Crystal structure of diaqua(1,10-phenanthroline-k2N,N′)bis[o-(4-methyl-benzoyl)benzoato-k2O,O′]cobalt(II), Co(H2O)2(C12H8N2)(C15H11O3)2
Zeitschrift für Kristallographie - New Crystal Structures
C 42 H 34 CoN 2 O 8 ,monoclinic, C12/c1(no. 15), a =27.750(6) Å, b =10.153(2) Å, c =14.204(3) Å, b =117.78(3)°, V =3540.7 Å 3 , Z =4,R gt (F) =0.032, wR ref (F 2 ) =0.090, T =113 K. Source of material Am ixture of o-(4-methylbenzoyl)benzoic acid (0.60 mmol, 1.442 g), cobalt chloride (0.3 mmol, 0.714 g) and 1,10-phenanthroline (phen, 0.3 mmol, 0.054 g) was dissolved in 15 ml of 95 %ethanol. The pH value of the resultant mixture was adjusted to about 6.0 by adding five drops of sodium hydroxide
... sodium hydroxide solution and the reaction was kept under water-bath condition at 341 Kfor 28 h. Afterwards, the system was filtered, and the filtrate was cooled to room temperature slowly. Red block-shaped single crystals suitable for X-ray diffraction analysis were obtained after three weeks. Experiemental details Hydrogen atoms bound to carbon atoms were placed in calculted positions and treated as riding on their parent atoms with d(C-H aromtic)=0.90(1) Å and Uiso(H) =1.2 Ueq(C). Hatoms of water molecule were initially located in adifference Fourier map and refined. Discussion Carboxylic complexes have become one of the hottest research fields due to their versatile topology, special properties and extensive applications in magnetic, optical, catalytic and biological devices [1,2]. So far, much attention in this field has been paid to the rigid aromatic carboxylic acid, and complexes constructed form heterocyclic carboxylic acid are still rare     . o-Methylbenzoylbenzoic acid is am ulti-dentate coordination ligand, which can serve as aterminal ligand or as abridging ligand. The title crystal structure contains Co(H 2 O) 2 (phen)(C 15 H 11 O 3 ) 2 units. The central cobalt(II) ion is coordinated by two nitrogen atoms from one 1,10-phenanthroline molecule, four oxygen atoms from two o-(4-methylbenzoyl)benzoate molecules and two water molecules, respctively, forming adistorted octahedral coordination. In the CoN 2 O 4 unit, N1, N1A, O4 and O4A locate at the equatorial plane, O1 and O1A occupy the axial positions. The cis bond angles ∠N1-Co1-N1A, ∠N1A-Co1-O4A, ∠O4A-Co1-O4 and ∠O4-Co1-N1 are 78.72(7)°,9 8.57(5)°, 84.66(7)°and 98.57(5)°,r espectively, with the sum of 360.52°( close to 360°). In the complex, there exist hydrogen bonding interactions. The uncoordinated carbonyl oxygen atoms of o-(4methylbenzoyl)benzoate ligands and the water molecules are linked by strong hydrogen bonds: O4-H4A···O3 (2.797(2) Å, 156(2)°)and O4-H4B···O2 (2.608(2) Å,173(2)°).