Crystal and molecular structures of three diimine adducts of diphenyltin dichloride

Abstract

Abstract The crystal structures of three diimine adducts of diphenyltin dichloride have been determined at room temperature. The colorless crystals of the adduct formed with 5-methylphenanthroline, [Ph2SnCl2(5-Mephen)], C25H20Cl2N2Sn, are monoclinic, space group P21/n with unit cell dimensions a = 9.393(5) Å b = 12.896(3) Å, c = 18.034(4) Å, β = 94.48(3)°, Z = 4 and D x = 1.641Mg m−3. The yellow crystals of the 4,7-dimethylphenanthroline adduct, [Ph2SnCl2(4,7-Me2phen)], C26H22Cl2N2Sn, are monoclinic, space group P21/n with unit cell dimensions a = 9.163(2) Å, b = 17.828(4) Å, c = 14.395(5) Å, β = 101.29(2)°, Z = 4 and D x = 1.590Mg m−3. Yellow crystals of the 4,5-diazafluorene-9-one adduct, [Ph2SnCl2(4,5-diazafluorene-9-one)], C23H16Cl2N2OSn, are orthorhombic, space group Pbca with unit cell dimensions a = 16.239(2) Å, b = 16.673(2) Å, c = 16.058(2) Å, Z = 8 and Dx = 1.607Mg m−3. The structures were solved by direct methods and refined by a full-matrix least-squares procedure to final R = 0.043 using 2542 reflections for [Ph2SnCl2(5-Mephen)], R = 0.060 using 2521 reflections for [Ph2SnCl2(4,7-Me2phen)], and R = 0.038 using 1919 reflections for [Ph2SnCl2(4,5-diazafluorene-9-one)]. The tin atoms in the three adducts exist in distorted octahedral geometries with the phenyl substituents occupying trans positions. An examinations of the derived parameters in the three structures shows that the two phenanthroline ligands have similar coordinating abilities towards Ph2SnCl2 and that these ligands are stronger Lewis bases than 4,5-diazafluorene-9-one.