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Title:	Pengkompleksan garam nikel, kobalt dan zink dengan garam makrosiklik 5,5,7,12,12,14-heksametil-1,4,8,11-tetraazasiklotetradeka-7,14-dienium ditiosianat dihidrat
Authors:	Nur Iliyani Mohd Ishak (P64432)
Supervisor:	Bohari Mohd Yamin, Prof. Dr.
Keywords:	Macrocyclic compounds
Issue Date:	12-Jun-2015
Description:	Garam makrosiklik 5,5,7,12,12,14-heksametil-1,4,8,11-tetraazasiklotetradeka-7,14-dienium ditiosianat dihidrat [(Me6[14]N4H4)](NCS)2.2H2O telah disintesis daripada tindak balas etilinadiamina dengan asid tiosianik. Garam tersebut telah dicirikan dengan kaedah spektroskopi inframerah, ultralembayung-boleh nampak, resonans magnet nukleus, analisis mikrounsur dan spektrometer jisim. Kajian kristalografi sinar-X menunjukkan garam makrosiklik tersebut terdiri daripada dwikation (Me6[14]N4H4), dua anion tiosianat dan dua molekul air penghabluran. Gelang makrosiklik ini terdiri daripada 4 atom nitrogen di mana 2 daripada atom nitrogen tersebut adalah terproton dan 2 atom nitrogen yang lain merupakan kumpulan azometin. Pasangan atom nitrogen kumpulan azometin dan amina berada pada kedudukan pepenjuru yang bersetentangan. Pengkompleksan ligan tetraaza tersebut dengan logam Ni2+, Zn2+ dan Co2+ melibatkan penyahprotonan dua atom hidrogen daripada amina terproton. Pengkompleksan dengan Ni(OAc)2 dalam aseton menghasilkan [(Me6[14]N4H2)Ni(II)](NCS)2.H2O. Pengkompleksan dengan ZnCl2 dalam metanol menghasilkan komplek yang tidak analogus dengan nikel iaitu [(Me6[14]N4H2)ClZn(II)]2[(NCS)4Zn(II)]. Pengkompleksan dengan CoCl2 dan CoSO4 dalam air menghasilkan kompleks yang sama iaitu [(Me6[14]N4H2)(NCS)2Co(III)]NCS. Ketiga-tiga kompleks tersebut telah dicirikan dengan kaedah IR, UV, CHNS, spektroskopi jisim dan disokong oleh kajian kristalografi sinar-X. Walaupun pada umumnya, pasangan anion tiosianat kekal dalam pembentukan garam kompleks, ia boleh juga bertindak sebagai ligan kepada logam seperti dalam komplek kobalt [(Me6[14]N4H2)(NCS)2Co(III)]NCS. Dalam situasi begini, kobalt telah mengalami pengoksidaan. Kajian antibakteria terhadap 6 jenis bakteria (3 gram positif dan 3 gram negatif) dilakukan dengan menentukan nilai kepekatan perencatan minimum (MIC). Ligan tetraaza, kompleks nikel dan kobalt didapati aktif terhadap bakteria. Ligan tetraaza menunjukkan aktiviti terhadap semua bakteria kecuali B. subtilis. Komplek kobalt merencat pertumbuhan semua bakteria manakala komplek nikel pula didapati merencat pertumbuhan bakteria E. coli sahaja. Walau bagaimanapun, nilai agak tinggi berbanding kawalan. Komplek zink pula tidak menunjukkan keaktifannya terhadap bakteria.,The tetraaza macrocyclic salt of 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-7,14-dienium dithiocyanate dihydrate [(Me6[14]N4H4)](NCS)2.2H2O was synthesized by the reaction of ethylenediamine with thiocyanic acid. The salt was characterized by infrared, ultraviolet-visible spectrophotometer and nuclear magnetic resonance spectroscopy, including microelemental analysis and mass spectrometer. X-ray crystallographic study showed that the macrocyclic salt consists of [(Me6[14]N4H4)] dication, two thiocyanate anions and two hydrated water molecules. Two of the nitrogen atoms in the macrocyclic ring are protonated and located diagonally against one another. The other two nitrogen atoms are also diagonally positioned but as azomethine groups. The complexation of tetraaza ligand with Ni2+,, Zn2+ and Co2+ metals involve deprotonation of the protonated amines. Complexation with Ni(OAc)2 in acetone gave [(Me6[14]N4H2)Ni(II)](NCS)2.H2O. However, the complex with ZnCl2 in methanol is a salt complex type, [(Me6[14]N4H2)ClZn(II)]2[(NCS)4Zn(II)]. On the other hand, both CoCl2 and CoSO4 in water formed same complex of the type [(Me6[14]N4H2)(NCS)2Co(III)]NCS. All the complexes were characterized by IR, UV-Vis, microelemental analysis, mass spectrometer and supported by X-ray crystallographic study. Although in general thiocyanate anion remains as counter anion in the complex, it can also act as a ligand to the metal as displayed by the cobalt complex. In this situation, cobalt has undergone oxidization. Antibacterial study of the ligand and complexes against six types of bacteria (3 gram-positive and 3 gram-negative) was carried out by determine the minimum inhibitory concentrations (MICs) value. Tetraaza ligand showed activity against all the bacteria except for B. subtilis. Cobalt complex showed activity against all the bacteria while nickel only showed activity against E. coli only. However, MICs value was found to be higher than control positive. On the contrary, zinc complex showed no activity against all the bacteria.,Sarjana Sains
Pages:	108
Call Number:	QD400.N847 2015
Publisher:	UKM, Bangi
Appears in Collections:	Faculty of Science and Technology / Fakulti Sains dan Teknologi

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