The first organically templated layered cobalt phosphates: Hydrothermal syntheses and crystal structures of [H3N(CH2)3NH3] 0.5[Co(PO4)] · 0.5H2O and [H3N(CH2)4NH3] 0.5[Co(PO4)]

Jeffrey R.D. DeBord, Robert C. Haushalter, Jon Zubieta

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Abstract

The first organically templated layered cobalt phosphates have been prepared and structurally characterized by single crystal X-ray diffraction. The layered cobalt phosphate [H3N(CH2)3NH3] 0.5[Co(PO4)] · 0.5H2O (1) was prepared hydrothermally at 170°C over 48 h from an aqueous solution of CoCl2 · 6H2O, 1,3-diaminopropane, H3PO4 (85%), and H2O in the mole ratio 1:7.2:4:444. Phosphate 2, [H3N(CH2)4 NH3]0.5[Co(PO4)], was prepared in an analogous fashion from a mixture of CoCl2 · 6H2O,1,4-diaminobutane, H3PO4 (85%), (n-C4H9)4NOH, and H2O in the mole ratio 1:4:3.5:3:444 heated at 170°C for 47 h, to give brilliant blue plates in 70% yield. Crystal data for [H3N(CH2)3NH3] 0.5[Co(PO4)] · 0.5H2O (1): orthorhombic Cmc21, a = 22.663(3) Å, b = 7.6255(8) Å, c = 6.7676(7) Å, V = 1174.7(6) Å3, Z = 8, dcalc = 2.273 g cm-3; structure solution and refinement based on 507 reflections with I0 ≥ 3 σ (I0) (MoKα radiation, λ = 0.71073 Å) converged at R = 0.030. Crystal data for [H3N(CH2)4NH3] 0.5[Co(PO4)] (2): monoclinic P21/a, a = 7.508(3) Å, b = 23.655(4) Å, c = 6.775(1) Å, β = 90.55(2)°, V = 1203.3(5) Å3, Z = 8, dcalc = 2.185 g cm-3; structure solution and refinement based on 1305 reflections with I0 ≥ 3σ (I0) (MoKα, λ = 0.71073 Å) converged at R = 0.048. Magnetization measurements indicate that 2 orders to a weak ferromagnetic state near 25 K.

Original languageEnglish (US)
Pages (from-to)270-273
Number of pages4
JournalJournal of Solid State Chemistry
Volume125
Issue number2
DOIs
StatePublished - Sep 5 1996

ASJC Scopus subject areas

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

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