X-ray Diffraction and Thermal Characterization Study of SmIII Complex of Sulphonylurea, Glipizide: An Oral Antidiabetic Drug

Abstract

The present paper deals with the study of sulphonylurea glipizide (GLP) drug in order to give a thought concerning its coordinating potentiality towards some inner transition metals. Metal complex of GLP drug issynthesized and characterized by using analytical data, molar conductance, X-ray diffraction and thermogravimetric analysis (TGA and DTA) studies. From the analytical data, the complex is proposed to have general formula(C21H26N5O4S)2Sm(OH2)4.Low values of molar conductance indicate that complex have non ionic nature. The conductometric titration using monovariation method reveal that complexis L2M type which is further confirmed by Job’s method of continuous variation as modified by Turner and Anderson. Geometery of complex is assigned to be hexagonal in which ligand molecules lie horizontally joining the central metal atomand four water molecules attached vertically and horizontally with the metal, supported by spectroscopic study. Powder X-ray diffraction data have been used to calculate particle size, porosity, volume of unit cell and density of synthesized complex.The thermal decomposition of complex is studied using thermogravimetric (TGA) and differential thermal analysis (DTA) techniques. The kinetic parameters such as, energy of activation (Ea), enthalpy (ΔH), entropy (ΔS) and free energy change (ΔG) of the complexis evaluated by employing the Freeman-Carroll and Sharp-Wentworth methodsand the relative thermal stability of the complexisalso discussed.

Synthesis and structural characterization of nano‐sized metal complexes of 3‐(1‐methyl‐4‐hydroxy‐2‐oxo‐1,2‐dihydroquinolin‐3‐yl)‐2‐nitro‐3‐oxopropanoic acid. XRD, thermal, 3D modeling, and antitumor activity studies

“…3.1.6 | X-ray powder diffraction studies X-ray powder diffraction (XRD) analysis is primarily used for phase identification of a crystalline material and can provide information on unit cell dimensions. [52] The diffraction patterns were recorded within diffraction angle (2θ) from 10 to 80 for the ligand, H 3 L, and its Fe(III), Co(II), Ni(II), Cu(II), and Zn(II) complexes, Figure 4, revealed a series of sharp and intense diffraction peaks which indicate their crystalline characteristic. The values of diffraction angles, lattice spacing (d-spacing), and X-ray intensities of different diffraction peaks were measured, and the particle size (crystallite size) of metal complexes was calculated from X-ray line broadening with help of Debye Scherrer formula, D = Kλ/βcosθ [53] , where D is the particle size, K is a coefficient with a value close to unity (it has a typical value is equal to 0.89), λ is the wavelength of X-ray, θ is the diffraction angle obtained from 2θ values corresponding to maximum intensity peak in XRD pattern, and β is full width at half maximum.…”