Mechanochemical Synthesis of Alkaline Earth Mg – Ba Saccharinates. Connectivity in the Crystal Structures of Mg(sac)2∙7H2O, Ca(sac)2∙7H2O and Ba(sac)2∙4.5H2O (sac = saccharinate)

Alkaline earth saccharinates Mg – Ba were synthesized by the known solution-based methods and also by mechanochemical synthesis. The compounds were characterized by TG/DSC, X-ray powder diffraction, and Mg, Ca and Ba saccharinates by single-crystal X-ray analysis. The structure of Mg(sac)2∙7H2O (sac = saccharinate), is known but the diffraction data were collected at 170 K in this study for comparison with other structures. Crystals of hydrates of Ca – Ba saccharinates are very thin needle-like. A 4 μm crystal of Ca(sac)2∙7H2O gave a low intensity diffraction pattern of sufficient quality to locate non-hydrogen atoms (triclinic crystal system, space group P-1, Z = 4). Crystals of strontium saccharinate were too thin for data collection, however the formula Sr(sac)2∙4H2O, proposed in a previous publication was confirmed by thermogravimetric analysis. Diffraction from a 12 μm thick crystal of Ba(sac)2∙4.5H2O resulted in a complete data set (monoclinic crystal system, space group P2/c, Z = 8). In the corresponding structures, the Mg ion is six-coordinated forming an octahedron, both Ca ions are irregularly eight-coordinated with the polyhedra bridged by saccharinate ions into chains, whereas both Ba ions are irregularly nine-coordinated with the polyhedra sharing edges and corners through bridging water molecules and bridging saccharinate ions into double chains. All water molecules are included into hydrogen bonding into layers with only van der Waals and weak C–H∙∙∙O bonds between the chains

Ternary Coordination Compounds of Copper(II) with Glycine and 2,2\u27-bipyridine: Synthesis, Structural Characterization, Magnetic and Biological Properties

Three new coordination compounds of copper(II) with glycine (HGly) and 2,2\u27-bipyridine (bipy) were synthesized by solution-based and mechanochemical methods: [Cu(Gly)(H2O)(bipy)][Cu(Gly)(SO4)(bipy)]·6H2O (1a·6H2O), [Cu(Gly)(H2O)(bipy)]2SO4 (1b), [Cu(Gly)(H2O) (bipy)]2SO4·H2O (1b·H2O). The amount of water in the reaction mixture influenced the product of crystallization. All compounds were characterized by X-ray diffraction methods and form 1D infinite chains or 2D sheets of complex ions connected by π-interactions. Compounds 1a·6H2O and 1b were characterized by X-band electron spin resonance (ESR) spectroscopy and the values of g-tensors for Cu(II) ions were determined. Compounds 1a·6H2O and 1b showed pronounced antiproliferative activity toward a panel of six human cell lines. The most impared was HepG2 cell line at 10−5 mol dm−3 concentration (74.5 % reduction of cell growth) followed by moderate activity toward KATO III, Caco-2, MDA-MB-231, PANC-1 and MRC-5 cells at 10−4 mol dm−3 concentration of compounds 1a·6H2O and 1b. Generally, both compounds express similar antiproliferative effect on evaluated cells

Cobalt, nickel and copper complexes with glycinamide: structural insights and magnetic properties

Ten new compounds of Co, Ni and Cu with glycinamide (HL = glycinamide): [Co(H2O)2(HL)2]Cl2 (1a), [Co(H2O)2(HL)2]Br1.06Cl0.94 (1b), [Co(H2O)2(HL)2]I2 (1c), [Ni(H2O)2(HL)2]Cl2 (2a), [Ni(H2O)2(HL)2]Br0.94Cl1.06 (2b), [Ni(H2O)2(HL)2]I2 (low and room temperature polymorph, 2cLT and 2cRT), [CuCl2(HL)2] (3a), [CuBr1.3Cl0.7(HL)2] (3b) and {;[Cu(HL)2]2[Cu2I6]};n (3c), as well as glycinamide hydroiodide (H2LI) and a new polymorph of glycinamide hydrochloride (β- H2LCl) were prepared and characterized by single-crystal X-ray diffraction, infrared spectroscopy, thermal analysis (TG/DTA) and ESR spectroscopy. 1a, 1b, 2a and 2b are isostructural, as well as 1c and 2cRT, while the Cu compounds (3a–c) have entirely different molecular structures. All investigated compounds are mononuclear with exception of the 1D coordination polymer 3c. Compound 3c contains copper ions in the mixed oxidation state Cu(I) and Cu(II) with interesting magnetic properties. Paramagnetic behaviour was found in 1a, 1b, 3a and 3b. Temperature induced polymorphic transformation was observed in 2c. Compounds 1a and 3a showed moderate antiproliferative activity and selectivity toward the human breast tumor cell line MCF-7

