Utilizing mononuclear complex Ni(2-mpac)2(H2O)2 as the molecular building block,a novel coordination polymer [Ni2(2-mpac)4(4,4'-bpy)·2H2O]n(1,2-mpac = 5-methyl-2-pyrazinecar-boxylic acid,4,4'-bpy = 4,4'-bipyridine) was successfully synthesized and structurally characterized by X-ray single-crystal diffraction method.Crystal data:monoclinic,space group C2/c,a = 23.870(1),b = 9.887(4),c = 18.929(9) ,β = 126.840(5)°,V = 3575(3) 3,Z = 4,S = 1.046,μ = 1.594 mm-1,F(000) = 1768 and Dc = 1.127 g·cm-3.The final R = 0.0351 and wR = 0.0792 for 2372 observed reflections with Ⅰ 〉 2σ(Ⅰ) and R = 0.0564 and wR = 0.0938 for all reflections.
Four solid complexes of Ln(Me2dtc)3(phen) (Ln=Eu, Gd, Tb, Dy) were synthesized in anhydrous ethanol by the reaction of lanthanide chloride low hydrate with the mixed ligands of sodium dimethyldithiocarbamate and 1, 10-phenanthroline·H2O (abbreviated as phen·H2O), and characterized by elemental analysis, IR spectroscopy, TG-DTG and X-ray diffraction techniques. Combining with the crystal structures, the complexes are identified as the general formula of Ln(Me2dtc)3(phen). TG-DTG with X-ray powder diffraction showed that these compounds could decompose to lanthanide sulfides under relatively lower temperature, which indicated that the title complexes could be ideal precursors to prepare lanthanide sulfides.