Transients from a mixture of [(R(O)Sn)2C(CH3)2]2 and (RCl2Sn)2C(CH3)2 [R = (SiMe3)2CH]: an identification in situ by 1D 119Sn and 2D 1H119Sn HMQC NMR spectroscopy and electrospray mass spectrometry

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The reaction of the 2,2‐bis(organodichlorostannyl)propane [(Me3Si)2CH(Cl2)Sn]2CMe2 (A) with the corresponding organotin oxide {[(Me3Si)2CH(O)Sn]2CMe2}2 (B) does not provide the corresponding normally expected tetraorganodistannoxane {[(Me3Si)2CH(Cl)SnCMe2Sn(Cl)CH(SiMe3)2]O}n but a complex reaction mixture. One major product, namely the 2,4,6,8‐tetraorgano‐2,6‐dichloro‐1,5,9‐trioxa‐2,4,6,8‐tetrastannabicyclo[3.3.1]nonane derivative [(Me3Si)2CHSnCMe2Sn(Cl)CH(SiMe3)2]2O3 (C) was identified in situ by 2D 1H119Sn and 1H13C heteronuclear multiple quantum coherence and heteronuclear multiple bond correlation NMR spectroscopy as well as electrospray mass spectrometry. Compound C is proposed to be in equilibrium with an ionic species C′, the cation of which has an adamantane‐type structure.