C 22 H 22 CoN 4 O 8 ,monoclinic, P2 1 /n (no. 14), a =8.2100(3) Å, b =10.6200(3) Å, c =25.4621(7) Å, b =90.618(2)°, V =2219.9 Å 3 , Z =4,Rgt(F) =0.031, wRref (F 2 ) =0.080, T =293 K.
Source of materialAm ixed solution of 2,3-naphthalenedicarboxylic acid (H 2 L, 0.05 mmol) and 4,4'-azopyridine (azpy, 0.05 mmol) in the presence of excess 2,6-dimethylpyridine (ca. 0.05 mL for adjusting the pH value to basic condition) in CH 3OH (10 mL) was carefully layered on top of aH 2 Osolution (15 mL) of Co(ClO 4 ) 2. · . 6H 2 O (0.1 mmol) in atest tube. After about two weeks at room temperature, pink single crystals suitable for X-ray analysis were obtained (yield 40 %based on H2L). Elemental analysis -found: C, 49.68 %; H, 4.53 %; N, 10.29 %; calculated for C 22 H 22 CoN 4 O 8 :C,49.92 %; H, 4.19 %; N, 10.58 %.
Experimental detailsThe hydrogen atoms of water were refined with d(O-H) = 0.85 Å and U iso (H) =1.2 U eq (O). The hydrogen atoms bound to carbon atoms were included in calculated positions and treated as riding with d(C-H) =0 .93 -0 .96 Å and U iso(H) =1 .2 or 1.5 U eq (C).
DiscussionIn recent years, infinite 1D chains are of great interest because they can be used as non-linear optical [1], magnetic [2], and luminescent materials [3], as well as the structural constructing units being further expanded to 2D layers or 3D networks either by covalent bonds [4,5] or by hydrogen bonds, p-p interactions [6][7][8]. In many of these investigating the linear N,N'-donor spacers such as 4,4'-bipyridine ligand and its analogues were used [9,10]. 4,4'-azopyridine (azpy) ligand, the more extended ligand compared with 4,4'-bipyridine, is an ideal connector between metal atoms for the propagation of coordination networks due to its bidentate character [11,12]. The title crystal structure consists of 1D Co(L)(azpy)(H 2 O) 3 chains. The asymmetric unit of the title structure contains one Co(II) center, one L 2-ligand, one azpy ligand, three coordinated water molecules, and one lattice water molecule. Each Co atom is octahedrally coordinated by two Natoms from two different azpy ligands, one Oatom from L 2-ligand, and three Oatoms from water molecules. The Co-Oand the Co-Nbond lengths are in the range of 2.030(1) -2.152(2) Å and 2.206(2) -2.173(2) Å,respectively. The L 2-ligand coordinates Co in am onodentate mode. With regard to pypz ligand, it takes abidentate bridging coordination fashion and links two Co(II) centers with two Nd onors to form anearly linear chain containing alternative Co centers separated by 13.369(5) Å.Inaddition, the adjacent chains are interlinked to form a3 Ds upramolecular strucutre through O-H···O hydrogen bonding interactions between carboxylate Oatoms of Lligands and coordinated water molecules. Moreover, the lattice water molecules were included within the voids of the framework and form O-H···Ohydrogen bonding interactions with Lligands and coordinated water molecules.