Search

Objective: The objective of this study is to synthesize and comprehensively characterize a novel iodine-containing coordination compound, di-aminopropionic acid hydrogen tri-iodide. This involves determining its structural, physicochemical, and thermal properties, as well as evaluating its antimicrobial activity against a range of bacterial strains, including multidrug-resistant pathogens. The aim is to explore the potential of this compound as a candidate for developing new antibacterial agents to address the challenge of antibiotic resistance. Results: An original iodine-containing semiorganic coordination compound was synthesized and characterized. The physicochemical properties were studied via diffraction, FTIR spectroscopy and thermogravimetric/differential scanning calorimetry (TG/DSC). In vitro antimicrobial activity evaluation was performed using two-fold serial dilution method. The obtained results demonstrated efficiency against both gram-positive (Staphylococcus aureus) and gram-negative (Escherichia coli, Pseudomonas aeruginosa, Acinetobacter baumannii) bacteria including MDR strains that cause infectious disease. The results of the antibacterial evaluation revealed that the new iodine coordination compound – di-aminopropionic acid hydrogen tri-iodide possesses high bactericidal properties and exhibits better antimicrobial activity against both susceptible and multidrug-resistant strains than does Lugol solution and ampicillin sodium, which are used as reference drugs. [ABSTRACT FROM AUTHOR]

Two new compounds - a mononuclear nickel(II) compound with di-p-tolylglyoxime (DpatH2) - [Ni(DpatH2)3]SO4∙1,4-H2bdc∙2.5DMF∙H2O (1) and a binuclear manganese(II) compound with dianilineglyoxime (DAnH2) - [Mn2(DAnH2)2(1,3-bdc)2(DMSO)4] (2) (1,4- and 1,3-bdc are 1,4- and 1,3-benzenedicarboxylic acids, respectively) have been obtained. The IR spectra of the complexes were studied and molecular and crystal structures of the compounds were determined by single crystal X-ray diffraction method. Compound 1 has an ionic structure and contains a complex cation in which three neutral DpatH2 ligands are coordinated to the nickel atom. Complex 2 is a molecular binuclear complex in which, in addition to the two neutral ligands DAnH2 and four DMSO molecules, two 1,3-benzenedicarboxylic anions are coordinated to the metal atoms in a bridging manner.

Synthesis and full characterization of a new coordination compound, which was synthesized by mixed ligands under hydrothermal condition, namely [Cu(L)2(phen)2(H2O)2]·4H2O (1) (phen = 1,10-phenanthroline, H2L = 3-carboxy-1-carboxymethyl-2-oxidopyridinium). Cu(II) is six-coordinated in a slightly twisted [CuN2O4] octahedral geometry. 1 displays 2D supramolecular layer, which is further extended into a 3D network by the π-π stacking and hydrogen bonds. 3D Hirshfeld surface analysis is combined with 2D fingerprint plots to investigate the contribution of different intermolecular interactions within the crystal. DFT calculations are also performed. [ABSTRACT FROM AUTHOR]

Cobalt sulfide, a class of metal chalcogenide with tunable electronic structure and component distribution, has attracted considerable interest in renewable energy conversion and utilization. In this work, we report a facile, efficient and scalable method to synthesize Co9S8 supported on nitrogen and sulfur co doped porous carbon (Co9S8/N,S‐PC) hybrid from the annealing treatment of a coordination compound assembled by 2‐mercaptobenzimidazole, 4,4‐bipyridine and cobalt salt. The heteroatom of organic ligand could efficiently tune the electronic properties of Co9S8 nanoparticles and well‐designed carbon. Meanwhile the interaction of organic ligands provides a platform for the high dispersion of Co9S8. Owing to the synergetic effect, the Co9S8/N,S‐PC catalyst shows an admirable oxygen reduction reaction (ORR) activity with the E1/2 of 0.804 V vs. RHE, together with good durability, and tolerance to methanol poisoning in alkaline media. [ABSTRACT FROM AUTHOR]

Candida species undeniably rank as the most prevalent opportunistic human fungal pathogens worldwide, with Candida albicans as the predominant representative. However, the emergence of non-albicans Candida species (NACs) has marked a significant shift, accompanied by rising incidence rates and concerning trends of antifungal resistance. The search for new strategies to combat antifungal-resistant Candida strains is of paramount importance. Recently, our research group reported the anti-Candida activity of a coordination compound containing copper(II) complexed with theophylline (theo) and 1,10-phenanthroline (phen), known as "CTP" – Cu(theo)2phen(H2O).5H2O. In the present work, we investigated the mechanisms of action of CTP against six medically relevant, antifungal-resistant NACs, including C. auris, C. glabrata, C. haemulonii, C. krusei, C. parapsilosis and C. tropicalis. CTP demonstrated significant efficacy in inhibiting mitochondrial dehydrogenases, leading to heightened intracellular reactive oxygen species production. CTP treatment resulted in substantial damage to the plasma membrane, as evidenced by the passive incorporation of propidium iodide, and induced DNA fragmentation as revealed by the TUNEL assay. Scanning electron microscopy images of post-CTP treatment NACs further illustrated profound alterations in the fungal surface morphology, including invaginations, cavitations and lysis. These surface modifications significantly impacted the ability of Candida cells to adhere to a polystyrene surface and to form robust biofilm structures. Moreover, CTP was effective in disassembling mature biofilms formed by these NACs. In conclusion, CTP represents a promising avenue for the development of novel antifungals with innovative mechanisms of action against clinically relevant NACs that are resistant to antifungals commonly used in clinical settings. [ABSTRACT FROM AUTHOR]

