Syntheses, Structures, and Complexation Studies of Tris(organostannyl)methane Derivatives

The syntheses of tris(organostannyl)methanes HC(SnX(n)Ph((3‐n)))(3) (1, n=0; 2, n=1, X=I; 3, n=1, X =F; 4, n=1, X=Cl; 5, n=1, X=OAc; 6, n=2, X=I; 7, n=2, X=Cl) and the organostannate complexes Et(4)N[HC(SnIPh(2))(3)⋅F] (8), Ph(4)P[HC(SnClPh(2))(3)⋅Cl] (9), and [Ph(4)P](2)[HC(SnCl(2)Ph)(3)⋅2 Cl] (10) are reported. The compounds were characterized by (1)H, (13)C, (19)F, and (119)Sn NMR spectroscopy, IR spectroscopy, electrospray mass spectrometry, and (with the exception of 3) single‐crystal X‐ray diffraction analysis. From the reaction between 2 and AgClO(4) resulted the unprecedented hexanuclear organotin oxocluster [HC{Sn(ClO(4))(2)Ph(2)}(2)Sn(OH)(2)Ph](2) (11), the molecular structure of which was elucidated by using X‐ray crystallography.