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Synthesis and Crystal Structure of the Iron(III) Oxotellurate(IV) Phosphate Oxide Chloride Fe 11 (TeO 3 ) 2 (TeO 4 ) 3 (PO 4 ) 2 O 4 Cl 3
Author(s) -
Zimmermann Iwan,
Johnsson Mats
Publication year - 2014
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.201400349
Subject(s) - lone pair , monoclinic crystal system , crystallography , valence (chemistry) , chloride , chemistry , covalent bond , ion , crystal structure , space group , counterion , inorganic chemistry , x ray crystallography , molecule , physics , organic chemistry , diffraction , optics
The new compound Fe 11 (TeO 3 ) 2 (TeO 4 ) 3 (PO 4 ) 2 O 4 Cl 3 containing Fe III and Te IV crystallizes in the monoclinic space group C 2/ c with the unit cell parameters a = 20.5816(5) Å, b = 26.7506(6) Å, c = 5.03910(10) Å, β = 93.587(2) o , Z = 4. Single crystals were grown in sealed and evacuated silica tubes at 550 °C. The compound exhibits an open framework structure built from [FeO 6 ], [FeO 5 Cl], [FeO 4 Cl], [PO 4 ], [TeO 3 ], and [TeO 4 ] polyhedra. The Te IV atoms adopt a one sided asymmetric coordination due to the stereochemically active lone‐pair. The lone‐pairs together with the chloride ions are excluded from the covalently bonded space and protrude into cavities extending along [001]. Bond valence sum calculations confirm iron to be in its Fe III state and the chloride ions to be underbonded and act more as counterions than being fully integrated in the covalent network.