Synthesis and solid-state spectroscopic investigation of some novel diorganotin(IV) complexes of tetraazamacrocyclic ligands |
| |
Authors: | Mala Nath Pramendra K Saini Xueqing Song |
| |
Institution: | a Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247 667, Uttarakhand, India b Department of Chemistry and Physics, University of the District of Columbia, Washington, DC 20008, USA |
| |
Abstract: | The tetradendate macrocyclic ligands, H2L-1 = 5,12-dioxa-7,14-dimethyl-1,4,8,11-tetraazacyclotetradeca-1,8-diene] and H2L-2 = 6,14-dioxa-8,16-dimethyl-1,5,9,13-tetraazacyclohexadeca-1,9-diene] have been prepared by the condensation reaction of 1,2-diaminoethane and 1,3-diaminopropane, respectively, with ethyl acetoacetate in methanol at room temperature. The diorganotin(IV) complexes of general formula R2Sn(L-1)/R2Sn(L-2)] (R = Me, n-Bu and Ph) have been synthesized by template condensation reaction of 1,2-diaminoethane or 1,3-diaminopropane and ethyl acetoacetate with R2SnCl2 (R = Me or Ph) or n-Bu2SnO in 2:2:1 molar ratio at ambient temperature (35 ± 2 °C) in methanol. The solid-state characterization of resulting complexes have been carried out by elemental analysis, IR, recently developed DART-mass, solid-state 13C NMR, 119mSn Mössbauer spectroscopic studies. These studies suggest that in all of the studied complexes, the macrocyclic ligands act as tetradentate coordinating through four nitrogen atoms giving a skew-trapezoidal bipyramidal environment around tin center. Since, the studied diorganotin(IV) macrocyclic complexes are insoluble in common organic solvents, hence good crystals could not be grown for single crystal X-ray crystallographic studies. Thermal studies of all of the studied complexes have also been carried out in the temperature range 0-1000 °C using TG, DTG and DTA techniques. The end product of pyrolysis is SnO2 confirmed by XRD analysis. |
| |
Keywords: | Diorganotin(IV) Macrocycles DART-mass Solid-state NMR 119mSn Mö ssbauer |
本文献已被 ScienceDirect 等数据库收录! |
|