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Perchlorato Complexes of Rare‐Earth Elements: Syntheses and Crystal Structures of Lu(ClO 4 ) 3 · 3 H 2 O, Er(ClO 4 ) 3 · H 2 O, and Sc(OH)(ClO 4 ) 2 · H 2 O
Author(s) -
Wickleder Mathias S.
Publication year - 1999
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/(sici)1521-3749(199909)625:9<1556::aid-zaac1556>3.0.co;2-k
Subject(s) - triclinic crystal system , monoclinic crystal system , crystallography , chemistry , octahedron , molecule , crystal structure , perchlorate , hydrogen bond , stereochemistry , ion , organic chemistry
Single crystals of Lu(ClO 4 ) 3 · 3 H 2 O were obtained by slow dehydration of Lu(ClO 4 ) 3 · 6 H 2 O at 140 °C under flowing argon. The compound crystallizes in the triclinic crystal system (P1, Z = 2, a = 750.3(1), b = 838.4(1), c = 1054.6(2) pm, α = 79.77(2)°, β = 79.18(2), γ = 63.83(2), R all = 0.0426) with Lu 3+ eightfold coordinated by oxygen atoms, which belong to five ClO 4 – groups and three H 2 O molecules. The [LuO 8 ] polyhedra and ClO 4 – groups are connected to form chains which are held together only via hydrogen bridges. Er(ClO 4 ) 3 · H 2 O can also be prepared by dehydration of the respective hexahydrate but only at higher temperature and under vacuum. The triclinic compound (P1, Z = 2, a = 678.31(9), b = 783.4(1), c = 955.9(1) pm, α = 77.29(1)°, β = 75.71(1)°, γ = 78.31(1)°, R all = 0.0292) contains Er 3+ ions which are coordinated by seven ClO 4 – groups and one H 2 O molecule. The linkage of the [ErO 8 ] polyhedra and ClO 4 – tetrahedra results in a three‐dimensional network. Attempts to dehydrate Sc(ClO 4 ) 3 · 6 H 2 O led to the basic perchlorate Sc(OH)(ClO 4 ) 2 · H 2 O. In the monoclinic structure (P2 1 /n, Z = 4, a = 942.8(1), b = 735.16(8), c = 1157.9(2) pm, β = 93.76(2)°, R all = 0.0579), Sc 3+ is surrounded by six oxygen atoms which belong to three ClO 4 – ions, two OH – groups and one H 2 O molecule. These octahedra are connected via common edges which are formed by the OH – groups to pairs according to [Sc 2 (OH) 2 (ClO 4 ) 6 (H 2 O) 2 ] 2– . Four of the six ClO 4 – groups link the pairs to two‐dimensional infinite sheets, which are held together via hydrogen bonds.