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Crystal Structure and Formation of TlPd 3 and its new Hydride TlPd 3 H
Author(s) -
Kurtzemann Nadine,
Kohlmann Holger
Publication year - 2010
Publication title -
zeitschrift für anorganische und allgemeine chemie
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.354
H-Index - 66
eISSN - 1521-3749
pISSN - 0044-2313
DOI - 10.1002/zaac.201000012
Subject(s) - hydride , chemistry , crystal structure , hydrogen , hydrogen storage , tetragonal crystal system , crystallography , organic chemistry
TlPd 3 was synthesised from the elements in evacuated silica tubes at 600 °C. Alternatively, TlPd 3 was yielded by reduction of TlPd 3 O 4 in N 2 gas atmosphere. Reduction of the oxide in H 2 gas atmosphere resulted in the formation of the new hydride TlPd 3 H. The structure of tetragonal TlPd 3 (ZrAl 3 type, space group I 4/ mmm , a = 410.659(9) pm, c = 1530.28(4) pm) was reinvestigated by X‐ray and also by neutron powder diffraction as well as the structure of its previously unknown hydride TlPd 3 H (cubic anti ‐perovskite type structure, space group Pm \bar{3} m , a = 406.313(1) pm). In situ DSC measurements of TlPd 3 in hydrogen gas atmosphere showed a broad exothermic signal over a wide temperature range with two maxima at 280 °C and at 370 °C, which resulted in the product TlPd 3 H. A dependency of lattice parameters of the intermetallic phase on reaction conditions is observed and discussed. Results of hydrogenation experiments at room temperature with gas pressures up to 280 bar hydrogen and at elevated temperatures with very low hydrogen gas pressures (1–2 bar) as well as results of dehydrogenation of the hydrides under vacuum will be discussed.