title: Preparation and Structural Properties of InIII-H Complexes.
abstract: The use of the tripodal ligands tris[(N'-tert-butylureaylato)-N-ethyl]aminato ([H3buea]3-) and the sulfonamide-basedN,N',N"-[2,2',2"-nitrilotris(ethane-2,1-diyl)]tris(2,4,6-trimethylbenzene-sulfonamidato) ([MST]3-) has led to the synthesis of two structurally distinct In(III)-OH complexes. The first example of a five-coordinate indium(III) complex with a terminal hydroxide ligand, K[InIIIH3buea(OH)], was prepared by addition of In(OAc)3and water to a deprotonated solution of H6buea. X-ray diffraction analysis, as well as FTIR and1H NMR spectroscopic methods, provided evidence for the formation of a monomeric In(III)-OH complex. The complex contains an intramolecular hydrogen bonding (H-bonding) network involving the In(III)-OH unit and [H3buea]3-ligand, which aided in isolation of the complex. Isotope labeling studies verified the source of the hydroxo ligand as water. Treatment of the [InIIIMST] complex with a mixture of 15-crown-5 ether and NaOH led to isolation of the complex [15-crown-5⊃NaI-(μ-OH)-InIIIMST], whose solid-state structure was confirmed using X-ray diffraction methods. Nuclear magnetic resonance studies on this complex suggest it retains its heterobimetallic structure in solution.
authors.affiliation: Department of Chemistry, University of California-Irvine, 1102 Natural Sciences II, Irvine, CA 92697.
authors.forename: Nathaniel S
authors.initials: NS
authors.lastname: Sickerman
authors.affiliation: Department of Chemistry, University of California-Irvine, 1102 Natural Sciences II, Irvine, CA 92697.
authors.forename: Renée M
authors.initials: RM
authors.lastname: Henry
authors.affiliation: Department of Chemistry, University of California-Irvine, 1102 Natural Sciences II, Irvine, CA 92697.
authors.forename: Joseph W
authors.initials: JW
authors.lastname: Ziller
authors.affiliation: Department of Chemistry, University of California-Irvine, 1102 Natural Sciences II, Irvine, CA 92697.
authors.forename: A S
authors.initials: AS
authors.lastname: Borovik