Structural transformations in complexes of cobalt, nickel and copper with selected α-amino acids and their derivatives

Istražene su reakcije kobaltovih(II), niklovih(II) te bakrovih(II) soli s glicinamidom (HGlyam), D-allo- i L-izoleucinom te L-homoserinom s ciljem priređivanja bis(didentatnih) koordinacijskih spojeva. Priređeno je i strukturno karakterizirano 17 bis(didentatnih) i jedan tris(didentatni) koordinacijski spoj te je proučena cis-trans izomerizacija u otopini i u čvrstom stanju. Utvrđena je značajna uloga metalnog iona u kristalizaciji određenog izomera, a također ključan čimbenik može biti anion, otapalo, atmosfera, temperatura i pH-vrijednost otopine. Dodatno je proučen temperaturno ovisan reverzibilan polimorfni prijelaz u spoju cis-[Ni(H2O)2(HGlyam)2]I2 čiji kristali pokazuju zanimljivo svojstvo samocijeljenja. U reakcijama s 2,2'-iminodiacetamidom priređeno je i strukturno karakterizirano 7 bis(tridentatnih) spojeva kobalta(II) i nikla(II). Priređena su i strukturno karakterizirana 22 ternarna koordinacijska spoja bakra(II) s α-aminokiselinama (glicin, L-serin i L-homoserin) i heterocikličkim bazama (2,2’-bipiridin i 1,10-fenantrolin). U nekoliko slučajeva uspješno je određen mehanizam međupretvorbe različitih solvata u čvrstom stanju, što je prvo takvo istraživanje na ovoj skupini spojeva.Reactions of cobalt(II), nickel(II), and copper(II) salts with glycinamide (HGlyam), D-allo- and L-isoleucine, and L-homoserine were investigated and 17 bis(bidentate) and one tris(bidentate) coordination compounds were prepared and structurally characterized. Cis-trans isomerization of bis(bidentate) compounds in solution and solid-state was studied. The role of a metal ion in the crystallization of a certain isomer was determined, however, in some cases the key factor was anion, solvent, atmosphere, temperature, or pH of the solution. In addition, temperature dependent reversible polymorphic transition, with self-healing property of cis-[Ni(H2O)2(HGlyam)2]I2 crystals was studied. In reactions involving 2,2'-iminodiacetamide 7 new bis(tridentate) coordination compounds with cobalt(II) and nickel(II) were prepared and structurally characterized. Moreover, 22 ternary coordination compounds of copper(II) with α-amino acids (glycine, L-serine, L-homoserine) and heterocyclic bases (2,2'-bipyridine and 1,10-phenanthroline) were synthesized and structurally characterized. For some compounds, the mechanism of interconversion of different solvatomorphs in the solid-state was successfully determined, which is the first such study on this group of compounds

Structural transformations in complexes of cobalt, nickel and copper with selected α-amino acids and their derivatives

