Sinteza i strukturna karakterizacija kompleksnih soli [Co(NH3)6][Fe(C2O4)3] i [CoC2O4(NH3)4][Fe(C2O4)2(OH2)2]

master's thesis

• Title (english): Synthesis and structural characterization of complex salts [Co(NH3)6][Fe(C2O4)3] and [CoC2O4(NH3)4][Fe(C2O4)2(OH2)2]
• Author: Kristian Nakić
• Mentor: Marina Cindrić (mentor)
• Committee member: Marina Cindrić (predsjednik povjerenstva)
• Committee member: Davor Kovačević (član povjerenstva)
• Committee member: Sanda Rončević (član povjerenstva)
• Committee member: Višnja Vrdoljak (član povjerenstva)
• Granter: University of Zagreb; Faculty of Science; (Department of Chemistry); Zagreb
• Defense date and country: 2017-09-25, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

U okviru ovog diplomskog rada priređene su kompleksne soli [Co(NH3)6][Fe(C2O4)3], [CoC2O4(NH3)4]- -[Fe(C2O4)2(OH2)2] ∙ H2O i [CoC2O4(NH3)4][Fe(C2O4)2(OH2)2] ∙ 2H2O. Spojevi su priređeni reakcijama izmjene kationa i aniona pri čemu su kao ishodne supstancije korišteni kompleksni spojevi [CoC2O4(NH3)4]NO3·H2O, K3[Fe(C2O4)3]·3H2O i FeC2O4. Prilikom priprave navedenih kompleksnih soli željeza(III) i kobalta(III) primijenjeni su različiti reakcijski uvjeti, kao što su npr. različite reakcijske temperature, mijenjan je množinski omjer reaktanata kao i volumen otapala. Ovisno o reakcijskim uvjetima bilo je moguće izolirati dvije hidratne forme kompleksne soli [CoC2O4(NH3)4][Fe(C2O4)2(OH2)2], mono- i dihidrat.
Rentgenskom strukturnom analizom je ustanovljeno da produkt formule [Co(NH3)6][Fe(C2O4)3] u vodenoj otopini podliježe transformaciji u dihidratnu formu [CoC2O4(NH3)4][Fe(C2O4)2(OH2)2]. Pri transformaciji kod [Co(NH3)6][Fe(C2O4)3] dolazi do preraspodjele liganada u koordinacijskim sferama i željezovog(III) i kobaltovog(III) metalnog centra.
Svi su spojevi identificirani i okarakterizirani temeljem podataka difrakcije rentgenskog zračenja na polikristalnom uzorku, infracrvene spektroskopije i termičke analize. Molekulska i kristalna struktura kompleksnih soli određena je difrakcijom rentgenskog zračenja na jediničnom kristalu.

Abstract (english)

In this diploma thesis three new complex salts were described, [Co(NH3)6][Fe(C2O4)3], [CoC2O4(NH3)4][Fe(C2O4)2(OH2)2] ∙ H2O and [CoC2O4(NH3)4][Fe(C2O4)2(OH2)2] ∙ 2H2O. Those complexes were prepared by reactions of ion exchange with [CoC2O4(NH3)4]NO3·H2O, K3[Fe(C2O4)3]·3H2O and FeC2O4 as reactants and at various reaction conditions, such as different reaction temperatures, molar ratio of reactants and solvent volumes. Depending on rection conditions it was possible to isolate two hydrate forms of [CoC2O4(NH3)4][Fe(C2O4)2(OH2)2]: monohydrate and dihydrate.
It was established that complex salt [Co(NH3)6][Fe(C2O4)3] undergoes transformation into dihydrate form of [CoC2O4(NH3)4][Fe(C2O4)2(OH2)2], in aqueous solution and at room temperature. Upon mentioned transformation, the rearangement of ligands within both iron(III) and cobalt(III) coordination spheres takes place.
All compounds were identified and characterized by means of powder X-ray diffraction, IR spectroscopy and by thermal analysis. Molecular and crystal structure of complex salts was defined by means of single crystal X-ray diffraction.

• Keywords: kompleksni spojevi željeza; kompleksni spojevi kobalta; kompleksne soli; sinteze u anorganskoj kemiji; infracrvena spektroskopija; rentgenska strukturna analiza; termička analiza
• Keywords (english): complex compounds of iron; complex compounds of cobalt; complex salts; inorganic syntheses; infrared spectroscopy; X-ray diffraction analysis; thermal analysis
• Language: croatian
• URN:NBN: urn:nbn:hr:217:831842
• Study programme: Title: Graduate university studies in chemistry; specializations in: Research programme; Course: Research programme; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra kemije (magistar/magistra kemije)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Open access; Embargo expiration date: 2019-09-25
• Created on: 2017-10-24 11:49:15