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Synthesis and Characterization of Homoleptic Rare Earth Nitrato Complexes with the Quarternary Ammonium Cations Et4N+ and nPr4N+

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Two periodic series of homoleptic rare earth nitrato complexes, [R 4 N] x [M(NO 3 ) y ]}(M = La-Nd, Sm-Lu, Y); R = Et, n Pr; x = 2-3; y = 5-6) have been synthesized, and characterized by single crystal X-ray diffraction, IR and Raman spectroscopy, comparing the solid state speciation of the nitrate ions as a function of lanthanide ion and quarternary ammonium cation. The series of the form [Et 4 N] 3 [M(NO 3 ) 6] } crystallizes in the rhombohedral space group R bar3, as a twelve-coordinate hexanitrato complex [Et 4 N] 3 [Ln(NO3) 6 ] with cocrystallized HNO 3  for La, Pr, and Nd. For Ce, a distinct orthorhombic phase retaining the same formula, [Et 4 N] 3 [Ce(NO3) 6 ]} is isolated in the absence of HNO 3  to prevent oxidation of the Ce(III) to Ce(IV) in nitric acid. A ten-coordinate pentanitrato complex, [Et 4 N] 2 [Ln(NO 3 ) 5 ]}, in monoclinic symmetry forms for the remainder of the series, and for Y(III). The entire series crystallized in the presence of n Pr 4 N] +  counterions forms a pentanitrato complex n Pr 4 N] 2 [M(NO 3 ) 5 ] in the orthorhombic space group, Pccn . Analysis of trends in the structural and spectroscopic characteristics of these series reveal insight into the structure-directing influences of both the lanthanide contraction and the quarternary ammonium cations.

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