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The reaction of [Rh(H)(PEt3)3] (1) with the refrigerant HFO‐1234yf (2,3,3,3‐tetrafluoropropene) affords an efficient route to obtain [Rh(F)(PEt3)3] (3) by C–F bond activation. Catalytic hydrodefluorinations were achieved in the presence of the silane HSiPh3. In the presence of fluorosilane the fluorido complex 3 provides a C–H bond activation followed by a 1,2‐fluorine shift to produce [Rh{(E)‐C(CF3)=CHF}(PEt3)3] (4). Similar rearrangements of HFO‐1234yf were observed at [Rh(E)(PEt3)3] (E = Bpin (6), C7D7 (8), Me (9)). The ability to favor C–H bond activation using [Rh(F)(PEt3)3] (3) and fluorosilane is also demonstrated with 3,3,3‐trifluoropropene. Studies are supported by DFT calculations.

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