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Tp′Rh[P(OMe)3](Me)H, loses methane in pentane solution containing CH2F2 to give the scorpionate complex bis(μ‐dimethyl phosphito)‐κ2P:O;κ2O:P‐bis{methyl[tris(3,5‐dimethyl‐1H‐pyrazol‐1‐yl‐κN2)borato]rhodium(III)}, [Rh2(CH3)2(C2H6O3P)2(C15H22BN6)2], in which the phosphine O—Me bond is cleaved. The product is dimeric and resembles the Arbusov‐type rearrangement product known to form from trimethyl phosphite.
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