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The First Spacer‐Bridged Tetraorganodistannoxanes with a Mixed Double Ladder Structure
Author(s) -
Mehring Michael,
Paulus Ingo,
Zobel Bernhard,
Schürmann Markus,
Jurkschat Klaus,
Duthie Andrew,
Dakternieks Dainis
Publication year - 2001
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/1099-0682(20011)2001:1<153::aid-ejic153>3.0.co;2-m
Subject(s) - chemistry , yield (engineering) , electrospray mass spectrometry , crystallography , mass spectrometry , nuclear magnetic resonance spectroscopy , crystal structure , x ray crystallography , spectroscopy , stereochemistry , diffraction , electrospray , materials science , physics , optics , chromatography , quantum mechanics , metallurgy
The reaction of Me 3 SiCH 2 Cl 2 Sn(CH 2 ) 3 SnCl 2 Ph ( 6 ) with ( t Bu 2 SnO) 3 gave a statistical mixture of the corresponding tetraorganodistannoxanes whereas the reaction of the spacer‐bridged ditin tetrachlorides RCl 2 Sn(CH 2 ) 4 SnCl 2 R ( 3 , R = Me 3 CCH 2 ; 4 , R = Me 2 CHCH 2 ; 10 , R = Me 3 SiCH 2 ) with the polymeric spacer‐bridged ditin oxides [R(O)Sn(CH 2 ) 4 Sn(O)R] n ( 7 , R = Me 2 CHCH 2 ; 8 , R = Me 3 CCH 2 ; 11 , R = Me 3 SiCH 2 ) provided the mixed double ladder compounds {[R(Cl)Sn(CH 2 ) 4 Sn(Cl)R][R′(Cl)Sn(CH 2 ) 4 Sn(Cl)R′]O 2 } 2 ( 9 , R = Me 3 CCH 2 , R′ = Me 2 CHCH 2 ; 12 , R = Me 3 CCH 2 , R′ = Me 3 SiCH 2 ) in almost quantitative yield. In solution, 9 and 12 are in equilibrium with their corresponding dimers, as was evidenced by 119 Sn NMR spectroscopy, molecular mass determination, and electrospray mass spectrometry. The molecular structures of 9 and 12 were established by single crystal X‐ray diffraction.