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The three‐component reaction of the tetrahedral diphosphorus complex [Cp 2 Mo 2 (CO) 4 (η 2 ‐P 2 )] ( 1 ), with Ag[BF 4 ] ( 2 ) in the presence of 2,2′‐bipyrimidine ( 3 ) leads to the formation of the two novel two‐dimensional networks  4  and  5 . Compound  4  is a new two‐dimensional organometallic‐organic hybrid polymer, while derivative  5  represents a unique two‐dimensional organometallic‐inorganic‐organic hybrid polymer. These results show the possibility of synthesizing a new class of coordination polymers, which could not be obtained from two‐component reactions with organic molecules in addition of metal ions.

The Diphosphorus Complex [Cp 2 Mo 2 (CO) 4 (η 2 ‐P 2 )] as a Building Block for the Synthesis of Mixed‐Hybrid Coordination Polymers