A dinuclear metal‐organic cage with four acrylate side chains was prepared by self‐assembly. Precipitation polymerization of the cage with N‐isopropylacrylamide yielded a thermoresponsive nanogel. The host properties of the cage were retained within the gel matrix, endowing the nanogel with the capability to serve as a sorbent for chloride ions in water. Moreover, a heteroleptic cage with the drug abiraterone as co‐ligand was integrated into a nanogel. The addition of chloride ions induced a structural rearrangement of the metal‐ligand assembly, resulting in the gradual release of abiraterone. [ABSTRACT FROM AUTHOR]

The coordination compound [NiCl2L(2-PrOH)]n (where L is 2-(4-bromophenoxy)acetohydrazide; 2-PrOH is isopropanol) was obtained for the first time. The complex was characterized by means of elemental analyses, molar conductance, thermogravimetric analysis, IR spectroscopy, and single crystal X-ray diffraction analysis. It was determined that the coordination compound exhibits a polymeric structure. The complexing agent is six-coordinated, and its distorted octahedron forms due to the bidentate coordination of 2-(4-bromophenoxy)acetohydrazide through the carbonyl oxygen atom and the amine nitrogen. The oxygen of the molecule of isopropanol, the chlorine atom, and two chlorine atoms serve as bridges between two metal atoms. [ABSTRACT FROM AUTHOR]

A lutetium(III) complex based on the anion of the ligand dimethyl (2,2,2-trichloroacetyl)phosphoramidate (HL) and tetraphenylphosphonium, of composition PPh4[LuL4] (L = CAPh = carbacylamidophosphate), or (C24H20)[Lu(C4H6Cl3NO4P)4], has been synthesized and structurally characterized. The X-ray diffraction study of the compound revealed that the lutetium ion is surrounded by four bis-chelating CAPh ligands, forming the complex anion [LuL4]− with a coordination number of 8[O] for LuIII, while PPh4+ serves as a counter-ion. The coordination geometry around the Lu3+ ion was determined to be a nearly perfect triangular dodecahedron. The complex crystallizes in the monoclinic crystal system, space group P21/c, with four molecules in the unit cell. Weak hydrogen bonds O...HC(Ph), Cl...HC(Ph) and N...HC(Ph) are formed between the cations and anions. For a comparative study, HL-based structures were retrieved from the Cambridge Structural Database (CSD) and their geometries and conformations are discussed. A Hirshfeld surface analysis was also performed.

A lutetium(III) complex based on the anion of the ligand dimethyl (2,2,2-trichloroacetyl) phosphoramidate (HL) and tetraphenylphosphonium, of composition PPh4[LuL4] (L = CAPh = carbacylamidophosphate), or (C24H20)-[Lu(C4H6Cl3NO4P)4], has been synthesized and structurally characterized. The X-ray diffraction study of the compound revealed that the lutetium ion is surrounded by four bis-chelating CAPh ligands, forming the complex anion [LuL4]- with a coordination number of 8[O] for LuIII, while PPh4+ serves as a counter-ion. The coordination geometry around the Lu3+ ion was determined to be a nearly perfect triangular dodecahedron. The complex crystallizes in the monoclinic crystal system, space group P21/c, with four molecules in the unit cell. Weak hydrogen bonds O⋯HC(Ph), Cl⋯HC(Ph) and N⋯HC(Ph) are formed between the cations and anions. For a comparative study, HL-based structures were retrieved from the Cambridge Structural Database (CSD) and their geometries and conformations are discussed. A Hirshfeld surface analysis was also performed. [ABSTRACT FROM AUTHOR]

Template condensation of S-methylisothiosemicarbazones of acetyl- or benzoylacetone with 8‑quinolinecarboxaldehyde in the presence of nickel(II) and copper(II) ions gave four new mononuclear coordination compounds [NiL1]I (I), [CuL1I] (II), [NiL2]I (III), and [CuL2I] (IV). The chemical composition of the products was confirmed by elemental analysis, IR spectroscopy, and mass spectrometry, and the crystal structure of compounds I and II was determined by X-ray diffraction analysis (CCDC nos. 2266386, 2266387). X-ray diffraction study revealed a square planar coordination environment of the central ion of the cationic Ni(II) complex and square pyramidal geometry for the molecular Cu(II) complex. [ABSTRACT FROM AUTHOR]

