The layered amorphous and crystalline samples of zirconium [N-(phosphonomethyl)morpholine-phosphate] Zr(HPO4)[O3PCH2N(CH2CH2)(2)O].nH(2)O (1a, 2a), zirconium [N-(phosphonomethyl)iminodiacetic acid-phosphate] Zr(HPO4)[O3PCH2N(CH2CO2H)(2)].nH(2)O (1b, 2b) and zirconium [N,N-di(phosphonomethyl) acetic acid] Zr[(O3PCH2)(2)NCH2CO2H].nH(2)O (1c, 2c) were synthesized for the first time with zirconium oxychloride, sodium dihydrogen phosphate and H2O3PCH2N(CH2CH2)(2)O, H2O3PCH2N(CH2CO2H)(2) or (H2O3PCH2)(2)NCH2CO2H in the absence and presence of hydrofluoric acid. The samples were comparatively characterized by XRD, IR, TG and elemental analysis. XRD data showed that the crystalline samples 2a, 2b and 2c are highly crystalline with interlayer spacings of 1.606, 1.538 and 1.239 nm, respectively. The amorphous and crystalline samples lost nearly the weight calculated for their organic component over the same broad temperature range of 172-664, 184-680 and 176-668 degreesC, respectively. XPS data indicated that the coordination bonds formed between nitrogen and palladium in the palladium complexes. Their palladium complexes possessed good activities for the hydrogenation of the carbon-carbon double bond. The catalytic activities of the palladium complexes of amorphous 1a, 1b and 1c is 1.5-3.1 times as high as that of the palladium complexes of crystalline 2a, 2b and 2c. (C) 2003 Elsevier B.V. All rights reserved.