Cj. Cardin et al., THE FIRST STRUCTURALLY AUTHENTICATED COMPOUND CONTAINING A BOND BETWEEN DIVALENT TIN AND TETRAVALENT TIN, Organometallics, 17(11), 1998, pp. 2144-2146
The reaction of 1 equiv of [Li(thf)(3) . Sn-(SiMe3)(3)] (1) with [Sn(2
-{(Me3Si)(2)C}-C5H4N)Cl] in Et2O at ambient temperature affords the co
rresponding divalent Sn-tetravaLent Sn compound, [Sn(2-{(Me3Si)(2)C}-C
5H4N){Sn(SiMe3)(3)}] (2) in high yield. A single-crystal X-ray diffrac
tion study reveals 2 to be monomeric and the divalent Sn-tetravalent S
n bond to be 2.8689(5) Angstrom; this is the first measurement of such
a bond. The Sn-119-(H-1) NMR spectrum exhibits two singlet resonances
at delta 897 and -502, each with well-resolved, isotopically, shifted
, Sn-119 and Sn-117 satellites (ca. 6700 and ca. 6400 Hz, respectively
); this is the first measurement of (1)J coupling between Sit atoms of
different valence.