Study on syntheses and structures of nine-coordinated mononuclear K[Tb~(III)(edta) (H_2O)_3] 5 H_2O and binuclear K_4[Tb~(III)_2(Httha)_2] 14 H_2O complexes

摘要

The crystal and molecular structures of the K[Tb~(III)(edta)(H_2O)_3].5 H_2O (edta = ethylenediaminetetraacetic acid) and K_4[Tb~(III)_2(Httha)_2].14 H_2O (ttha = triethylenetetraminehexaacetic acid) complexes have been determined by single-crystal X-ray diffraction analyses. The crystal of the K[Tb~(III)(edta)(H_2O)_3].5 H_2O complex belongs to orthorhombic crystal system and Fdd 2 space group. The crystal data are as follows: a = 1.9373(5) nm, b = 3.5429(10) nm, c = 1.2114(3) nm, V 8.315(4) nm~3, Z= 16, M= 630.35, Dc = 2.014 g cm~(-3), m = 3.683 mm~(-1) and F(000) = 5024. The final Rand wR values are 0.0224 and 0.0557 for 3189 [I> 2.0 sigma(I)] unique reflections, and 0.0245 and 0.0567 for all 8206 reflections, respectively. The [Tb~(III)(edta)(H_2O)_3]~- complex anion has a nine-coordinated pseudo-monocapped square antiprismatic structure in which the nine coordinate atoms, two N and seven O come from one edta ligand and three water molecules. The crystal of the K_4[Tb~(III)_2(Httha)_2].14 H_2O complex belongs to monoclinic system and P 2(1) space group. The crystal data are as follows: a = 1.1326(3) nm, b = 2.5675(7) nm, C =2.2076(6) nm, bate = 102.943(5) centre dot, V =6.256(3) nm~3, Z = 4, M = 1705.26, Dc = 1.802 g cm~(-3), m = 2.611 mm~(-1) and F(000) = 3424. The final R and wR are 0.0339 and 0.0667 for 10699 [I>2.0 sigma (I)] unique reflections, and 0.0543 and 0.0741 for all 22190 reflections, respectively. The total complex molecule is composed of two close parts in structure.