Synthesis and Structural Characterization of Cu(pic)2CO(NH2)22 and (picH2)2Cu(pic)2(SCN)2

摘要

Two new compounds Cu(pic)2[CO(NH2)2]2 1 and (picH2)2[Cu(pic)2(SCN)2] 2 were prepared from the reaction of picolinic acid and copper(Ⅱ) per-chlorate by using carbamide to adjust pH=4 in the preparation of compound 1 and KSCN to adjust pH=6 in the preparation of 2. Crystal data for 1: monoclinic system, space group P21 with a=7.441(1), b=14.291(2), c=7.790(1) A, β=95.855(2)°, V=824.0(2) A3, Dc=1.724 g/cm3, F(000)=438, C14H16N606Cu, Mr=427.87,μ(MoKα)=1.375 mm-1, Z=2 and the final R=0.0365 for 1164 observed reflections. Crystal data for 2: monoclinic system, space group P21/c with a=9.8237(3), b=10.0409(3), c=14.5867(2) A, β -= 104.190(2), V=1394.91(6) A3, Dc= 1.595 g/cm3, F(000)=686, C26H20N6O8S2Cu, Mr=672.14,μ(MoKα)=0.994 mm-1, Z=2 and the final R=0.0442 for .1651 observed reflections. The Cu(Ⅱ)atom in both 1 and 2 has a 4+2 elongated octahedral environment with the pic- ligands locating on the equatorial plane, and carbamide and SCN- occupying the axial sites, respectively. In compound 2,there also exist two protonated picolinate cations for charge balance.