Synthesis and Characterization of a Neutral Six-coordinate Tris-adduct of an Indium(III) Trihalide. X-ray Crystal Structure of InCl3(THF)3
DUKE UNIV DURHAM NC DEPT OF CHEMISTRY
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The reaction of InCl3 with excess THF afforded the adduct InCl3THF3 in a good yield 77.1 based on InCl3, and the X-ray crystal structure shows it to be a hexa-coordinated tris-adduct of indiumIII chloride. The crystal structure consists of discrete monomeric units with no abnormally short intermolecular separations. The geometry about the indium atom approximates to octahedral with the three chlorine atoms mean In-Cl 2.422 A and the oxygen atoms of each THF molecule mean In-O 2.254 A residing in the meridional conformation. Crystals of InCl3THF3 belong to the monoclinic space group P 2 sub 1c with unit cell parameters a 8.18632A, b 12.51412 A, c 16.8154 A, Beta 93.844 deg, V 1718.87 A3 for Z 4. Full-matrix least-squares refinement based on 1603 reflections with I 2.5sigma I converged at R sub w 0.062 R sub w 0.084. IR spectroscopic measurements gave absorption bands near 1027 and 857cm, which are consistent with coordinated THF molecules. Variable temperature NMR studies showed that the tris-adduct was stable to disproportionation in solution between 20-60 deg C. Indium compound, Six coordinate synthesis, Crystal structure.
- Inorganic Chemistry
- Physical Chemistry