posted on 2016-08-08, 12:51authored byNour Alashkar, Christina Dietz, Samer Baba Haj, Wolf Hiller, Klaus Jurkschat
The syntheses of the intramolecularly coordinated organotin compounds
{Me<sub>2</sub>N(CH<sub>2</sub>)<sub>3</sub>}Ph(X)SnCH<sub>2</sub>SnPh<sub>2</sub>X (<b>3</b>, X = I; <b>4</b>, X = F)
and {Me<sub>2</sub>N(CH<sub>2</sub>)<sub>3</sub>}Ph(F)Sn(CH<sub>2</sub>)<sub>3</sub>SnPh<sub>2</sub>F (<b>7</b>) are reported.
The compounds have been characterized by elemental analysis, electrospray
mass spectrometry, <sup>1</sup>H,<sup>1</sup>H DOSY (<b>4</b>), <sup>13</sup>C, <sup>19</sup>F, and <sup>119</sup>Sn NMR spectroscopy,
and single-crystal X-ray diffraction analysis. In the solid state,
compound <b>4</b> is a head-to-tail dimer as a result of unsymmetrical
Sn–F–Sn bridges, whereas compound <b>7</b> is
a monomer with F→Sn intramolecular coordination, giving a six-membered
ring. In solution, both <b>4</b> and <b>7</b> are monomeric.
The reactions of both <b>4</b> and <b>7</b> with fluoride
anion in CD<sub>2</sub>Cl<sub>2</sub> have been investigated by variable-temperature <sup>19</sup>F and <sup>119</sup>Sn NMR spectroscopy.