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Transients from a mixture of [(R(O)Sn) 2 C(CH 3 ) 2 ] 2 and (RCl 2 Sn) 2 C(CH 3 ) 2 [R = (SiMe 3 ) 2 CH]: an identification in situ by 1D 119 Sn and 2D 1 H 119 Sn HMQC NMR spectroscopy and electrospray mass spectrometry
Author(s) -
Biesemans Monique,
Duthie Andrew,
Jurkschat Klaus,
Verbruggen Ingrid,
Willem Rudolph,
Zobel Bernhard
Publication year - 2003
Publication title -
applied organometallic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.53
H-Index - 71
eISSN - 1099-0739
pISSN - 0268-2605
DOI - 10.1002/aoc.443
Subject(s) - chemistry , heteronuclear molecule , mass spectrometry , protonation , nuclear magnetic resonance spectroscopy , derivative (finance) , crystallography , stereochemistry , analytical chemistry (journal) , medicinal chemistry , ion , organic chemistry , chromatography , financial economics , economics
Abstract The reaction of the 2,2‐bis(organodichlorostannyl)propane [(Me 3 Si) 2 CH(Cl 2 )Sn] 2 CMe 2 (A) with the corresponding organotin oxide {[(Me 3 Si) 2 CH(O)Sn] 2 CMe 2 } 2 (B) does not provide the corresponding normally expected tetraorganodistannoxane {[(Me 3 Si) 2 CH(Cl)SnCMe 2 Sn(Cl)CH(SiMe 3 ) 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 [(Me 3 Si) 2 CHSnCMe 2 Sn(Cl)CH(SiMe 3 ) 2 ] 2 O 3 (C) was identified in situ by 2D 1 H 119 Sn and 1 H 13 C 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. Copyright © 2003 John Wiley & Sons, Ltd.