Synthesis, structure and thermal transformations of aluminophosphates containing the nickel complex [Ni(diethylenetriamine)₂]²⁺ as a structure directing agent

[Ni(diethylenetriamine)(2)](2+), (Ni(deta)(2)), acts as a structure directing agent for aluminophosphates and metalloaluminophosphates with the CHA and AFI framework topologies.. In the presence of ammonium fluoride, triclinic Ni(deta)(2)-UT-6; P 1, a = 9.289(l) Angstrom, b = 9.095(l) Angstrom, c = 9.356(l) Angstrom, alpha = 88.35(1)degrees, beta = 78.91 (1)degrees, gamma = 89.21(1)degrees, with the CHA topology and orthorhombic Ni(deta)(2)-AlPO(F)-5; Ccc2, a = 13.8603(5) Angstrom , b = 23.1285(5) Angstrom, c = 8.5420(4)degrees Angstrom with the AFI topology and prepared, the latter being favoured by higher water contents in the synthesis gel. Upon heating in nitrogen or oxygen at temperatures of 500 degreesC and above, Ni(deta)(2)-UT-6 is transformed reconstructively to an aluminophosphate with the AFI topology whereas heating at lower temperatures followed by heating in oxygen at 600 degreesC removes the organic and gives a solid with the CHA topology. Calcination of all samples prepared in the absence of fluoride leaves the original frameworks intact. Ni K-edge X-ray spectroscopy of Ni(deta)(2)-UT-6 calcined in oxygen at 600 degreesC reveals the formation of nanoparticulate NiO. (C) 2002 Elsevier Science Inc. All rights reserved.