Preparation and Crystal Structures of LaCl_3（12－crown－4）（MeOH）and［LaCl_3（phen）_2（H_2O）］·MeOH

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Preparation and Crystal Structures of LaCl_3(12-crown-4)(MeOH)and[LaCl_3(phen)_2(H_2O)]·MeOH

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 ofLaCl3 (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 P1P21/α];V=784.5(5)2580(1)3,Z=24];μ(MoKα)=32.820. 2]cm-1;F (000)=4441296];R=0.0420.045];Rω=0.0440.036] 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.