Pb2PdO2(OH)2 and Pb2PdO(OH)4(H2O): Synthesis and crystal growth at ambient conditions

Komarek AC, Merz P, Guo H, Suard E, Chen JM, Felser C, Jansen M (2015)

Publication Type: Journal article

Publication year: 2015

Journal

Zeitschrift für Anorganische und Allgemeine Chemie Wiley

Book Volume: 641

Pages Range: 1473-1479

Journal Issue: 8-9

DOI: 10.1002/zaac.201500217

Abstract

New Pb2PdO2(OH)2 and Pb2PdO(OH)4(H2O) were synthesized at ambient conditions from respective KOH alkaline and metal nitrate aqueous feed stocks in high purity and as coarse crystals. The constitutions of the two lead palladates were determined by combined powder neutron and single-crystal X-ray diffraction studies. Both crystal structures exhibit a distinct pseudo symmetry, and settling the true lattice symmetry [Pb2PdO2(OH)2: a = 5.9512(3) Å, b = 5.9479(3) Å, c = 7.9480(2) Å, α = 90.256(4)°, β = 90.392(4)°, γ = 119.694(1)°; Pb2PdO(OH)4(H2O): a = 10.706(2) Å, b = 10.32(1) Å, c = 5.7813(3) Å, α = β = γ = 90°] required to employ high resolution synchrotron powder diffraction data. The combined use of neutron and X-ray diffraction measurement has enabled solving the crystal structure of Pb2PdO2(OH)2 including hydrogen positions. For Pb2PdO(OH)4(H2O) only a high symmetry, heavy atoms (Pb, Pd, O) average structure was determined, since the background in the neutron data was strongly enhanced due to the high amount of incoherently scattering hydrogen atoms and considerable disorder present. The crystal structures feature unprecedent connectivities, however, as expected square-planar coordination of palladium(II) and typical crooked surroundings of lead(II) with the 6s² lone pair acting as a virtual ligand.

Involved external institutions

Max-Planck-Institut für Chemische Physik fester Stoffe (MPI CPfS) / Max Planck Institute for Chemical Physics of Solids

Germany (DE) Institute Laue-Langevin (ILL)

France (FR) National Synchrotron Radiation Research Center (NSRRC)

Taiwan (TW)

How to cite

APA:

Komarek, A.C., Merz, P., Guo, H., Suard, E., Chen, J.-M., Felser, C., & Jansen, M. (2015). Pb2PdO2(OH)2 and Pb2PdO(OH)4(H2O): Synthesis and crystal growth at ambient conditions. Zeitschrift für Anorganische und Allgemeine Chemie, 641(8-9), 1473-1479. https://doi.org/10.1002/zaac.201500217

MLA:

Komarek, Alexander Christoph, et al. "Pb2PdO2(OH)2 and Pb2PdO(OH)4(H2O): Synthesis and crystal growth at ambient conditions." Zeitschrift für Anorganische und Allgemeine Chemie 641.8-9 (2015): 1473-1479.

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