Reactions of polyoxomolybdates with oximes. The crystal and molecular structures of...

Shuncheng Liu, Huizhe Zhu, Jon Zubieta

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Abstract

Title full: Reactions of polyoxomolybdates with oximes. The crystal and molecular structures of [(C4H9)4N]2[Mo2O 5C6H4(O)CHNO2] · CH2Cl2 and [(C4H9)4N]2[Mo2O 5C6H5CH(O)C(NO)C6H 52]. The reactions of [(C4H9)4N]2[Mo2O 7] with the oximes benzoinoxime and salicylaldoxime yielded the complexes [(C4H9)4N]2[Mo2O 5C6H4(O)CHNO2] · CH2CI2(7) and [(C4H9)4N]2[Mo2O 5C6H5CH(O)C(NO)C6H5 2] (8). The structures of 7 and 8 exhibit the [Mo2O5]2+ core with the oximato moieties of the ligands functioning as μ2-O,N bridging donors. The metrical parameters are consistent with the sp2 hybridization of the oximato nitrogen with double bond character localized on the C{single bond}N bond. Crystal data: Compound 7, monoclinic space group, P21/c, a = 16.271(6), b = 14.010(4), c = 25.390(8) Å, β = 101.34(2)°, V = 5672.9(19) Å3, Dcalc = 1.30 g cm-3 for Z = 4. Structure solution and refinement based on 4718 reflections with Fo ≥ 6σ(Fo)(Mo-Kα, λ = 0.71073 Å) converged at a conventional residual of 0.064. Compound 8, rhombohedral space group (hexagonal setting) R over(3, -), a = b = 47.188(14), c = 15.766(3) Å, V = 30403.4(27) Å3, Dcalc = 1.19 g cm-3 for Z = 18. Structure solution and refinement based on 3015 reflections with Fo ≥ 6σ(Fo) converged at a value of 0.069 for the conventional R factor. Reaction of the related salicylhydroxamic acid with [(C4H9)4N]2[Mo2O 7] in methanol yielded the complex [(C4H9)4N][MoO2C6 H4(OH)C(O)NOC6H4(OH)C(O)NHO] (11), a species exhibiting both hydroximato(2-) and hydroxamato(1-) forms of the ligand. Crystal data: Compound 11, monoclinic space group P21/c, a = 10.261(2), b = 17.864(4), c = 18.270(3) Å, β = 91.98(1)°, V = 3347.0(10) Å3, Dcalc = 1.34 g cm-3 for Z = 4. Structure solution and refinement based on 3406 reflections converged at a value of 0.049 for the conventional R factor.

Original languageEnglish (US)
Pages (from-to)2473-2480
Number of pages8
JournalPolyhedron
Volume8
Issue number20
DOIs
StatePublished - 1989
Externally publishedYes

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ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

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