Isolation and characterization of [n-Bu2Sn(OH2)(phen)(OSO2CF3)](O3SCF3) (phen = 1,10-phenanthroline): The missing link

Abstract

Reaction of [n-Bu₂Sn(μ-OH)(H₂O)(OSO₂CF₃)]₂ (1) with 1,10-phenanthroline (phen) in acetonitrile at room temperature in a 1:0.75 molar ratio leads to the formation of a mixture of three species comprising [{n-Bu₂Sn(H₂O)}₂O·n-Bu₂Sn(OH)₂](O₃SCF₃)₂ (2) and [{n-Bu₂Sn(OH)(OSO₂CF₃)}(n-Bu₂SnO)]₂ (3) as well as the title compound [n-Bu₂Sn(OH₂)(phen)(OSO₂CF₃)](O₃SCF₃) (4). Compounds 1, 2 and 3 crystallize in dichloromethane at –20 °C, while 4 remains in solution under these conditions. After filtration and by repeating this procedure several times (four in total), it was possible to isolate only 4. Single-crystals of 4, suitable for an X-ray diffraction analysis, were grown from a mixture of dichloromethane/toluene. Compound 4 consists of a mononcationic di-n-butyltin(IV) complex, N,N-chelated by one phen ligand and coordinated by one water molecule and one trifluoromethanesulfonato ligand. In the crystal lattice, the individual molecule of 4 are associated in dimers resulting from intermolecular hydrogen-bonding interactions between aqua ligands and trifluoromethasulfonate counteranions. The isolation and characterization of compound 4 provides new insights into the reactivity of 1 with phen.