Synthesis, crystal structure and electrochemical properties of [Co(phen)3] · (H3btec) · (H2btec)0.5 · DMF · 6H2O

Abstract

A new complex [Co(phen) 3 ] ⋅ (H 3 btec) · (H 2 btec) 0.5 · DMF · 6H 2 O (1) (H 4 btec = 1,2,4,5 Ben zenetetracarboxylic acid, phen = 1,10 phenanthroline, DMF = dimethylformamide) was synthesized by the reaction of pyromellitic dianhydride, phen · H 2 O and CoSO 4 · 7H 2 O. Complex 1 crystallizes in the triclinic system, space group P 1 with a = 11.8123(14) Å, b = 13.0356(16) Å, c = 17.575(2) Å, α = 91.461(2)°, β = 101.347(2)°, γ = 99.830(2)°, FW = 1159.94, Z = 2, V = 2609.5(5) Å 3 . X ray crystal structural determination indicates that the Co(II) ion is octahedral coordinated by six nitrogen atoms of three phenanthroline ligands. The [Co(phen) 3 ] 2+ cation engages its phen ligands in π-π interactions with H 2 btec anion. Extensive hydro gen bonding interactions occur between water molecules, DMF, H 3 btec and H 2 btec anions. The highly crys talline compounds 1, which are insoluble in water as well as common organic solvents, have been character ized in the solid state by elemental analysis, thermogravimetric analysis and IR spectra. Moreover, the study of the electrochemistry of complex 1 was carried out by using cyclic voltammetry. It revealed that the Co(II) complex exhibits a quasi reversible one electron redox process.

Complex of Tris(Phenanthroline)Cobalt(II)Trifluoroacetate: Characterisation and Powder XRD Analysis

“…For the complex (Fig. 3A-red) a broad band at about 3400 cm -1 might be due to -OH stretching of H 2 O molecule as observed at 3417 cm -1 according to Tao et al, 3 , but at 3512 cm -1 reported by Yesilel el al., 5 . Another medium band at 3080 cm -1 is due to aromatic C-H bond as reported by Hamdani et al, 28 at 3100 cm -1 and Zang et al, 29 at 3064 cm -1 .…”

“…The single crystals of cation [Co(phen) 3 ] 2+ with par ticularly various anions have been reported with cell parameters as shown in Table 4 28 . They were found as triclinic-PI space group for the first two 3,6 , monoclinic-P2 1 /c for the second two 5,7 , and monoclinic-C 2 /c for the last two 4,8 , respectively. In fact, no cell parameters are found to be very close one to another although they are in the same symmetry and space group.…”

“…Crystal structure of tris-bidentate-cobalt(II) complexes have been well known, particularly those with N-donor atoms in six-membered ring system, bipyridine (bipy) 1,2 and 1,10-phenanthroline (phen) 3 . Structural studies through single crystal XRD analyses of tris(phen)cobalt(II) with several counter anions, the perchlorate (ClO 4 ) 4 , squarate (C 4 O 4 ) 5 , tetrathionate (S 4 O 6 ) 6 , triiodide (I 3 ) 7 and the trichloroacetate (CCl 3 COO) 8 have been well refined.…”

Synthesis and Structural Analysis of Powder Complex of Tris(bipyridine)cobalt(II) Trifluoromethanesulfonate Octahydrate

“…The chemistry of Co(II) complexes with bidentate ligands such as ethylenediamine (en) [1], phenanthroline (phen) [2] and bipyridine (bipy) [3] have been well known. In particular, the crystal structure of [Co(bipy)3](ClO4)2 has also been determined [4].…”

Tris(1,10-phenanthroline-κ2 N,N′)cobalt(II) bis(2,4,5-tricarboxybenzoate) monohydrate

“…However, reports of benzene-1,2,4,5-tetracarboxylate acting only as a counter-anion are rare, e.g. tris(1,10-phenan-data reports throline)cobalt(II) 2,3,4-tricarboxybenzoate hemi(2,4-dicarboxybenzene-1,3-dicarboxylate) dimethylformamide solvate hexahydrate (Tao et al, 2012) and bis [tetraaqua-(1,10phenanthroline-…”