Synthesis and characterization of tetra-armed-thiosemicarbazone and its salen/salophen capped transition metal complexes: Investigation of their thermal and magnetic properties


UYSAL Ş. , ER M. , TAHTACI H.

SYNTHETIC COMMUNICATIONS, cilt.46, ss.1820-1832, 2016 (SCI İndekslerine Giren Dergi) identifier identifier

  • Cilt numarası: 46 Konu: 22
  • Basım Tarihi: 2016
  • Doi Numarası: 10.1080/00397911.2016.1229791
  • Dergi Adı: SYNTHETIC COMMUNICATIONS
  • Sayfa Sayıları: ss.1820-1832

Özet

In this work, we aimed to synthesize and characterize a novel tetra-directional ligand, (2E,2E)-2,2-((((2-(1,3-bis(4-((E)-(2-carbamothioylhydrazono)methyl)phenoxy)propan-2-ylidene)propane-1,3-diyl)bis(oxy))bis(4,1-phenylene))bis(methanylylidene))bis(hydrazinecarbothioamide) (5), including thiosemicarbazone group and its novel tetra-directional-tetra-nuclear Schiff base complexes. For this purpose, we used 1,4-dibromo-2,3-bis(bromomethyl)but-2-ene (2) as starting material. 4,4-((2-(1,3-Bis(4-formylphenoxy)propan-2-ylidene)propane-1,3-diyl) bis(oxy))dibenzaldehyde (3) was synthesized by the reaction of an equivalent 1,4-dibromo-2,3-bis(bromomethyl)but-2-ene (2) and 4 equivalents of 4-hydroxybenzaldehyde. Then, compound 5 was synthesized in high yield (86%) by a condensation reaction of compound 3 with thiosemicarbazide (4). Finally, four novel tetra-nuclear Cr(III) or Fe(III) complexes of compound 5 were synthesized. The synthesized compounds were characterized using elemental analyses, H-1 NMR, Fourier transform-infrared spectrometry, liquid chromatography-mass spectrometry (ESI+), and thermal analyses. The metal ratios of the prepared complexes were determined using an atomic absorption spectrophotometer. We also investigated their effects on the magnetic behaviors of [salen, salophen, Cr(III)/Fe(III)] capped complexes. The complexes were found to be low-spin distorted octahedral Fe(III) and distorted octahedral Cr(III), all bridged by thiosemicarbazone.