150592-85-1Relevant academic research and scientific papers
Synthesis, spectroscopic investigations, and molecular structures of 1-phenyl-1-chalcogeno-4-methyl-4-chloro-1λ 5,4-phosphastanninanes, Me(Cl)Sn(CH2-CH2)2P(E)Ph (E = O, S, Se)
Weichmann, Horst,Meunier-Piret, Jacqueline
, p. 4097 - 4103 (2008/10/08)
A series of 1-phenyl-1-chalcogeno-4-methyl-4-chloro-1λ 5,4-phosphastanninanes Me(Cl)Sn-(CH2-CH2)2P(E)Ph with E = S, Se, O (7-9) has been synthesized by chlorodemetalation of the related tetraorganotin derivatives Me2Sn(CH2-CH2)2P(E)Ph (1-3) with Me2SnCl2. 119Sn, 31P, and 1H NMR studies in nonpolar solvents show that 7-9 exhibit a P=E?Sn coordination which is intramolecular for 7 and 8 (E = S, Se) and intermolecular for 9 (E = O). In donor solvents the intramolecular interaction of 7 and 8 is no longer present. The molecular structures of 7-9 were determined by X-ray analysis. The structure determination of 7 gave the monoclinic space group P21/c (a = 12.256(15), b = 9.293(6), c = 12.622(13) A?; β = 96.64(10)°; V = 1427.9(25) A?3; Z = 4; R = 0.040). 8 crystallizes in the orthorhombic space group Pccn (a = 22.703(3), b = 16.910(22), c = 7.523(4) A?; V = 2888.1(51) A?3; Z = 8; R = 0.053). 9 has the triclinic space group P1 (a = 7.606(3), b = 10.179(2), c = 9.883(2) A?; α = 117.97(2), β = 96.58(3), γ = 87.80(3)°; V = 671.2(3) A?3; Z = 2; R = 0.0395). In the solid state 7-9 also exhibit pentacoordination at the tin with the ligand polyhedron approaching an ideal trigonal bipyramid in the order 7 a chair conformation for the 1λ5,4-phosphastanninane ring system, whereas 7 and 8 are monomeric with intramolecular P=E?Sn coordination and a boat conformation of the six-membered ring.
