Crystal structure of tris(dibenzoylmethanato)-[(R,R)-6,6-dimethyl-3- pyridin-2-yl-5,6,7,8-tetrahydro-5,7-methanoisoquinoline)]- gadolinium(III), Gd(C15H11O2)3(C17H18N2)

Abstract

Source of materialThe chiral ligand (R,R)-6,6-dimethyl-3-pyridin-2-yl-5,6,7,8-tetrahydro-5,7-methanoiso-quinoline was prepared by the procedures [1] and Gd(dbm) 3 ·2H 2 Owas synthesized according to [2]. As olution of Gd(dbm) 3 ·2 H 2 O( 86 mg, 0.1 mmol) in ethanol (10 mL) was addedt oas olution of chiral ligand (25 mg, 0.1 mmol) in acetone (10 mL). The mixture was stirred 10 minutes and kepta tR T. Yellow single crystals of title complex suitable for X-ray analysis were obtained in 73 %yield by slow evaporation of the solvent over two weeks. Experimental detailsHa toms were included in calculated positions and treated as riding atomswith d(C-H) =0.93 (aromatic), 0.97 (methylene) or 0.96 (methyl) Åa nd U iso (H) =1 .2 or 1.5 U eq (C). TheF lack parameter is 0.02(1). DiscussionChiral lanthanide complexes have attracted considerable attention of research in thefield of coordinationchemistry, material scienceand life sciencedue to theirdiverse applications in asymmetric catalysis, enantioselective synthesis, medical diagnotic and therapy [3][4][5][6][7]. Among them,t he Gd-based complexes are commonly used as chiral shift reagents for resolving NMR spectra [8]. The introduction of the chiral bipyridine derivative ligand results in the chirality of the title compound, which crystallizes with space group P2 1 .The chirality is dominated by the two centers C12 and C14 of the bipyridine derivative. the Gd(III)ion is coordinated by six oxygen atomsfrom three b-diketonate ligands and two nitrogen atomsofchiral pinene bipyridine. The arrangement of O 6 N 2 donors can be best approximated as ad istorted square antiprism.T he bond lengths d (Gd-O) are in the range of 2.328(5) -2.386(7) Åand d(Gd-N) are 2.574(5) and 2.599(5) Å, respectively. TheO3, O4, O5, O6 (bottom plane) and O1, O2, N1, N2 atoms(top plane) comprise the two square-basic planes of the antiprism with mean deviations of 0.072(3)and 0.113(3)Åfrom each plane, their dihedral angle is 1.7(2)°.