Crystal structure of [(R,R)-6,6-dimethyl-3-pyridin-2-yl-5,6,7,8- tetrahydro-5,7-methanoisoquinoline]-tris[4,4,4-trifluoro-1-(2-thienyl)- butane-1,3-dionato]dysprosium(III), Dy(C17H18N2)(C8H4O2SF3)3

Abstract

C 41 H 30 DyF 9 N 2 O 6 S 3 ,monoclinic, P2 1 (no. 4), a =10.174(2) Å, b =19.018(4) Å, c =12.037(2) Å, b =113.742(3)°, V =2131.9 Å 3 , Z =2,R gt (F) =0.048, wR ref (F 2 ) =0.112, T =291 K. Source of materialThe chiral ligand was prepared by the documented procedures [1] and Dy(tta) 3 · 2H2O( tta =4 ,4,4,-trifluoro-1-(2-thienyl)butane-1,3-dionato) was synthesized according to literature method [2]. As olution of Dy(tta) 3 · 2H 2 O( 87 mg, 0.1 mmol) in ethanol (5 mL) was added to as olution of chiral ligand (R,R)-6,6-dimethyl-3-pyridin-2-yl-5,6,7,8-tetrahydro-5,7-methanoisoquinoline (25 mg, 0.1 mmol) in acetone (5 mL). The mixture was kept at RT. Yellow single crystals of title complex, suitable for Xray analysis, were obtained in 73 %yield by slow evaporation of solvents over two weeks. Elemental analysis -found: C, 45.36 %; H, 3.02 %; N, 2.91 %; calculated for C 41 H 30 DyF 9 N 2 O 6 S 3 :C,45.75 %; H, 2.81 %; N, 2.60 %. Experimental detailsHatoms were included in calculated positions and treated as riding atoms with d(C-H) =0.93 Å (aromatic), 0.98 Å (tertiary), 0.97 Å (methylene) or 0.96 Å (methyl) and U iso(H) =1.2 or 1.5 U eq(C). The Flack parameter is 0.03(2). DiscussionOver the last decades, chiral complexes have been an active area of research in coordination chemistry due to their diverse application in asymmetric catalysis, enantioselective synthesis, bioinorganic and supramolecular chemistry [3][4][5][6]. An effective and facile method to prepare such kind of complexes is the generating of chiral motifs in the target molecule. Based on this strategy, as a continuance of our research [7], we employed ac hiral ligand (R,R)-6,6-dimethyl-3-pyridin-2-yl-5,6,7,8-tetrahydro-5,7-methanoisoquinoline to react with Dy(tta) 3 · 2H2O. Subsequently, the enantiomerically pure title compound was obtained. The unit cell of the title crystal structure contains two mononuclear neutral complexes. Each molecule is formed by three bdiketonate anions, ac hiral bipyridine derivative ligand and an eight-coordinated Dy(III) cation. The Dy(III) ion is coordinated with six Oatoms from three b-diketonate ligands. The other two coordination sites are occupied by two Na toms of ac hiral bipyridine derivative. The Dy-Ob ond lengthes range from 2.344(6) to 2.405(6) Å,w hile the Dy-Nb ond lengths are 2.527(7) and 2.567(7) Å.Eight bonds with different lengths give rise to astrongly distorted square antiprismatic environment of the Dy(III) ion. The two square planes are defined by O5, O6, N1, N2 and O1, O2, O3, O4 with the mean deviations of 0.024 and 0.030 Å,respectively. The dihedral angle is 3.38(1)°.