The title compound, C22H18N4O2S2, was characterized by 1H and 13C NMR, solid-state IR spectroscopy and X-ray crystallographic techniques. The crystal structure determination reveals that the twisting modes of the two side arms are different [C—N—C—O and C—N—C—N torsion angles = −1.2 (3) and 1.1 (3)°, respectively, in one arm and 24.1 (3) and −5.1 (3)°, respectively, in the other]. The crystal structure involves N—H⋯O and N—H⋯S hydrogen bonds.
The tridentate N 4 -type Schiff base was synthesized from the condensation reaction of 2-hydrazinopyridine and pyridine-2-carbaldehyde. Neodymium and Samarium complexes were isolated when the corresponding nitrate salt was added to the solution of the ligand. The isolated compounds were characterized by elemental analyses, IR study, room temperature magnetic measurements and single X-ray crystal diffraction of the two crystals. Both complexes crystallize in the monoclinic system with space group P21/c.
KEYWORDSLanthanide complexes, hydrazino, antioxidant activity, X-ray structure.
The coordination chemistry towards the M(II) metal centre (M = Mn, Ni, Cu or Zn) of the hydrazone ligand (E)-2-amino-N'-[1-(pyridin-2-yl)ethylidene]benzohydrazide (H3L) has been explored and complexes having formulae [Mn(H2L)2] (1), {[Ni(H2L)2]. DMF. 0.4H2O} (2), {[Cu2(H2L)2(µ-Cl)2]. DMF} (3) and [Zn(H2L)2] (4) have been isolated and characterized by IR, UV-Visible spectroscopy, elemental analysis and Xray crystal diffraction. Structural studies reveal that the mononuclear complexes (1), (2) and (4) adopt highly distorted octahedral geometries while the dinuclear complex (3) adopts a square pyramidal geometry around each copper(II) ion.
Mononuclear complexes of 1-(pyridin-2-ylmethylidene)-2-(pyridin-2-yl)hydrazine (HL 1 ) and 1-(pyridin-2-yl)-2-(1-, [Zn(HL 1 )(CH3COO)2] . (H2O)3 (2), [Mn(HL 2 )2] . (ClO4)2 (3) and [Cu(HL 2 )(NO3)2] (4), were synthesized and characterized by physico-chemical and spectroscopic methods and X-ray structure determination. The mononuclear compounds 1, 2 and 4 contain one ligand molecule per metal atom while the manganese (II) atom in the compound 3 is coordinated to two ligand molecules. Both ligands coordinated to the transition metal center in tridentate fashion through two Npyridyl atoms and one Nimino atom. The chloride and acetate anions coordinate in monodentate manner respectively in complex 1 and in complex 2. In complex
The reaction of benzoyl chloride and ethylendiamine in the presence of potassium thiocyanate yielded a white solid, C18H18N4O2S2, which consists of two benzoylthioureido moieties connected by an ethylene chain. The asymmetric unit consists of one half of the molecule, the complete molecule being generated by crystallographic inversion symmetry. Both thiourea moieties are in a trans conformation. An intramolecular N—H...O hydrogen bond occurs. In the crystal, C—H...S and C—H...O hydrogen bonds link the molecules, forming layers parallel to the ac plane.
Key indicators: single-crystal X-ray study; T = 293 K; mean (C-C) = 0.006 Å; R factor = 0.042; wR factor = 0.102; data-to-parameter ratio = 14.0.The title compound, [ZnCl 2 (C 18 H 14 N 4 O)], crystallizes with two molecules in the asymmetric unit, which differ in the tautomeric (neutral and zwitterionic) forms of the coordinating organic ligand. In both molecules, the Zn II atom adopts a distorted square-pyramidal geometry by two N and one O atoms of the Schiff base ligand and two Cl atoms acting as monodentate chloride anions. The crystal packing is stabilized by N-HÁ Á ÁN and N-HÁ Á ÁCl hydrogen bonds, forming a twodimensional network parallel to the ac plane.
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In the title compound, [Tb(C2H3O2)2(C11H10N4)(H2O)2]NO3·H2O, the Tb3+ ion is nine-coordinated in a distorted tricapped trigonal-prismatic geometry by the three N atoms of the tridentate 1-(pyridin-2-ylmethylidene)-2-(pyridin-2-yl)hydrazine ligand, four carboxylate O atoms of two chelating acetate groups and two O atoms of the coordinating water molecules. The organic hydrazine ligand is disordered over two orientations with a refined occupancy ratio of 0.52 (3):0.48 (3). All bond lengths in the coordination environment of the Tb3+ ion are slightly larger than those observed in the isostructural Y3+ and Er3+ complexes. In the crystal, the complex cations are linked by pairs of O—H...O hydrogen bonds into dimers. These dimers, nitrate anions and non-coordinating water molecules are joined by O—H...O and N—H...O hydrogen bonds into a three-dimensional structure.
In the title compound, [Ni(C9H9N4O2)2], the NiII ion is situated on a twofold rotation axis and is coordinated by two O and four N atoms from two tridentate {2-amino-2-oxo-N-[(1E)-1-(pyridin-2-yl-κN)ethylidene]acetohydrazidate ligands in a distorted octahedral geometry. In the crystal, N—H⋯O and N—H⋯N hydrogen bonds link the molecules into columns in [001]. The porous crystal packing is further stabilized via π–π interactions between the pyridine rings of neighbouring molecules [centroid–centroid distance = 3.746 (3) Å] with voids of 270 Å3.
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