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Title:Sinteza in strukturne značilnosti novih luminiscentnih lantanoidnih kompleksov z izbranimi N-donorskimi ligandi
Authors:ID Hojnik, Nuša (Author)
ID Kristl, Matjaž (Mentor) More about this mentor... New window
ID Drofenik, Miha (Comentor)
Files:.pdf DOK_Hojnik_Nusa_2015.pdf (3,43 MB)
MD5: 57B686A78355ABC39DFEE60F1646A87D
 
Language:Slovenian
Work type:Dissertation
Typology:2.08 - Doctoral Dissertation
Organization:FKKT - Faculty of Chemistry and Chemical Engineering
Abstract:Namen doktorskega dela je bila razširitev in poglobitev znanja s področja kemijske sistematike koordinacijskih spojin s centralnimi atomi elementov f – bloka periodnega sistema. V doktorskem delu smo obravnavali sintezo in karakterizacijo novih koordinacijskih spojin lantanoidov z biološko pomembnimi N−donorskimi ligandi, saj se je izkazalo, da so ti prekurzorji zelo uporabni za tvorbo koordinacijskih spojin s kovinami, saj lahko njihova koordinacija poteka na različne načine. Kot ligande smo uporabili nikotinsko kislino (NIC) in dipikolinsko kislino (Pydc). Raziskave smo razširili še na področje sintez koordinacijskih spojin z mešanimi ligandi. Sintetizirali smo prve primere spojin, ki hkrati vsebujejo z dipikolinsko kislino in 2−aminobenzotiazol (ABT), za kakršne v kristalografski podatkovni zbirki (CSD) še ni obstajal zapis. To področje je do sedaj slabše raziskano zaradi razlik v reaktivnosti posameznih ligandov. Zaenkrat naše spojine niso vsebovale 2−aminobenzotiazol kot ligand ampak kot kation. Zasledovanje sintez in analiza struktur koordinacijskih spojin z organskimi ligandi nam je omogočilo delno napovedovanje povezovanja gradnikov v kristalno mrežo že na osnovi poznavanja molekulske zgradbe samih gradnikov. Realizacija raziskovalnega dela je vodila do priprave novih spojin in tudi prispevala k boljšemu razumevanju nastanka koordinacijskih spojin. Uspešni pripravi monokristalov je sledila skrbna analiza strukture, kjer smo uporabili difraktometer s CCD detektorjem za monokristale v sodelovanju s FKKT Univerze v Ljubljani. Opravili smo še infrardečo spektroskopijio, termogravimetrično in elementarno analizo, magnetne meritve, v nekaterih primerih pa tudi fluorescenčno spektroskopijo. Pripravili smo skupaj sedem novih spojin z različnimi razmerji med centralnim atomom in dušikovim ligandom. V nekaterih primerih je v strukturi koordinacijske molekule vezana tudi voda. Raziskave so potekale v smeri iskanja novih sintez, na ta način smo izolirali različne dvojedrne komplekse kot so, [Yb2(NIC)6(H2O)4] in [Gd2(NIC)6(H2O)4] ter prav tako določili strukturo koordinacijske spojine [Nd2(NIC)6(H2O)4], za katero so bili v literaturi objavljeni samo parametri osnovne celice, enojedrne kompleksne spojine z Na3[Ho(Pydc)3]14H2O in Na3[Dy(Pydc)3]14H2O ter različne enojedrne kompleksne spojine z ABT in Pydc (ABT)3[Eu(Pydc)3]5H2O, (ABT)3[Tb(Pydc)3]5H2O, (ABT)[Cu(Pydc)(PydcH)]3H2O. S primerjavo z izbranimi strukturnimi parametri lahko lažje razumemo dobljene rezultate, ki nam jih nudijo spektroskopske ali druge metode. Večina rezultatov je objavljenih v mednarodnih znanstvenih revijah.
Keywords:Lantanoidni kompleksi, rentgenska strukturna analiza, luminiscenca, magnetne meritve, vodikove vezi
Place of publishing:Maribor
Publisher:[N. Hojnik]
Year of publishing:2015
PID:20.500.12556/DKUM-47971 New window
UDC:52-628:542.057(043.3)
COBISS.SI-ID:18725398 New window
NUK URN:URN:SI:UM:DK:5T8AIEHC
Publication date in DKUM:01.06.2015
Views:2161
Downloads:286
Metadata:XML DC-XML DC-RDF
Categories:KTFMB - FKKT
:
HOJNIK, Nuša, 2015, Sinteza in strukturne značilnosti novih luminiscentnih lantanoidnih kompleksov z izbranimi N-donorskimi ligandi [online]. Doctoral dissertation. Maribor : N. Hojnik. [Accessed 17 April 2025]. Retrieved from: https://dk.um.si/IzpisGradiva.php?lang=eng&id=47971
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Secondary language

Language:English
Title:SYNTHESIS AND STRUCTURAL CHARACTERIZATION OF NOVEL LUMINISCENT LANTHANIDE COMPLEXES WITH N−DONOR LIGANDS
Abstract:The presented work extends and deepens general knowledge in the field of chemical systematics of coordination compounds with central atoms regarding f – block elements in periodic table. The investigation describes the syntheses, and characterisation of new lanthanide(III) coordination compounds with biologically important nitrogen donor ligands such as nicotinic (NIC) and dipicolinic acid (Pydc). It has been shown that these precursors are very useful for forming coordination compounds with metals, because of its coordination mode. Having successfully synthesised and characterised lanthanide complexes with simple N−donor ligands, we further used the synthesis principle to synthesise lanthanide metal complexes with certain mixed ligands. The first examples of coordination compounds with dipicolinc acid and 2−aminobenzothiazole (ABT) were synthesised according to the Cambridge Structural Database (CSD). This research area has so far been less well studied due to differences reactivities of individual organic ligands. The recent research on synthesis and structure of metal complexes enabled us to make partial predictions regarding the connectivity of crystalline lattices based on the molecular structure of the small building blocks used in their assembly. The realization of this research work gave us new compounds, but also contributed to better understanding of the formation of coordination compounds. Syntheses of the compounds were followed by their characterization by elemental and thermogravimetric analysis, IR and fluorescence spectroscopy, and magnetic measurements. In the case of successful single−crystal preparation we determined the crystal−structure using X−ray diffractometer with CCD detector in collaboration with Faculty of Chemistry and Chemical Tehnology University of Ljubljana. We prepared seven new lanthanide(III) coordination compounds with pyridine ligands. Additional molecules of solvent (water) are also present in some structures. The research was also directed toward searching of new syntheses, in this way we isolated various di−nuclear complexes such as: [Yb2(NIC)6(H2O)4], [Gd2(NIC)6(H2O)4], and [Nd2(NIC)6(H2O)4] (only the structural details of this compound were already known), mononuclear complexes: Na3[Ho(Pydc)3]14H2O, and Na3[Dy(Pydc)3]14H2O, and also mononuclear complexes with mixed ligands: (ABT)3[Eu(Pydc)3]5H2O, (ABT)3[Tb(Pydc)3]5H2O, (ABT)[Cu(Pydc)(PydcH)]3H2O. The comparison between the selected structural parameters enables easier understanding of the results obtained by spectroscopic or other methods. The majority of the results in this thesis were published in international scientific journals.
Keywords:Lanthanides complexes, X−ray structure determination, luminiscent properties, magnetic properties, hydrogen bonds


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