摘要
A 3D infinitely extended structural rare earth coordination compound with a formula of K3{[Sm(H2O)7]2Na[a-SiW11O39Sm(H2O)4]2}·14H2O has been synthesized by reaction of Sm2O3,HClO4,NaOH with a-K8SiW11O39·nH2O,and characterized by IR,UV spectra,ICP,TG-DTA,cyclic voltammetry,variable-temperature magnetic susceptibility and X-ray single-crystal diffrac-tion.X-ray single-crystal diffraction indicates that the title compound crystallizes in a triclinic lat-tice,Pi space group,with a = 1.2462(3) nm,b = 1.2652(3) nm,c = 1.8420(4) nm,α = 87.45(3)°,β = 79.91(3)°,γ = 82.57(3)°,Z = 1,R1 = 0.0778,wR2 = 0.1610.Structural analysis reveals that Sm3+(1) coordination cation has incorporated into the vacant site of [α-SiW11O39]8? entity,forming the [α-SiW11O39Sm(H2O)4]5? subunit.The two adjacent [a-SiW11O39Sm(H2O)4]5? subunits are combined with each other through two Sm(1)-O-W bridges accompanying the formation of dim-mer structural unit [α-SiW11O39Sm(H2O)4]210? of the title compound.The neighboring dimmer structural units [α-SiW11O39Sm(H2O)4]210? are linked to form the 1D chainlike structure by means of two Sm3+(2) and a Na+(1) coordination cations.The K+(1) cations connect the 1D packing chains constructing the 2D netlike structure,and adjacent netlike layers are also grafted by K+(2) cations to build the novel 3D infinitely extended structure.The result of TG-DTA curves manifests that the decomposition temperature of the title polyanionic framework is 554℃.The cyclic volt-ammetry measurements show that the title polyanion has the two-step redox processes in aqueous solution with pH = 3.1.Variable temperature magnetic susceptibility indicates the title compound obeys the Cruie-Weiss Law in the higher temperature range from 110 to 300 K,while in the lower temperature range from 2 to 110 K the comparatively strong antiferromagnetism in-teractions can be observed.
A 3D infinitely extended structural rare earth coordination compound with a formula of K3{[Sm(H2O)7]2Na[a-SiW11O39Sm(H2O)4]2}·14H2O has been synthesized by reaction of Sm2O3,HClO4,NaOH with a-K8SiW11O39·nH2O,and characterized by IR,UV spectra,ICP,TG-DTA,cyclic voltammetry,variable-temperature magnetic susceptibility and X-ray single-crystal diffrac-tion.X-ray single-crystal diffraction indicates that the title compound crystallizes in a triclinic lat-tice,Pi space group,with a = 1.2462(3) nm,b = 1.2652(3) nm,c = 1.8420(4) nm,α = 87.45(3)°,β = 79.91(3)°,γ = 82.57(3)°,Z = 1,R1 = 0.0778,wR2 = 0.1610.Structural analysis reveals that Sm3+(1) coordination cation has incorporated into the vacant site of [α-SiW11O39]8? entity,forming the [α-SiW11O39Sm(H2O)4]5? subunit.The two adjacent [a-SiW11O39Sm(H2O)4]5? subunits are combined with each other through two Sm(1)-O-W bridges accompanying the formation of dim-mer structural unit [α-SiW11O39Sm(H2O)4]210? of the title compound.The neighboring dimmer structural units [α-SiW11O39Sm(H2O)4]210? are linked to form the 1D chainlike structure by means of two Sm3+(2) and a Na+(1) coordination cations.The K+(1) cations connect the 1D packing chains constructing the 2D netlike structure,and adjacent netlike layers are also grafted by K+(2) cations to build the novel 3D infinitely extended structure.The result of TG-DTA curves manifests that the decomposition temperature of the title polyanionic framework is 554℃.The cyclic volt-ammetry measurements show that the title polyanion has the two-step redox processes in aqueous solution with pH = 3.1.Variable temperature magnetic susceptibility indicates the title compound obeys the Cruie-Weiss Law in the higher temperature range from 110 to 300 K,while in the lower temperature range from 2 to 110 K the comparatively strong antiferromagnetism in-teractions can be observed.
