Synthesis and characterization of metal carboxyalkylphosphonates hybrid materials
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Several carboxyalkylphosphonate hybrid materials have been prepared under hydrothermal conditions: Mn2(OH)(O3PCH2CO 2)1/2H2O, Mn2(OH)(O3PCH 2CO2), Al3(OH)3(O 3PCH2CH2CO2)2 3H2O, Pb5(O3PCH2CH 2CO2)2(O3PCH2CH 2COOH)2 and Pb3(O3PCH 2CH2CO2)2. The influence of some variables in the syntheses such as pH or metal/phosphonic acid molar ratios have been examined. Mn2(OH)(O3PCH2CO 2)1/2H2O crystallizes in a triclinic cell with parameters a=8.405 , b=8.789 , c=4.910 , =90.71, =98.58, =103.68and V=348.6 3. Its dehydration lead to Mn2(OH)(O 3PCH2CO2), which unit cell has also been determined: a=8.307 , b=8.322 , c=4.940 , =103.31, =98.81, =80.79and V=325.6 3. The diffraction data suggest a layered structure. Al 3(OH)3(O3PCH2CH2CO 2)23H2O crystallizes in a monoclinic unit cell with a=10.534 , b=7.880 , c=10.320 , =109.86and V=805.7 3. Its X-ray powder pattern and the spectroscopic data are consistent with a pillared layered structure. Finally, Pb5(O3PCH2CH2CO 2)2(O3PCH2CH2COOH) 2 is monoclinic with a=11.889(1) , b=12.746(1) , c=9.835(1) , =114.081(2), V=1360.6(2) 3, Z=2, space group P21/c. Its structure has been solved from single crystal data, R1=0.069, and shows a pillared layered framework. There are two types of carboxyethylphosphonate chains, one being protonated which is pillaring the layers and the other chain is twisted and bonded to a unique inorganic layer through both carboxylate and phosphonate moieties. Thermal and IR data for these compounds are reported and discussed. 2004 Elsevier SAS. All rights reserved.