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In order to correlate 119Sn Mössbauer parameters and structural data for dimethyltin(IV) derivatives, the molecular structures of bis(acetato)dimethyltin(IV) and bis(trifluoroacetato)dimethyltin(IV) were determined by single crystal X‐ray diffration. Crystals of Me2Sn(OOCCH3)2 are monoclinic, a = 26.282(4), b = 5.282(1), c = 14.434(3) Å, β = 101.17(2)°, Z = 8, space group C2/c, and those of [Me2Sn(OOCCF3)2]n are monoclinic, a = 8.444(1), b = 17.689(1), c = 15.368(1) Å, β = 93.013(9)°, Z = 8, space group Cc. The structures were solved by the Patterson method and were refined by full‐matrix least‐squares procedures to R = 0.025 and 0.027 (Rw = 0.023 and 0.030) for 2 298 and 4 182 reflections with I ≥ 3σ(F2), respectively.

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