151193-50-9Relevant academic research and scientific papers
Azastannatranes: Synthesis and structural characterization
Plass, Winfried,Verkade, John G.
, p. 5145 - 5152 (2008/10/08)
Syntheses of the new azastannatranes ZSn(MeNCH2CH2)3N (5, Z = n-Bu; 7, Z = Me; 9, Z = Ph; 11, Z = Me2N; 12, Z = 1/2O) and ZSn(HNCH2CH2)3N (6, Z = n-Bu; 8, Z = Me; 10, Z = Ph) are reported. Evidence for a pentacoordinate structure in these compounds is adduced from 3J(119SnH) couplings in the apical Z groups and from their 119Sn chemical shifts measured in solution and in the solid state. In the case of 10, two crystallographically different tin sites were suggested by 13C and 119Sn CP/MAS NMR spectroscopy. X-ray crystallographic experiments on this compound confirmed the presence of two trigonal bipyramidal structures featuring different Sn-Nax bond lengths (238.0(2), 245.3(2) pm). Crystal data: triclinic, P1, a = 1089.6(2) pm, b = 1097.7(2) pm, c = 1356.9(3) pm, α = 107.80(1)°, β = 112.67(1)°, γ = 101.19(1)°, Z = 4, R = 0.031, Rw = 0.053. VT 1H NMR spectral studies of 5-11 gave ΔGTo? values ranging from 33.3 to 36.4 kcal/mol for the racemization of the rings in the triclinic cage moiety. Mass spectral and infrared features of 5-12 are also discussed.
