A dipyrazol-bridged macrocyclic palladium(II) complex [{Pd(en)}4L4](NO3)8 (en=ethylenediamine, L=3,3′,5,5′-tetramethyldipyrazol) 1 was prepared in water through a macrocyclization of cis-(ethylenediamine)Pd(II) nitrate and the neutral form of the dipyrazol ligand 3,3′,5,5′-tetramethyldipyrazol. This cationic palladium macrocycle is highly distorted rather than a planar macrocycle and can hold eight nitrate anions around the macrocyclic framework through both hydrogen bonding and electrostatic interactions. CCDC: 192017.
A mononuclear complex, cis-1,10-phenanthroline-palladium(Ⅱ)(THF)2]dinitrate (THF = tetrahydrofuran) [Pd(C10H8N2)(C4H8O)2](NO3)2 1, has been prepared and structurally characterized by single-crystal X-ray diffraction. The crystal belongs to monoclinic system, space group P21/c with a = 7.881(1), b = 27.371(3), c = 10.178(1) ? ?= 103.313(3)? V = 2136.5(4) 3, Mr = 554.83, Dc = 1.725 g/cm3, Z = 4, F(000) = 1128 and (MoK) = 0.926 mm-1. The structure was refined to R = 0.0678 and wR = 0.1651 for 1687 observed reflections with I > 2(I). It is revealed that the central Pd(Ⅱ) ion in the title complex is bonded to two THF and two phenanthroline molecules in a cis-configuration to form the coordination geometry, deviating slightly from the square plane.
HUANG Hui YU Shu-Yan② (State Key Laboratory of Polymer Physics and Chemistry, Joint Laboratory of Polymer Science and Materials, Institute of Chemistry, The Chinese Academy of Sciences, Beijing 100080, China)
