Synthesis and X-ray Powder Structure of a New Pillared Layered Cadmium Phosphonate, Giving Evidence that the Intercalation of Alkylamines into Cd(O(3)PR).H(2)O Is Topotactic.
A new pillared layered phosphonate, cadmium 2-aminoethylphosphonate, Cd(O(3)PC(2)H(4)NH(2)) (1), has been synthesized, and its structure was solved ab initio from X-ray powder diffraction data and refined by Rietveld methods. Compound 1 is orthorhombic: space group Pna2(1), a = 15.4643(2) Å, b = 5.16512(7) Å, c = 6.27650(8) Å, and Z = 4. Its layer arrangement is similar to that in Cd(O(3)PR).H(2)O, except that the water molecule coordinated to cadmium in Cd(O(3)PR).H(2)O is replaced by the nitrogen atom from the amino ends of the ethyl chains borne by phosphorus of the upper and lower layers. The strong similarity of the IR, (31)P, and (113)Cd NMR data for Cd(O(3)PC(2)H(4)NH(2)) and Cd(O(3)PCH(3)).n-NH(2)C(4)H(9) clearly shows the topotactic character of the intercalation of n-alkylamines in the dehydrated form of Cd(O(3)PR).H(2)O to yield Cd(O(3)PR).n-NH(2)R'.
Fredoueil
Florence
F
Laboratoire de Synthèse Organique, UMR CNRS 6513, BP 92208, 2 Rue de la Houssinière 44322 Nantes Cedex 03, France, Centre de Recherche sur les Matériaux à Haute Température, UPR CNRS 4212, 1D Avenue de la Recherche Scientifique, 45071 Orléans Cedex 02, France, Department of Chemistry, Texas A&M University, College Station, Texas 77843, and Institut des Matériaux de Nantes, UMR CNRS 6502, BP 92208, 2 Rue de la Houssinière 44322 Nantes Cedex 03, France.
Massiot
Dominique
D
Janvier
Pascal
P
Gingl
Franz
F
Bujoli-Doeuff
Martine
M
Evain
Michel
M
Clearfield
Abraham
A
Bujoli
Bruno
B