F-Element/crown ether complexes III: Synthesis and structural characterization of [Y(NO 3) 2(OH 2) 5][NO 3]·2(15- crown-5)

Abstract

[Y(NO 3) 2(OH 2) 5][NO 3]·2(15- crown-5) was prepared by the addition of 15- crown-5, dissolved in a 1:3 solution of CH 3OH:CH 3CN, to a solution of Y(NO 3) 3·nH 2O in the same solvent mixture. The crystal and molecular structures of the title compound were determined by single-crystal X-ray diffraction using counter methods with crystals obtained by slowly cooling the reaction mixture. The complex is monoclinic, P2 1 c , with unit cell data a = 12.399(8) A ̊ , b = 10.488(4) A ̊ , c = 27.248(9) A ̊ , β = 91.47(5)° and D calc = 1.51g cm −3 for Z = 4 formula units. The structure was refined to a conventional R value of 0.107 using 2930 observed reflections [ I ⩾ 3 σ(I)]. High thermal motion and disorder were encountered when refining the two crownether molecules and the uncoordinated nitrate group. The yttrium atom is ninecoordinate with two bidentate nitrate groups (Y-O average length, 2.44(6) Å) and five-coordinated water molecules (Y-O average length, 2.36(3) Å).