Search

A new 2D polymeric Mn–acetate complex [Mn3(CH3COO)6·2H2O]n has been synthesized in a two step reaction process and characterized by single crystal X-ray crystallography, IR and thermal analyses. Structural analysis indicates that complex 1 crystallized in the P21/n space group and also shows that syn–syn and μ-oxo bridging of acetate ligands forms antiferromagnetic trimeric metal cores which are further connected by syn–anti and anti–anti bridging of acetates, leading to the formation of a 2D coordination sheet structure. These 2D coordination sheets are further connected by supramolecular hydrogen bonding interactions, leading to the formation of a 3D supramolecular structure. During the 3D supramolecular structure formation, the complex forms both right handed and left handed helical supramolecular chains. A variable temperature magnetic study indicates that complex 1 is antiferromagnetic above 105 K, while at lower temperatures (

The condensation of diacetylmonoxime (damnx) with morpholine N-thiohydrazide (mth) in 1:1 molar ratio in ethanol (16 h) afforded a nitrogen–sulfur zwitterionic heterocyclic compound, N-(3,4-dimethyl-1,2,5-thiadiazole-2-ium-2-yl)morpholine-4-carbothioate (dtmc). However, the same reaction in presence of [Zn(OAc)2]·2H2O in ethanol under gentle reflux on (3 h) yielded the zinc complex, [Zn(Hdammthiol)(OAc)(H2O)]·H2O, where H2dammthiol (H2L2) is the thiol form of tridentate NNS donor thiohydrazone ligand, diacetylmonoxime morpholine N-thiohydrazone (Hdammth). Both the nitrogen–sulfur heterocyclic compound and the zinc complex have been characterized by elemental analyses, spectroscopy (IR, UV–Vis, 1H NMR and 13C NMR) and single crystal X-ray crystallography. It is noteworthy that the heterocyclic compound shows S⋯S interaction with distance 2.738 A in its planar conformation. The heterocyclic compound forms two dimensional supramolecular sheets through C–H⋯O and π⋯π interactions while the zinc complex, with distorted square pyramidal geometry, forms 1D supramolecular chain. A mechanism has been proposed for the formation of nitrogen–sulfur heterocyclic compound.

The Reaction of phenylmercury(II) acetate with salicylaldehyde morpholine N-thiohydrazone (H2smth) and 2-hydroxyacetophenone morpholine N-thiohydrazone (H2apmth) in dry ethanol under gentle refluxing condition form light yellow complexes [PhHg(Hsmth)] (1) and [PhHg(Hapmth)] (2) involving formation of Hg-S bond from the thiol form of the ligands after deprotonation of the SH proton. The structures of the complexes as determined by X-ray crystallography shows that the complex (1) has a distorted T-shaped geometry while the complex (2) adopts familiar linear coordination geometry. Complex (2) has two independent molecules comprising the asymmetric unit. Both the complexes form two-dimensional supramolecular assemblies due to a combination of weak intermolecular Hg····π and Hg····Hg interactions. The Hg····π and Hg····Hg distances are 3.937 and 4.0216(10) A, respectively, possibly indicating weak mercuriophilic interactions. The luminescent properties of the complexes in solution and in the solid state at room temperature are also described.

The reaction of phenylmercury(II) acetate and cadmium(II) acetate with a refluxed solution of diacetylmonoxime and morpholine N-thiohydrazide formed a novel phenylmercury(II) complex, [PhHg(Hdammthiol)] (1) and a cadmium(II) complex, [Cd(Hdammthiol)2] (2), respectively (where H2dammthiol is the thiol form of diacetylmonoximemorpholine N-thiohydrazone (Hdammth) formed by the condensation of diacetylmonoxime and morpholine N-thiohydrazide in the presence of phenylmercury(II) and cadmium(II) ions). The complexes were characterised by elemental analyses and spectral data (electronic, infrared and 1H NMR) and also by X-ray crystal structure analysis. The X-ray crystallography shows that the phenylmercury(II) complex attained a tricoordinated distorted T-shaped structure, while the cadmium(II) complex attained a trapezoidal bipyramidal geometry. The phenylmercury(II) complex forms a two-dimensional sheet via C–H⋯O and O–H⋯N hydrogen bonding and also forms a two-dimensional supramolecular dimer, having C–H⋯π synthons. Intermolecular C–H⋯O and O–H⋯O hydrogen bonding of the cadmium(II) complex forms a two-dimensional supramolecular sheet along the bc plane and posses an impressively short intermolecular C(sp3)⋯O(sp3) contact.