New lead triphosphonates: synthesis, properties and crystal structures

Abstract

Two new lead nitrilotris(methylene)triphosphonates, Pb[(H₂O₃PCH₂)N(CH₂PO₃H)₂] I and Pb₂[(O₃PCH₂)N(CH₂PO₃H)₂]·H₂O II, have been synthesised. I is triclinic, space group P1, a=8.5077(2), b=11.2363(3), c=5.9484(2) Å, α=98.802(2), β=104.955(1), γ=80.911(2)°, Z=2. II is monoclinic, space group Pn, a=7.3614(2), b=11.3889(2), c=7.2541(2) Å, β=100.389(2)° and Z=2. Their structures have been solved from laboratory X-ray data by using ab initio powder diffraction methodology. The reliability factors were R_wP=9.28%, R_P=7.20% and R_F=2.67%, for I, and R_wP=12.51%, R_P=9.38% and R_F=4.45%, for II. I shows a new layered structure which has small cavities, inside an inorganic layer, in which the hydrogen phosphonate and the dihydrogen phosphonate groups are located. II is also layered with the water molecule situated in the interlamellar space. Thermal data, IR data and ion-exchange properties are also reported and discussed. II dehydrates to yield orthorhombic Pb₂[(O₃PCH₂)N(CH₂PO₃H)₂] III. Hydrolysis of I leads to II.

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