From a Heterocycle Through a Hetero(spiro)cycle to a “Genuine Heterocycle”

References

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• Spectroscopic data for 3: Isolated yield 37%; NMR (CD2Cl2) 31P{1H}: 55 ppm; 13{1H}: 130, 129.9, 129.5, 128.5 (d, J = 3.8Hz), 46.9, 2.2, 1.2 ppm; 1H: 7.36 (m, 5H), 3.51 (m, 2H), 2.48 (s, 1H), 0.31 (s, 6H), 0.24 ppm (s, 6H); IR (Nujol, CsI, cm-1): 3313m, 2722w, 1953w, 1602w, 1587w, 1493m, 1411w, 1258s, 1187w, 1130w, 1070sh, 1050s, 979s, 912s, 880sh, 846s, 829sh, 809s, 777s, 758s, 699s, 673m, 647m, 612w, 595m, 551s, 531s, 508s, 487s, 439w, 417m.
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• X-ray data for 3: C13H26AlCl2N2PSSi2 MW = 427.45, colourless plates, monoclinic, P21/n, Z = 4, a = 12.694(2)Å, b = 12.275(3)Å, c = 15.541(3)Å, β = 107.95(1)°, V = 2303.8(8)Å3, Dc = 1.232 g cm-3, F(000) = 896, reflections with I > 3[sgrave]I = 1269, parameters = 199, R = 0.0406, Rw = 0.0551, GOF = 2.441.
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