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Beiträge zur Kristallchemie und zum thermischen Verhalten von wasserfreien Phosphaten. XXXVI [1] Synthese, Kristallstruktur und spektroskopische Charakterisierung von Palladium(II)‐diphosphat Pd 2 P 2 O 7
Author(s) -
Panagiotidis K.,
Glaum R.,
Schmedt auf der Günne J.,
Hoffbauer W.,
Görzel H.
Publication year - 2005
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.200500208
Subject(s) - palladium , crystal structure , chemistry , raman spectroscopy , crystallography , context (archaeology) , physics , catalysis , paleontology , optics , biology , biochemistry
Synthesis, Crystal Structure and Spectroscopical Characterization of Palladium(II)‐Diphosphate Pd 2 P 2 O 7 Pd 2 P 2 O 7 is synthesized by heating (T max = 500 °C) stoichiometric amounts of PdO and phosphoric acid. Using chemical vapour transport experiments (850 °C → 750 °C, addition of PdCl 2 ) Pd 2 P 2 O 7 was crystallized. Pd 2 P 2 O 7 adopts its own structure type (C 2/c (No. 15), Z = 4, a = 13,151(2) Å, b = 5,172(1) Å, c = 8,139(1) Å, β = 97,52(1)°, 1160 independent reflections, 55 variables, R1 = 0,021 and wR2 = 0,050). Square‐planar [PdO 4 ]‐units $({\bar d}\rm (Pd-O)=2,020 \AA)$ are linked by diphosphate‐groups generating a 3D framework. Within this framework ribbons $^{1}_{\infty}\rm[Pd(P_{2}O_{7})]^{2-}$ may be distinguished. Thus Pd 2 P 2 O 7 might be described as palladium(II)‐[diphosphatopalladate(II)]. The results of various spectroscopic measurements (IR, Raman, UV/VIS, 31 P‐MAS‐NMR) are reported and discussed within the context of the crystal structure.