palladium POP complexes, [Pd2Cl2(μ‐Cl){μ‐κ3‐P,O,P−OB(NCH2PtBu2)2−o‐C6H4}] (2 a), [Pd4(μ‐Cl)2(μ‐O)2{μ‐κ3‐P,O,P−OB(NCH2PPh2)2−o‐C6H4}2] (2 b), [Pd2{μ‐κ4‐P,P,P,P−O(B(NCH2PPh2)2−o‐C6H4)2}{μ‐κ2‐P,P−(NHCH2PPh2)2−o‐C6H4}] (3), were obtained. It was found that the PBP pincer backbone can easily be converted into a POP backbone in the presence of water. From the crystal structures of the resultant palladium complexes, possible pincer backbone transformation pathways were discussed.
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