Geçiş metal kompleksi katyon heptaborat yapılarının sentezi ve karakterizasyonu

Abstract

Geçiş metali kompleks katyonları içeren heptaborat yapıları sentezlenmiş ve elementel analiz, erime noktası belirleme, FT-IR, TGA/DTA analizi, UV analizi ve x-ışını kırınımı (XRD) analiz yöntemleri kullanılarak karakterize edilmiştir. Heptaborat tuz yapılarının kızılötesi spektrumlarında, geçiş metali kompleksinin varlığını gösteren (-M-N)phen ve (-M-N)pyrd gerilme titreşimlerinin pikleri gözlendi. Heptaborat yapısının karakteristik titreşimleri olarak, yapılarda bulunan B-OH bağlarının -OH pikleri ve yapılarda dört trigonal borat molekülünün varlığını doğrulayan asimetrik ve simetrik gerilme titreşimleri keskin pikler olarak ortaya çıkmıştır. Geçiş metalli kompleks katyonları ile heptaborat tuz yapılarının termal analiz ayrışma eğrilerinin benzer olduğu gözlendi. Moleküllerin benzer bozunma özelliklerine bağlı olarak tüm yapılarda koordinasyon küresi dışında bulunan hidrat sularının tek bir adımda yapılardan uzaklaştığı görülmektedir. Heptaborat tuz yapılarının ikinci bozunma basamağı olarak borat halkalarındaki -OH gruplarının tüm yapılarda su buharı halinde uzaklaşmasına atfedilebilecek miktarlarda su kaybı tespit edilmiştir. Bu bozunma adımının tüm yapılarda tek adımda gerçekleştiği ve ilgili deneysel teorik kütle kayıplarının birbiri ile uyumlu olduğu görülmüştür. Metal katyon kompleksli heptaborat tuz yapılarının son bozunma aşaması olarak organik ligandların yanarak bozunması gözlendi. Kaydedilen toz x-ışını kırınım modellerinden heptaborat halkalarına ait pikler gözlenirken, elektronik geçiş verileri de metal katyon kompleksinin oktahedral geometride olduğunu desteklemektedir.

Keywords

• boratlar
• heptaborat
• metal katyonlu boratlar
• bor kimyası
• siklik boratlar

Synthesis and characterization of transition metal complex cation heptaborate structures

Abstract

Heptaborate structures with transition metal complex cations were synthesized and characterized using elemental analysis, melting point determination, FT-IR, TGA/DTA analysis, UV analysis, x-ray diffraction (XRD) analysis methods. In the infrared spectra of heptaborate salt structures, peaks of (-M-N)phen and (-M-N)pyrd stretching vibrations, which indicate the presence of transition metal complex, were observed. As the characteristic vibrations of the heptaborate structure, the -OH peaks of the B-OH bonds present in the structures and the asymmetric and symmetrical stretching vibrations, which confirm the presence of four trigonal borate molecules in the structures, appeared as sharp peaks. It was observed that the thermal analysis decomposition curves of heptaborate salt structures with transition metal complex cations were similar. Depending on the similar degradation characteristics of the molecules, it is seen that the hydrate waters settled outside the coordination sphere in all structures move away from the structures in a single step. As the second degradation step of heptaborate salt structures, the removal of water in amounts that can be attributed to the removal of -OH groups in the borate rings in the form of water vapor in all structures was detected. It was seen that this degradation step took place in a single step in all structures and the related experimental theoretical mass losses were compatible with each other. Combustion degradation of organic ligands was observed as the final degradation step of heptaborate salt structures with metal cation complexes. While peaks belonging to heptaborate rings were observed from the recorded powder x-ray diffraction patterns, electronic transition data also supported that the metal cation complex was in octahedral geometry.

Keywords

• borates
• heptaborate
• borates with metal cations
• boron chemistry
• cyclic borates

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