Istražene su reakcije kobaltovih(II), niklovih(II) te bakrovih(II) soli s glicinamidom (HGlyam), D-allo- i L-izoleucinom te L-homoserinom s ciljem priređivanja bis(didentatnih) koordinacijskih spojeva. Priređeno je i strukturno karakterizirano 17 bis(didentatnih) i jedan tris(didentatni) koordinacijski spoj te je proučena cis-trans izomerizacija u otopini i u čvrstom stanju. Utvrđena je značajna uloga metalnog iona u kristalizaciji određenog izomera, a također ključan čimbenik može biti anion, otapalo, atmosfera, temperatura i pH-vrijednost otopine. Dodatno je proučen temperaturno ovisan reverzibilan polimorfni prijelaz u spoju cis-[Ni(H2O)2(HGlyam)2]I2 čiji kristali pokazuju zanimljivo svojstvo samocijeljenja. U reakcijama s 2,2'-iminodiacetamidom priređeno je i strukturno karakterizirano 7 bis(tridentatnih) spojeva kobalta(II) i nikla(II). Priređena su i strukturno karakterizirana 22 ternarna koordinacijska spoja bakra(II) s α-aminokiselinama (glicin, L-serin i L-homoserin) i heterocikličkim bazama (2,2’-bipiridin i 1,10-fenantrolin). U nekoliko slučajeva uspješno je određen mehanizam međupretvorbe različitih solvata u čvrstom stanju, što je prvo takvo istraživanje na ovoj skupini spojeva.Reactions of cobalt(II), nickel(II), and copper(II) salts with glycinamide (HGlyam), D-allo- and L-isoleucine, and L-homoserine were investigated and 17 bis(bidentate) and one tris(bidentate) coordination compounds were prepared and structurally characterized. Cis-trans isomerization of bis(bidentate) compounds in solution and solid-state was studied. The role of a metal ion in the crystallization of a certain isomer was determined, however, in some cases the key factor was anion, solvent, atmosphere, temperature, or pH of the solution. In addition, temperature dependent reversible polymorphic transition, with self-healing property of cis-[Ni(H2O)2(HGlyam)2]I2 crystals was studied. In reactions involving 2,2'-iminodiacetamide 7 new bis(tridentate) coordination compounds with cobalt(II) and nickel(II) were prepared and structurally characterized. Moreover, 22 ternary coordination compounds of copper(II) with α-amino acids (glycine, L-serine, L-homoserine) and heterocyclic bases (2,2'-bipyridine and 1,10-phenanthroline) were synthesized and structurally characterized. For some compounds, the mechanism of interconversion of different solvatomorphs in the solid-state was successfully determined, which is the first such study on this group of compounds

Structural transformations in complexes of cobalt, nickel and copper with selected α-amino acids and their derivatives

Istražene su reakcije kobaltovih(II), niklovih(II) te bakrovih(II) soli s glicinamidom (HGlyam), D-allo- i L-izoleucinom te L-homoserinom s ciljem priređivanja bis(didentatnih) koordinacijskih spojeva. Priređeno je i strukturno karakterizirano 17 bis(didentatnih) i jedan tris(didentatni) koordinacijski spoj te je proučena cis-trans izomerizacija u otopini i u čvrstom stanju. Utvrđena je značajna uloga metalnog iona u kristalizaciji određenog izomera, a također ključan čimbenik može biti anion, otapalo, atmosfera, temperatura i pH-vrijednost otopine. Dodatno je proučen temperaturno ovisan reverzibilan polimorfni prijelaz u spoju cis-[Ni(H2O)2(HGlyam)2]I2 čiji kristali pokazuju zanimljivo svojstvo samocijeljenja. U reakcijama s 2,2'-iminodiacetamidom priređeno je i strukturno karakterizirano 7 bis(tridentatnih) spojeva kobalta(II) i nikla(II). Priređena su i strukturno karakterizirana 22 ternarna koordinacijska spoja bakra(II) s α-aminokiselinama (glicin, L-serin i L-homoserin) i heterocikličkim bazama (2,2’-bipiridin i 1,10-fenantrolin). U nekoliko slučajeva uspješno je određen mehanizam međupretvorbe različitih solvata u čvrstom stanju, što je prvo takvo istraživanje na ovoj skupini spojeva.Reactions of cobalt(II), nickel(II), and copper(II) salts with glycinamide (HGlyam), D-allo- and L-isoleucine, and L-homoserine were investigated and 17 bis(bidentate) and one tris(bidentate) coordination compounds were prepared and structurally characterized. Cis-trans isomerization of bis(bidentate) compounds in solution and solid-state was studied. The role of a metal ion in the crystallization of a certain isomer was determined, however, in some cases the key factor was anion, solvent, atmosphere, temperature, or pH of the solution. In addition, temperature dependent reversible polymorphic transition, with self-healing property of cis-[Ni(H2O)2(HGlyam)2]I2 crystals was studied. In reactions involving 2,2'-iminodiacetamide 7 new bis(tridentate) coordination compounds with cobalt(II) and nickel(II) were prepared and structurally characterized. Moreover, 22 ternary coordination compounds of copper(II) with α-amino acids (glycine, L-serine, L-homoserine) and heterocyclic bases (2,2'-bipyridine and 1,10-phenanthroline) were synthesized and structurally characterized. For some compounds, the mechanism of interconversion of different solvatomorphs in the solid-state was successfully determined, which is the first such study on this group of compounds

Impact of the Zn source on the RSN-type zeolite formation

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