Solid-state coordination chemistry of molybdenum oxides with di-2-picolylamine (pca): The hydrothermal syntheses and structures of the molecular cluster [{Ni(pca)(H2O)}2Mo8O26], the two-dimensional [{Cu(pca)}2Mo8O26], and the one-dimensional [{Cu3(pca)3MoO4}Mo8O 26]

Randy S. Rarig, Jon Zubieta

Research output: Contribution to journalArticle

33 Scopus citations

Abstract

The hydrothermal reaction of di-2-picolylamine (pca), MoO3 and NiSO4·6H2O yielded the bimetallic oxide cluster [{Ni(pca)(H2O)}2Mo8O26]· 2H2O (1.2H2O). Similarly, the reaction of pca, MoO3 and CuSO4·5H2O produced the two-dimensional material [{Cu(pca)}2Mo8O26] (2). The structure of 1 consists of β-{Mo8O26}4- clusters, decorated with {Ni(pca)(H2O)}2+ subunits, linked to terminal molybdenyl {Mo=O} moieties. The structure of 2 also contains β-{Mo8O26}4- clusters as building blocks; however, in this instance, the {Cu(pca)}2+ subunits serve to bridge adjacent clusters into a two-dimensional network. The hydrothermal reaction of pca and CuSO4·5H2O with MoO2 in place of MoO3 produced [{Cu3(pca)3MoO4}Mo8O 26]·2H2O (3.2H2O), a one-dimensional material, constructed from β-{Mo8O26}4- clusters linked through unusual {Cu3(pca)3MoO4}4+ subunits. Crystal data: C12H17N3O15Mo4Ni (1.2H2O): triclinic P1, a = 9.4024(5) Å, b = 10.9729(6) Å, c = 11.4183(6) Å, α = 102.710(1)°, β = 99.731(1)°, γ = 90.021(1)°, V = 1131.8(1) Å3, Z = 2, Dcalc = 2.596 g cm-3; C12H13N3O13Mo4Cu (2): monoclinic P21/n, a = 12.1547(4) Å, b = 12.5412(4) Å, c = 14.1160(4) Å, β = 92.746 (1)°, V = 2149.3(1) Å3, Z = 4, Dcalc = 2.638 g cm-3; C36H43Cu3 Mo9N9O32 (3.2H2O), monoclinic, P21/c, a = 17.9115(6) Å, b = 14.3637(5) Å, c = 22.6795(8) Å, β = 94.744(1)°, V = 5814.9(3) Å3, Z = 4, Dcalc = 2.476 g cm-3.

Original languageEnglish (US)
Pages (from-to)370-375
Number of pages6
JournalJournal of Solid State Chemistry
Volume167
Issue number2
DOIs
StatePublished - Sep 2002

Keywords

  • Hydrothermal synthesis
  • Molybdenum oxides
  • Organic-inorganic hybrid materials
  • Oxide clusters

ASJC Scopus subject areas

  • Electronic, Optical and Magnetic Materials
  • Ceramics and Composites
  • Condensed Matter Physics
  • Physical and Theoretical Chemistry
  • Inorganic Chemistry
  • Materials Chemistry

Fingerprint Dive into the research topics of 'Solid-state coordination chemistry of molybdenum oxides with di-2-picolylamine (pca): The hydrothermal syntheses and structures of the molecular cluster [{Ni(pca)(H<sub>2</sub>O)}<sub>2</sub>Mo<sub>8</sub>O<sub>26</sub>], the two-dimensional [{Cu(pca)}<sub>2</sub>Mo<sub>8</sub>O<sub>26</sub>], and the one-dimensional [{Cu<sub>3</sub>(pca)<sub>3</sub>MoO<sub>4</sub>}Mo<sub>8</sub>O <sub>26</sub>]'. Together they form a unique fingerprint.

  • Cite this