By the direct-synthesis of zinc oxide, nickel hydroxocarbonate with ethylenediaminedisuccinic acid was obtained a heterometallic complex of the composition C10H22N2Ni0.30O13Zn1.70. The crystal structure of this compound was characterized by X-ray diffraction analysis, absorption and IR-spectroscopy. The complex crystallizes in a triclinic system (spatial group P-1) with parameters of the elementary cell a=8,6844(3), b=10,4442(3), c=11,2520(3). The final values of the divergence factors R1=0,0581, wR2=0,0828, GOF 0,964 at reflections with I> 2σ (I). The final electronic difference from the Fourier series of the last-minute refinement cycle is 0.348 and -0.485 e/Å3. The heterometallic complex has a polymer structure, formed by structural units (NiEDDS)- and ZnOEDDS(H2O), which are bidentarily bound via atoms of the oxygen of the β-carboxyl group performing the bridge function and the oxygen atoms of the other three carboxyl groups of the ligand with their monodendental coordinates up to zinc atoms. In the ZnNiEDDS complex, the Ni2+ ion is coordinated with 5 donor atoms of the deprotonated anion EDDS4-, forming a distorted octahedral NiN2O4 environment. At the same time, three 5-membered (two glycine (Gly) and one ethylenediamine (En)) and one 6-membered β-alanine (Al) non-flat metallocycles are formed. Gly is simultaneously three 5-membered and one 6-membered non-flat metallocycles. -cycle, one-cycle Two 5-membered (En NiN2C6C5N1, Gly NiO5C8C7N2) 6-membered Al NiN1C4C3C2O3 cycles are located in the equatorial plane of the octahedron. The glitinous cycle of NiN1C4C1O2 is located in the axial plane of the coordination polyhedron and bound by C4N1 bonds with two cycles, En and Al. The molecule of water is in the axial plane, completing the structure of the polyhedron to the octahedral. In the axial position of the octahedron is a nitrogen atom N1, which, due to the stiffness of the ethylene diamine bridge structure, forms an angle N1-Ni-N2 with inequalities of Ni-N2 (2.151(3) Å) and Ni-N1 (2.108(3) Å), which leads to the formation of tetragonal distortion of the octahedron. The Zn2+ ion is bound to oxygen atoms of β-carboxylic groups of three different EDDS molecules, two of which are coordinated monodentally, and one is bidentanic, and with one molecule of water. In this case, one 4-membered cycle of ZnO7iC9iO8i is formed due to the β-carboxyl group of one of the EDDS molecules. The five-coordinated zinc ion forms a trigonal-bipimaramal distorted square pyramid, at the top of which is the atom of oxygen of the water molecule. In the complex there are molecules of crystallization water, which take part in the formation of the hydrogen bonds system. The distance of hydrogen bonds is in the range of 1.85 (4) - 3.378 (5) Å.
In the asymmetric unit of the title coordination polymer, {[CoNa(C10H12N2O8)(H2O)2]·2H2O}n, the CoII ion is coordinated in a distorted octahedral environment, defined by two N atoms and four carboxylate O atoms. Two CoII ions and two 2-({2-[(1,2-dicarboxylatoethyl)amino]ethyl}amino)butanedioate (EDDS) ligands form a dimeric complex dianion [Co2(EDDS)2]. These dimeric units are connected via Na+ ions, forming a three-dimensional polymeric structure. In the crystal, the ligand N—H groups and the coordinated and solvent water molecules are involved in intermolecular N—H⋯O and O—H⋯O hydrogen bonding, reinforcing the three-dimensional polymeric structure.
New complexes of 3d-metals (Co2+, Ni2+, Zn2+) with bis(phosphonomethyl)aminosuccinic acid (H6BPMAS) have been synthesized. The complexes were studied in aqueous solutions at ratios M2+:H6BPMAS = 1:1 in a wide pH range (1÷10). Regardless of the nature of the metal, the formation of complexes of the general composition [M(HnBPMAS)(OH)m] (n= 4÷0, m=1÷0) is shown. The stability constants of the formed differently protonated complexes are calculated and diagrams of their distribution are plotted. It is shown that the process of complexation takes place most completely in the region of pH>4. For all bis(phosphonomethyl)aminosuccinates of 3d metals, the dominance of the complex with one form of the ligand occurs in approximately the same pH ranges. A close order of change in the values of lgKst. complexes testifies to the same type of structure of their internal coordination sphere. Solid complexes of the composition Na4[MBPMAS]⋅4H2O were synthesized. Their composition, structure, and thermal characteristics were determined by the set of methods such as diffuse reflectance spectroscopy, IR spectroscopy, DTA and non-quantitative mass spectrometry. It is proved that the complexes have the structure of a distorted octahedron, in which the 3-d metal ions are bound to the oxygen atoms of the carboxyl and phosphonic groups and the tertiary nitrogen atom of the ligand. At the same time, two 5-membered (aminomethylenephosphonic and glycine) and one 6-membered (β-alanine) metallocycles are formed in bis(phosphonomethyl)aminosuccinates. The biological activity of H6BPMAS and its complexes with Ni(II) and Co(II) against non-pathogenic bacterial species of microorganisms Pseudomonas fluorescens and Pseudomonas aureofaciens was studied. The study of the activity of substances was carried out in a liquid sterile Hiss medium. The maximum stimulating effect on the growth of bacterial cultures for the studied compounds was recorded at a concentration of 1 µM in 24 hours after the start of cultivation of microorganisms. The highest growth of microorganisms was recorded for metal complexes (50% Na4[CoBPMAS]·4H2O and 35% Na4[NiBPMAS]·4H2O). The maximum stimulating effect on the growth of bacterial cultures is shown by the Co(II) complex, which is able to initiate the synthesis of one of the most important growth hormones - heteroauxin.
Complexation in M (II) – Rut systems (M(II) = Co, Cu) was studied by electron absorption spectroscopy and pH-metric titration in water-ethanol solutions depending on the metal: ligand ratio (1: 1; 2: 1) and the pH of the medium. It was shown that the structure and stoichiometric composition of the complexation reaction products are influenced by such basic parameters as L:M and the pH value of the medium. Depending on the pH value, chelation involves certain binding sites, which primarily is associated with the redistribution of the electron density in the flavonoid molecule. In a weakly acidic or neutral medium, regardless of the M(II): Rut ratio, the formation of monoligand complexes of rutin with 3-d metals occurs with the participation of 5-OH and 4-C=O fragments of the A and C rings, and in an alkaline medium, chelation proceeds on the catecholic fragment of ring B rutin. Biligand complexes are formed with the participation of the gydroxo groups of the catechol fragment of each rutin molecule, and the formation of compounds with a ratio of 2:1 occurs both due to 5-OH and 4C=O and due to 3 ', 4'-OH groups. The calculated values of the stability constants of the complexes showed that the stability of the Co (II) complexes is several orders of magnitude lower than the stability of the corresponding Cu (II) complexes.
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