Two Novel Organic Amine Templated Lanthanide Sulfates: Layer H3DETA · [Nd(H2O)(SO4)3] and Chain-Like H3DETA · [Ho(H2O)2(SO4)3]

摘要

Two novel organic amine templated lanthanide sulfates, layer (H3DETA)[Nd(H2O)(SO4)3] (I) and chain-like (H3DETA)[Ho(H2O)2(SO4)3] (II), are hydrothermally synthesized by using diethylenetriamine (DETA) as template, and are structurally characterized by ICP, elemental analysis, X-ray single-crystal diffraction, X-ray powder diffraction, IR, and TG. Compound I is monoclinic with space group P2_1 and data of unit cell: a = 6.6518(13),b= 10.373(2), c = 11.091(2) A, β = 93.61(3)°, V= 763.7(3) A~3, ρ_c= 2.421 g/cm~3, μ(MoK_α) = 3.885 mm , Z= 2, R1 = 0.0194 for 3312 reflections with F_o > 2σ(F_o). The Nd ions are nine-coordinated by one oxygen atom of coordinated water and eight oxygen atoms of sulfates. Compound I displays the layer structure constructed by linking Nd ions with three-linkage SO4 tetrahedra as the bridge (affording one coordinated vertex and toordinated edge). Compound II crystallizes in the monoclinic space group P2_1/c with unit cell data: a = 6.594(13) A, b = 14.783(3) A, c = 16.599(3) A, β = 93.47(3)°, V= 1614.2(6) A~3,ρ_c = 2.454 g/cm~3, μ(MoK_α) = 5.37 mm~(-1), Z=4,R1 = 0.0259 for 1815 reflections with F_o > 2σ(F_o). The Ho ions are eight-coordinated by two oxygen atoms of coordinated water and six oxygen atoms of sulfates. The straight chain-like structure of II is attained by alternatively arranging HoO8 polyhedra and two-linkage SO4 tetrahedra (affording two coordinated vertices). The TG results indicate that the two compounds experience three weight losses and lead to distinct residues: Nd9O3 for I and HoO(SO4)_(0.5) for II.