Synthesis and Structures of Nine-Coordinate K[Dy(Edta)(H2O)3] • 3.5H2O, (NH4)3[Dy(Ttha)] • 5H2O, and Eight-Coordinate NH4[Dy(Cydta)(H2O)2] • 4.5H2O Complexes

The title complexes, K[Dy(Edta)(H2O)(3)] center dot 3.5H(2)O (I) (H(4)Edta = ethylenediamine-N,N,N',N'-tetraacetic acid), (NH4)(3)[Dy(Ttha)] center dot 5H(2)O (II) (H(6)Ttha = triethylenetetramine-N,N,N',N '',N''',N'''-hexaacetic acid), and NH4[Dy(Cydta)(H2O)(2)] center dot 4.5H(2)O (III) (H(4)Cydta = trans-1,2-cyclohexanediamine-N,N,N',N'-tetraacetic acid), were prepared, and their compositions and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques, respectively. In complex I, the Dy3+ ion is nine-coordinated by an Edta ligand and three water molecules, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the orthorhombic crystal system with space group Fdd2. The crystal data are as follows: a = 19.751(7), b = 35.573(12), c = 12.227(4) angstrom, V = 8591(5) angstrom(3), Z = 16, space group Fdd2 rho(c) = 1.877 g/cm(3), mu = 3.742 mm(-1), F(000) = 4800, R = 0.0259, and wR = 0.0616 for 3218 observed reflections with I >= 2 sigma(I). For complex II, the Dy3+ ion is nine-coordinated by a Ttha ligand, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the monoclinic crystal system with space group P2(1)/c. In addition, there is a free non-coordinate carboxyl group (-CH2COO-) in the [Dy(Ttha)](3-) complex anion. The crystal data are as follows: a = 10.353(3), b = 12.746(4), c = 23.141(7) angstrom, beta = 91.005(5)degrees, V = 3053.2(15) angstrom(3), Z = 4, space group P2(1)/c rho(c) = 1.730 g/cm(3), mu = 2.532 mm(-1), F(000) = 1620, R = 0.0332 and wR = 0.0924 for 5390 observed reflections with I >= 2 sigma(I). For complex III, the Dy3+ ion is eight-coordinated by a ligand Cydta and two water molecules, yielding a distorted square antiprismatic conformation, and the complex crystallizes in the triclinic system with space group P (1) over bar. The crystal data are as follows: a = 8.604(3), b = 10.012(4), c = 14.369(6) angstrom, alpha = 88.330(6)degrees, beta = 75.363(6)degrees, gamma = 88.285(6)degrees, space group P (1) over bar V = 1196.9(8) angstrom(3), Z = 2, rho(c) = 1.776 g/cm(3), mu = 3.194 mm(-1), F(000) = 644, R = 0.0445 and wR = 0.1041 for 3931 observed reflections with I >= 2 sigma(I).