CuL(ClO 4 ) 2 ] complex of 14-membered hexaazamacrocyclic ligand (L = 6,13-dimethyl-3,10-dioctyl-1,3,5,8,10,12-hexaazacyclotetradecane) was synthesized by template condensation reaction of 1,2-diaminopropane, octylamine, and formaldehyde in ethanol. The product was characterized by elemental analysis, Fourier-transformed infrared spectroscopy (FT-IR), ultraviolet-visible spectroscopy (UV-vis), diffused reflectance spectroscopy (DRS), liquid chromatography-mass spectrometry (LC-MS), and X-ray crystallographic technique. Thermal behavior of this complex was studied by thermogravimetric analysis (TGA). The IR and other spectral properties were consistent with the result from X-ray diffraction. The electronic absorption spectra of [CuL(ClO 4 ) 2 ] complex showed one band at 500 nm corresponding to 2 B 1g ? 2 B 2g transition. The complex crystallized in the triclinic space group of Pī with a = 8.1307(6) Å , b = 9.3579(7) Å , c = 13.3930(10) Å , a = 95.932(2)°, b = 98.579(2)°, and c = 114.478(2)°. The copper(II) ion of the macrocyclic cation displayed a tetragonally distorted octahedral geometry with four nitrogen atoms in the equatorial plane and two oxygen atoms from the perchlorate ions weakly coordinated to the copper(II) ion in the axial positions. The complex exhibited only weak luminescent property.Graphical Abstract A new macrocyclic complex that can be easily obtained from the one-pot synthesis.
CuL(ClO 4) 2 ] (1) (L = 3,10-diisobutyl-1,3,5,8,10,12-hexaazacyclotetradecane) was synthesized by condensation reaction of ethylenediamine, formaldehyde and iso-butylamine in absolute ethanol. Characterization of 1 utilized various spectroscopic techniques, viz. elemental analysis, electrospray ionization-mass spectrometry (ESI-MS), Fourier-transform infrared spectroscopy (FT-IR), ultraviolet-visible spectroscopy (UV-Vis), diffuse reflectance spectroscopy (DRS) and thermogravimetric analysis (TGA). Based on these techniques, the structure of 1 was proposed as Cu(II) ion occupying octahedral geometry with four secondary amine nitrogens of the hexaazamacrocyclic ligand and two perchlorato anions. 1 was used as a precursor in the preparation of cyano-bridged bimetallic compound, [CuL] 3 [Fe(CN) 6 ] 2 •5H 2 O (2), by reaction with K 3 [Fe(CN) 6 ] in aqueous solution. Single-crystal X-ray analysis indicated that 2 crystallized in the monoclinic system with space group P 2 1 /n. The structure of 2 consisted of cyano-bridged Fe III-Cu II pentanuclear molecules having two [Fe(CN) 6 ] 3− anions connected to three cis-[CuL] 2+ cations via two cis-cyanide ligands from each ferrate unit. In each of pentanuclear unit, the central [CuL] 2+ cation exhibited a distorted octahedral geometry while the other two units exhibited a distorted square pyramidal geometry. The room temperature magnetic moments of both complexes were measured to be 1.92 B.M. for 1 and 5.61 B.M. for 2. The in vitro antibacterial activity of 1 against Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922, and Pseudomonas aeruginosa ATCC 27853 strains were studied and compared with standard drugs, which showed moderate antibacterial activity compared with Penicillin and Gentamicin.
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