Synthesis, crystal structure and magnetic property of a three-dimensional cagelike polymer [Co(4,4?-bpy)(NCS)2(py)2]n

Wei, Yibin; Song, Lianqing; Hou, Hongwei; Fan, Yaoting

doi:10.1360/02yb9066

Cited by 11 publications

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References 14 publications

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“…The bond angles of O2Fe1N3 and O1Fe1N1 are 86.99 (8)°and 86.98(9)°, and the bond angles of O2Fe1O1 and O1FeN3 are 101.0(1)°, 97.70(9)°, respectively. The bond length of S1C19 is 1.637(4) Å, which is a little longer than the literature reported (1.162 Å) [10]. Meanwhile, there are several intermolecular hydrogen bonds occurring between nitrogen atom from ethylenediamine and sulfur atom, which is from isothiocyanato ion of a neighboring molecule, N2H2A···S1 #1 , 3.544(3) Å, 150.4°, the bond length of N2H2A···S1 #1 is slightly longer than that reported in the literature (3.322 Å) [11] #1 is 2.73 Å, which does not fall in the region of 2.2 Å to 2.5 Å, and this leads to be presence of the weak hydrogen bonds [11].…”

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Crystal structure of bis(N-(2-aminoethyl)salicylaldiminato)iron(III) isothiocyanide, [Fe(C9H11N2O)2][NCS]

Feng

Han

Wang

2006

Zeitschrift Für Kristallographie - New Crystal Structures

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C19H22FeN5O2S, triclinic, P1 (no. 2), a = 9.613(1) Å, b = 9.913(1) Å, c = 10.869(2) Å, a = 84.958(2)°, b = 89.047(2)°, g = 86.098(1)°, V = 1029.3 Å 3 , Z = 2, Rgt(F) = 0.038, wRref(F 2 ) = 0.099, T = 291 K. Source of materialThe mixture of FeCl 2 · 4H 2 O (0.122 g, 0.5 mmol) and NH 4 SCN (0.192 g, 1 mmol) were refluxed in anhydrous methanol (15 mL) at a temperature of 60°C for 50 min, then were added 20 mL methanol solution of freshly distilled salicylaldehyde and ethylenediamine simultaneously. The mixture was stirred for 5 h, then filtered. The resulting clear solution was diffused with ethyl ether vapor at room temperature under ambient for three weeks. Blocklike dark-red crystals were formed and collected by filtration and dried in air (yield 0.202 g, 46 %). DiscussionIron complexes play an important role in biological field, catalysis application and earth chemistry research [1][2][3][4]. Schiff base complexes containing different central metal atoms such as Zn, Cu, Ni and Ru have been studied in great detail for their various crystallographic features, enzymatic reactions and magnetic properties [5][6][7]. To the best of our knowledge, the iron(III) salicylaldehyde Schiff base complexes have been seldom reported [8,9]. At the same time, the study of octahedron complexes involving an aromatic Schiff base as the primary ligand, isothiocyanato ion as secondary ligand can serve as a useful model for gaining a better understanding of enzyme-metal ion-substrate complexes, which plays an important role in metalloenzyme-catalyzed biochemical reactions.Based on the studies of the iron complexes and the salicylaldehyde Schiff base, in the present ferrum enzyme imitational investigation, an octahedral complex of iron(III) ion with sal-en Schiff base as ligand has been template synthesized and characterized. The asymmetric unit of the crystal structure consists of a discrete [Fe(sal-en)2] + cation and a counter isothiocyanato anion ( figure, top). The central iron(III) ion is six-coordinated (FeN4O2 ) and the coordination polyhedron can be described as an distorted octahedron formed by the four nitrogen atoms of the ethylenediamine molecule part, and two hydroxyl oxygen atoms from salicylaldehyde molecule part. In the complex, the salicylaldehyde-ethylenediamine Schiff base molecule acts as tridentate chelate ligand, obviously, only one of the amidocyanogen group of the ethylenediamine was involved in the reaction to salicylaldehyde to obtain the sal-en Schiff base during the template synthesis. N1, N3, O2, N2 are occupied at equatorial positions, O1, N4, are occupied at apical positions, Fe1, N1, N2, C8, N9 form a cyclopental ring, and Fe1, O1, N1, N2, C1, C2 form a cyclohexal ring. All the atoms of two six-membered rings are almost at the

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