Formation reactions of oxalatomolybdates with Co(III) ethylenediamine cations

U okviru ovog diplomskog rada ispitivani su uvijeti nastajanja kompleksnih soli s [Co(EDDA)(en)]+ kationom i oksalatomolibdatima, [Mo2O5(ox)2(H2O)2]2- i [MoO3(ox)]2-, kao anionima. Reakcije su provedene u otopini i to pri sobnoj temperaturi te u uvijetima povišenog tlaka i temperature te mehanokemijski, odnosno u čvrstom stanju s i bez dodatka male količine otapala, vode, odnosno acetona. Reakcije provedene u otopni dale su kao produkte dihidratni i tetrahidratni solvat [Co(EDDA)(en)]2[Mo2O5(ox)2(H2O)2. Reakcije s [MoO3(ox)]2- u vodenoj otopini nisu dale produkt, no mehanokemijskom sintezom uz dodatak male količine acetona u kombinaciji sa starenjem kao produkt reakcije dobiven je [CoEDDA(en)]2(enH2)[CoMo6O24]·3H2O. Svi izolirani produkti identificirani su na osnovi rezultata kemijske analize, termogravimetrijske analize i podataka iz infracrvenih spektara. Izoliranim kompleksima odreĎena je i molekulska i kristalna struktura metodom difrakcije rentgenskih zraka na jediničnom kristalu.In this diploma thesis we researched conditions for formation of complex salts containing [Co(EDDA)(en)]+ as cation and oxalatomolybdates, [Mo2O5(ox)2(H2O)2]2- i [MoO3(ox)]2-, as anions. Reactions were conducted in solution at room temperature, in the conditions of high pressure and high temperature, and in the solid state as liquid assisted grinding with water or acetone. Reactions in the solution resulted in formation of dihydrate and tetrahydrate solvate of [Co(EDDA)(en)]2[Mo2O5(ox)2(H2O)2. Reactions with [MoO3(ox)]2- in water solution didn’t result in the formation of product, but liquid assisted grinding with few drops of acetone in the combination with aging resulted in formation of [CoEDDA(en)]2(enH2)[CoMo6O24]·3H2O. All products were identified by chemical analysis, termogravimetric analysis and infrared spectroscopy. Crystal and molecular structure of isolated products was determined using single crystal X-ray diffraction