Journal article

Publication year: 1998

Pages: 1526-1532

Journal: Journal of Inorganic and General Chemistry

Volume number: 624

Issue number: 9

ISSN: 0044-2313

Open access status: Bronze

Publisher: Wiley

Abstract: 
i) New compounds Ln(12.33)V(6)O(23)(OH)Cl-20 (Ln = La, Ce) were prepared by heating mixtures of LnCl(3), LnOCl and V2O5 (4:8:3) in evacuated, sealed silica ampoules (850 degrees C, 4 d). Single crystals could be obtained by chemical vapor transport (T-2-->T-1, T-2 = 900 degrees C, T-1 = 800 degrees C, 14d, p(Cl-2, 298K) approximate to 70 mbar). The single-crystal study of the lanthanum compound [a = 17.8818(25)Angstrom, c = 4.0567(7) Angstrom, Z = 1, 1035 independent I-0, 70 parameters, R1 = 3.52%] showed that vanadium has CN=4 (tetrahedrally) and lanthanum has CN = 9 (threefold capped trigonal prismatic). A strong relationship to the structures of the Pr3NbO4Cl6-and the La2TaO4Cl3-type could be discussed. ii) Further we obtained dark red powder of La3ReO6Cl3 by heating (740 degrees C, 5 d) a mixture of ReO3 and LaOCl (1:3) in sealed silica ampoules under argon atmosphere (p(Ar, 298K)= 1 atm). This new rhenium-compound crystallizes in the hexagonal space group P6(3)/m (No.176) [a = 9.4164(6) Angstrom, c = 5.4248(4) Angstrom] and is isostructural to La3WO6Cl3.