Large metal ion-centered template reactions. A uranyl complex of cyclopentakis(2-iminoisoindoline)

Victor W. Day, Tobin J. Marks, William A. Wachter

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Abstract

The reaction of o-dicyanobenzene with anhydrous uranyl chloride does not yield a cyclic, four-subunit phthalocyanine complex. Rather, it yields an expanded, cyclic five-subunit pentakis(2-iminoisoindoline) complex-a "superphthalocyanine". Dioxocyclopentakis(2-iminoisoindoline)uranium(VI), UO2(N2C8H4)5, crystallizes in the monoclinic space group, P21/c, with a = 8.210 (3) Å, b = 21.667 (7) Å, c = 18.462 (5) Å, β = 103.16 (2)°, and Z = 4 (ρcald = 1.891, ρobsd = 1.882 g/cm3). Intensity measurements were made for 9564 independent reflections having 2θMo Kᾱ <60.4° at 20 ± 1° with Nb-filtered Mo Kᾱ radiation on a Syntex P-i autodiffractometer. The structure was solved using the heavy atom technique. Cycles of anisotropic full-matrix least-squares refinement have given a final value of 0.054 for the conventional unweighted residual, R, for 4709 independent reflections having I > 3σ(I). The coordination geometry of the uranium atom approximates an idealized compressed pentagonal bipyramid. The two axial ligands are oxygen atoms with an average U-O bond length of 1.744 (8) Å. The equatorial coordination is by five nitrogen atoms (the average U-N bond length is 2.524 (9) Å) of the 20-atom "inner" ring of the 50-atom (excluding hydrogens) macrocycle. The cyclopentakis(2-iminoisoindoline) ligand is severely and irregularly distorted from planarity, presumably as a consequence of appreciable steric strain within the macrocycle.

Original languageEnglish
Pages (from-to)4519-4527
Number of pages9
JournalJournal of the American Chemical Society
Volume97
Issue number16
Publication statusPublished - 1975

ASJC Scopus subject areas

  • Chemistry(all)

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