Malaysian Journal of Analytical Sciences Vol 18 No 3 (2014): 562 - 571

 

 

 

SYNTHESIS AND CHARACTERIZATION OF 5,5,7,12,12,14-HEXAMETHYL-1,4,8,11-TETRAAZACYCLOTETRADECA-7,14-DIENIUM DIPERCHLORATE COPPER(II) COMPLEX

 

(Sintesis dan Pencirian Kompleks Di(Perklorat) 5,5,7,12,12,14-Heksametil-1,4,8,11-Tetraazasiklotetradeka-7,14-Dienium Kuprum(II))

 

Nur Hasyareeda Hassan*, Noorhanani M Ali, Bohari M Yamin, Nurul Huda Abd Karim, Noor Azlina Abd Ghani

 

School of Chemical Sciences and Food Technology,

Faculty of Science and Technology,

Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor Darul Ehsan, Malaysia

 

*Corresponding author: syareeda@ukm.edu.my

 

 

Abstract

In this study, 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-7,14-dienium diperchlorate copper(II) complex was successfully synthesized by reacting macrocyclic tetraaza perchlorate with copper(II) acetate monohydrate in 1:1 ratio. The metal complex was characterized by variety of physicochemical techniques such as melting point, CHN elemental analysis, metal content, ultraviolet-visible spectroscopy, infrared spectroscopy, single crystal X-ray diffraction, thermogravimetric analysis, mass spectrometry and magnetic susceptibility. The infrared spectrum of complex showed four main peaks for v(N-H), ν(C-H), v(C=N) and ν(C-N) bands that appeared in the region of 3432, 2975, 1670 and 1088 cm^-1 respectively. X-ray single crystal structure showed a four-coordination geometry around the copper atom adopting a monoclinic system with a space group P/2c, unit cell dimension with a = 26.8271(17) Å, b = 7.8778(5) Å and c = 17.9908(12) Å; α = 90º, β = 99.05º and γ = 90º. The value of μ_eff (B.M) for copper (II) complex in the range of 1.23-2.21 B revealed that the complex was square planar geometry.

 

Keywords: one-pot synthesis, tetraaza macrocycles, copper (II) complex

 

Abstrak

Dalam kajian ini, kompleks 5,5,7,12,12,14-heksametil-1,4,8,11-tetraazasiklotetradeka-7,14-dienium diperklorat kuprum(II) telah berjaya disintesis hasil tindak balas makrosiklik tetraaza perklorat dengan kuprum(II) asetat monohidrat dengan nisbah 1:1. Kompleks yang terhasil dicirikan dengan pelbagai teknik fizikokimia seperti takat lebur, analisis unsur CHN, kandungan logam, spektroskopi ultra lembayung boleh nampak, spektroskopi inframerah, kristalografi sinar-X, analisis termogravimetri, spektrometri jisim dan penetapan kerentanan magnet. Spektrum inframerah kompleks menunjukkan terdapat empat jalur ν(N-H), ν(C=N), ν(C-H) dan ν(C-N) yang masing-masing wujud pada julat 3483-3151, 1668-1648, 2984-2917 dan 1292-1025 cm^-1. Struktur hablur tunggal sinar-X menunjukkan atom pusat kuprum berkoordinat empat dan hablur mempunyai sistem monoklinik dengan kumpulan ruang P/2c, dengan dimensi a = 26.8271(17) Å, b = 7.8778(5) Å dan c = 17.9908(12) Å; α = 90º, β = 99.05º dan γ = 90º. Nilai μ_eff (B) untuk kompleks kuprum(II) berada pada julat 1.7-2.2 B.M menunjukkan bahawa kompleks ini mempunyai geometri satah persegi empat.

 

Kata kunci: sintesis satu bikar, makrosiklik tetraaza, kompleks kuprum (II)

 

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