C 19 H 22 N 3 NdO 16 ,monoclinic, P12 1 /c1(no. 14), a =11.347(2) Å, b =10.857(2) Å, c =19.514(3) Å, b =92.927(2)°, V =2400.9 Å 3 , Z =4,Rgt(F) =0.022, wR ref (F 2 ) =0.053, T =296 K.
Source of materialThe mixture of Nd(NO 3)3.·.6H2O( 0.088 g, 0.2 mmol) and 4-hydroxypyridine-2,6-dicarboxylic acid (H 2CAM, 0.074 g, 0.4 mmol), was stirred into 15 ml aqueous solution. Then the pH value was adjusted to approx. 6with 1.5 Msolution of ammonia. And then 5m le thanol solution of 4-hydroxypyridine (4-Hpy, 0.025 g, 0.2 mmol) was added. The reaction mixture was heated on awater bath for 10 hat70°C, then filtered. The resulting clear solution was diffused with diethyl ether vapor at room temperature for two weeks, block-shaped pink crystals were obtained, the products are insoluble in water (yield 0.049 g, 36 %). Elemental analysis -found: C, 32.61 %; H, 3.18 %; N, 6.14 %; calculated for C 19 H 22 N 3 NdO 16 :C,32.95 %; H, 3.20 %; N, 6.06 %. IR data are available in the CIF.
DiscussionThe study of metal-organic supramolecule has gained great recognition as an important interface between synthetic chemistry and materials science and provides asolid foundation for understanding how molecules can be organized and how functions can be achieved [1][2][3]. The current attention is focus on the construction of metal-organic frameworks (MOFs) with novel topology, and on the crystal engineering of molecular architectures organized by coordination bonds and supramolecular contacts (such as hydrogen bonding, p-p stacking interactions, etc.) [4,5]. In this work, H 2 CAM was employed as the major ligand because the unit has unique acoordination geometry, which can potentially provide more coordination motifs [6]. The title crystal structure is composited of one neodymium(III) ion, two CAM 2-ligands, three coordinated water molecules, and two lattice water molecules as well as af ree 4-hydroxypyridinium cation. Nd(III) is nine-coordinated with at ricapped trigonal prism configuration. The Nd atom is coordinated by two CAM molecules using four oxygen atoms of chaleated deprotonated carboxylate group and two nitrogen atoms of the pyridine ring, and three oxygen atoms from the water molucules, with d(Nd-O) rang from 2.480(2) to 2.560(2) Å,and d(Nd-N) rang from 2.567(2) to 2.581(2) Å,which are within normal ranges [6,7]. The angles of the CAM to the central ion range from 61.72(7)°to 123.62(7)°.T he dihedral angle between the two pyridyl rings attached to the central ion is 60.21°,and the dihedral angle between pyridyl rings attached to the central ion and the pyridyl ring of free 4-Hpy ligand vary from 63.59°to 68.18°.In both CAM ligands the dicarboxylate groups are almost coplanar, and the atoms in the pyridine deviate from the mean plane defined by the pyridine ring by less than 0.100 Å.D eviation from the mean plane defined by the pyridine ring are observed for both of carboxylate groups with values ranging from O4 -0.0641 to O2 +0.0893 Å.This implies that the CAM is afairly rigid ligand and retains its integrity on metal che...