摘要
The interaction of lanthanum(Ⅲ) chloride with 12-crown-4 in MeCN/MeOH mixed solvent produces an anhydrous complex,LaCl3(12-crown-4)(MeOH)(complex Ⅰ),C9H20O5LaCl3(Mr= 453.6),in which the La(Ⅲ) ion is 8-coordinated by three Cl anions,four oxygen atoms from a crown ligand and a methanol oxygen atom,the complex molecules were connected into a dimer by two O(MeOH)…Cl hydrogen bonds.Reaction of complex Ⅰ with phen(1,10-phenanthroline) gives the crystallization of[LaCl3 (phen)2(H2O)]·MeOH(complex Ⅱ),C25H22O2N4LaCl3(Mr= 655.8) in which the crown ligand is totally replaced by two phen molecules.Cell parameters for the two complexes are a= 9.389(3)[13.228 (5)],b=11.382(4)[10.767(3)],c=7.542(3)[18.520(6) ];α=94.32(3)[90.0],β=102.10(2)[102.01(3)],γ=91. 83(3)[90. 0]°with space group P1[P21/α];V=784.5(5)[2580(1)3,Z=2[4];μ(MoKα)=32.8[20. 2]cm-1;F (000)=444[1296];R=0.042[0.045];Rω=0.044[0.036] for 2398 [2345] observed reflections withⅠ>3σ(Ⅰ).The La(Ⅲ) ion in complex Ⅱ is 8-coordinated by three Cl anions,four N atoms of two phen molecules and one water molecule.The methanolmolecule forms a hydrogen bond with Cl(3) atom.
The interaction of lanthanum(Ⅲ) chloride with 12-crown-4 in MeCN/MeOH mixed solvent produces an anhydrous complex,LaCl3(12-crown-4)(MeOH)(complex Ⅰ),C9H20O5LaCl3(Mr= 453.6),in which the La(Ⅲ) ion is 8-coordinated by three Cl anions,four oxygen atoms from a crown ligand and a methanol oxygen atom,the complex molecules were connected into a dimer by two O(MeOH)…Cl hydrogen bonds.Reaction of complex Ⅰ with phen(1,10-phenanthroline) gives the crystallization of[LaCl3 (phen)2(H2O)]·MeOH(complex Ⅱ),C25H22O2N4LaCl3(Mr= 655.8) in which the crown ligand is totally replaced by two phen molecules.Cell parameters for the two complexes are a= 9.389(3)[13.228 (5)],b=11.382(4)[10.767(3)],c=7.542(3)[18.520(6) ];α=94.32(3)[90.0],β=102.10(2)[102.01(3)],γ=91. 83(3)[90. 0]°with space group P1[P21/α];V=784.5(5)[2580(1)3,Z=2[4];μ(MoKα)=32.8[20. 2]cm-1;F (000)=444[1296];R=0.042[0.045];Rω=0.044[0.036] for 2398 [2345] observed reflections withⅠ>3σ(Ⅰ).The La(Ⅲ) ion in complex Ⅱ is 8-coordinated by three Cl anions,four N atoms of two phen molecules and one water molecule.The methanolmolecule forms a hydrogen bond with Cl(3) atom.
