Structure D 2000
04- 002
DOI: 10.1002/chin.201604002 Synthesis and Crystal Structure of Mixed Metal(III) Tungstenyl(VI) ortho-Pyrophosphates. — MIII (W VIO2)2(P2O7)(PO 4) (M: Sc, V, Cr, Fe, Mo, Ru, Rh, In, Ir) are obtained via vapor phase moderated solid state reactions of P4O10, WV OPO4, -VOPO4, and trivalent transition metal phosphates using PtCl2 as mineralizer and Cl 2 source (evacuated silica tubes, 1. 500 C, 2 d, 2. 800-950 C). The compounds with M: V, Ru, and Rh all crystallize in the monoclinic space group C2/c (Z = 16, single crystal XRD) and contain fairly regular MO6 and distorted WO6 octahedra which share vertices with PO4 and P2O7 units to form a 3D network. Magnetic measurements confirm the oxidation state of M in the ortho-pyrophosphates with M: V3+, Cr 3+, and Fe3+. 31 P-MAS-NMR spectra of the diamagnetic phosphates with M: Sc, In, and Ir show surprisingly different isotropic chemical shifts for the seven P sites. The scandium compound shows a fully inverted occupancy of the M sites according to the formulation W(Sc1/2W1/2O2)2(P2O7 )(PO4). — (ROY, S. C.; RAGUZ, B.; ASSENMACHER, W.; GLAUM*, R.; Solid State Sci. 49 (2015) 18-28, http://dx.doi.org/10.1016/j.solidstatesciences.2015.09.006 ; Inst. Anorg. Chem., Rhein. Friedrich-Wilhelms-Univ., D-53121 Bonn, Germany; Eng.) — J. Schramke
ChemInform 2016, 47, issue 04
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