SYNTHESIS AND STRUCTURAL CHARACTERISTICS OF ANHYDROUS PRASEODYMIUM(III) PERCHLORATO AND TRIFLATO COMPLEXES

The syntheses of Pr(ClO4)(3), Pr(OTf)(3) (OTf = CF3SO3), Pr(ClO4)(3).Cl2O6, and NO2Pr(ClO4)(4) are described. Vibrational spec troscopy, X-ray powder diffraction, and EXAFS (for Pr(ClO4)(3)) are used to characterize the structure of the complexes. [ClO4] and [OTf] appear as tridentate in Pr(ClO4)(3)...

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Bibliographic Details
Published inCanadian journal of chemistry Vol. 72; no. 10; pp. 2044 - 2049
Main Authors PASCAL, JL, ELHADDAD, M, RIECK, H, FAVIER, F
Format Journal Article
LanguageFrench
Published OTTAWA Natl Research Council Canada 01.10.1994
Subjects
Chemistry
Chemistry, Multidisciplinary
Physical Sciences
Science & Technology
NITRATES
PHASE
CL2O6
SPECTROSCOPY
RARE-EARTH
REACTIVITY
METAL PERCHLORATES
CHLORINE TRIOXIDE
EXAFS
LANTHANIDE TRIFLUOROMETHANESULFONATES
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Summary:The syntheses of Pr(ClO4)(3), Pr(OTf)(3) (OTf = CF3SO3), Pr(ClO4)(3).Cl2O6, and NO2Pr(ClO4)(4) are described. Vibrational spec troscopy, X-ray powder diffraction, and EXAFS (for Pr(ClO4)(3)) are used to characterize the structure of the complexes. [ClO4] and [OTf] appear as tridentate in Pr(ClO4)(3) and Pr(OTf)(3) and Pr is 9-coordinated. In Pr(ClO4)(3).Cl2O6, chlorine trioxide is included in the lattice of Pr(ClO4)(3) and shows the ionic <-> covalent equilibrium. In NO2Pr(ClO4)(4), Pr(ClO4)(4)(-) retains the structure of Pr(ClO4)(3), the extra [ClO4] is weakly bonded to Pr. Pr(ClO4)(3) crystallizes in the monoclinic system (P2(1)/m), a = 8.608; b = 11.827; c = 7.416 Angstrom; beta = 106.29 degrees, and V = 724.79 Angstrom(3). Distances Pr-O = 2.51 Angstrom and Pr-Cl 3.90 Angstrom are determined by EXAFS. Strong fluorescence phenomena are observed when Pr(ClO4)(3) is excited with the 488 nm line of an ionized Ar laser.
ISSN:0008-4042
DOI:10.1139/v94-261