caa a22 4500 378912569 CHVBK 20180305123545.0 cr unu---uuuuu 161128e20041201xx s 000 0 eng 10.1524/zkri.219.12.881.55867 doi (NATIONALLICENCE)gruyter-10.1524/zkri.219.12.881.55867 Structure determination of thermal decomposition products from laboratory X-ray powder diffraction [Elektronische Daten] [Thierry Bataille, Nathalie Audebrand, Ali Boultif, Daniel Louër] Ab initio structure determination from powder diffraction data of compounds resulting from solid state transformations is still rather limited. Two major factors influence the stages of the structure elucidation of these solids, i.e. the lower precision in peak position for indexing and the strong line overlap for extracting integrated intensities. The present study deals with the consideration of these two problems for solving the crystal structure of two thermal-decomposition inorganic products, Nd(NO3)3 · 4 H2O and Pb3O2(NO3)2. The new features of DICVOL04, as zero shift refinement, a priori zero search and tolerance of spurious lines have been used for indexing several phases obtained during the thermal treatment of neodymium nitrate hexahydrate. The crystal structures of Nd(NO3)3 · 4 H2O and Pb3O2(NO3)2 have been solved with the direct methods and the structure model of Pb3O2(NO3)2 has been completed using a global optimisation approach. The monoclinic structure of neodymium nitrate tetrahydrate [a = 10.1744(4) Å, b = 8.9716(5) Å, c = 11.7295(5) Å, β = 97.384(4)°, V = 1061.80 Å3, S.G. P21/c] is built from isolated ten-fold coordinated Nd polyhedra. The orthorhombic structure of lead oxide nitrate [a = 7.6034(4) Å, b = 5.7691(4) Å, c = 18.5817(9) Å, V = 815.09 Å3, S.G. Pnma] is built from double chains of edge-sharing OPb4 tetrahedra connected by nitrate groups. In order to estimate the chance of solving crystal structure of nanocrystalline powdered compounds, a comparison of the efficiency of direct methods and direct-space approaches is made from powder diffraction patterns simulated for various crystallite sizes from the crystal structure of the decomposition product γ-Zn2P2O7. © 2004 Oldenbourg Wissenschaftsverlag GmbH Crystallography nationallicence Inorganic chemistry nationallicence Organic chemistry nationallicence Bataille Thierry aut Audebrand Nathalie aut Boultif Ali aut Louër Daniel aut Zeitschrift für Kristallographie - Crystalline Materials De Gruyter Oldenbourg 219/12(2004-12-01), 881-891 2194-4946 219:12<881 2004 219 zkri https://doi.org/10.1524/zkri.219.12.881.55867 text/html Onlinezugriff via DOI 1 research article jats NATIONALLICENCE 856 40 https://doi.org/10.1524/zkri.219.12.881.55867 text/html Onlinezugriff via DOI NATIONALLICENCE 700 1- Bataille Thierry aut NATIONALLICENCE 700 1- Audebrand Nathalie aut NATIONALLICENCE 700 1- Boultif Ali aut NATIONALLICENCE 700 1- Louër Daniel aut NATIONALLICENCE 773 0- Zeitschrift für Kristallographie - Crystalline Materials De Gruyter Oldenbourg 219/12(2004-12-01), 881-891 2194-4946 219:12<881 2004 219 zkri CC0 http://creativecommons.org/publicdomain/zero/1.0 nationallicence BK010053 XK010053 XK010000 NATIONALLICENCE NATIONALLICENCE NL-gruyter