Synthesis and Characterization of a Neutral Six-coordinate Tris-adduct of an Indium(III) Trihalide. X-ray Crystal Structure of InCl3(THF)3
Abstract
The reaction of InCl3 with excess THF afforded the adduct InCl3(THF)3 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 indium(III) 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 InCl3(THF)3 belong to the monoclinic space group P 2 sub 1/c with unit cell parameters a = 8.1863(2)A, b = 12.5141(2) A, c =16.815(4) A, Beta = 93.84(4) deg, V = 1718.8(7) A3 for Z = 4. Full-matrix least-squares refinement based on 1603 reflections with I > 2.5(sigma) (I) converged at R sub w = 0.062 (R sub w = 0.084). IR spectroscopic measurements gave absorption bands near 1027 and 857/cm, 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.
Document Details
- Document Type
- Technical Report
- Publication Date
- May 05, 1994
- Accession Number
- ADA279169
Entities
People
- Peter S. White
- Richard L. Wells
- Ryan A. Baldwin
- Shreyas S. Kher
Organizations
- Duke University