The title compound, [Ni2(C8H6N3)2(C2H3O2)2(C5H8N2)2] or [Ni(μ-OOCCH3)(2-PyPz)(Me2PzH)]2 (1) [2-PyPz = 3-(pyridin-2-yl) pyrazole; Me2PzH = 3,5-dimethyl pyrazole] was synthesized from Ni(OOCCH3)2·4H2O, 2-PyPzH, Me2PzH and triethylamine as a base. Compound 1 {[Ni2(C30H34N10Ni2O4)]} at 100 K has monoclinic (P21/n) symmetry and the molecules have crystallographic inversion symmetry. Molecules of 1 comprise an almost planar dinuclear NiII core with an N4O2 coordination environment. The equatorial plane consists of N3,O coordination derived from one of the bidentate acetate O atoms and three of the N atoms of the chelating 2-PyPz ligand while the axial positions are occupied by neutral Me2PzH and the second O atom of the acetate unit. The Ni atoms are bridged by the nitrogen atom of a deprotonated 2-PyPz ligand. Compound 1 exhibits various inter- and intramolecular C—H...O and N—H...O hydrogen bonds.

The reaction of Co(NCS)2 with 4-methylpyridine N-oxide (C6H7NO) leads to the formation of two compounds, namely, tetrakis(4-methylpyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II), [Co(NCS)2(C6H7NO)4] (1), and tris(4-methylpyridine N-oxide-κO)bis(thiocyanato-κN)cobalt(II), [Co(NCS)2(C6H7NO)3] (2). The asymmetric unit of 1 consists of one CoII cation located on a centre of inversion, as well as one thiocyanate anion and two 4-methylpyridine N-oxide coligands in general positions. The CoII cations are octahedrally coordinated by two terminal N-bonding thiocyanate anions in trans positions and four 4-methylpyridine N-oxide ligands. In the extended structure, these complexes are linked by C—H...O and C—H...S interactions. In compound 2, two crystallographically independent complexes are present, which occupy general positions. In each of these complexes, the CoII cations are coordinated in a trigonal–bipyramidal manner by two terminal N-bonding thiocyanate anions in axial positions and by three 4-methylpyridine N-oxide ligands in equatorial positions. In the crystal, these complex molecules are linked by C—H...S interactions. For compound 2, a nonmerohedral twin refinement was performed. Powder X-ray diffraction (PXRD) reveals that 2 was nearly obtained as a pure phase, which is not possible for compound 1. Differential thermoanalysis and thermogravimetry data (DTA–TG) show that compound 2 start to decompose at about 518 K.

Novel supramolecular cation-anionic coordination compound (HPhen)4[(μ-O){Ge2(OH) (μ-Tart)2}2]·9H2O was synthesised and characterised by the X-ray, elemental, IR- and Hirshfeld surface analysis. It was established that original synthesis method and ability of 1,10-phenanthroline to be protonated promotes the formation of [(μ-O){Ge2(OH)(μ-Tart)2}2]4- anion. In this anion, dimeric fragments are connected by a bridging oxygen atom, and the coordination polyhedra around the germanium atoms adopt a distorted trigonal bipyramidal geometry. The cations HPhen+ serve as effective building blocks, strengthening the overall structure through classical hydrogen bonding and additional π-π stacking interactions. Biological screening of (HPhen)4[(μ-O){Ge2(OH) (μ-Tart)2}2]·9H2O demonstrated its remarkable enzyme-effector and antimicrobial activity. The compounds' efficacy can be attributed to the synergistic effects of the independent cations and anions, as well as the ability of protonated 1,10-phenanthroline to inhibit metal ions in enzymes and form stacking interactions with specific protein components. These characteristics make such compounds highly effective and promising antibacterial agents that minimize the risk of developing bacterial resistance.

The title coordination compound, [Cd(C2H3O2)2(C6H14N2O)2]·4H2O, was synthesized by mixing 2 moles of 4-(2-aminoethyl)morpholine and 1 mole of cadmium acetate in double-distilled water. The Cd atom is octahedrally coordinated by two N,N′-bidentate ligands [4-(2-aminoethyl)morpholine] and two trans-located acetate molecules. The Cd atom is located on a center of inversion, whereas the 4-(2-aminoethyl)morpholine and four water molecules are adjacent to the acetate molecules. The chair conformation of the morpholine molecules is confirmed. In the crystal, adjacent metal complexes and uncoordinated water molecules are linked via N—H...O and O—H...O hydrogen-bonding interactions, generating R22(6), R66(16), R66(20) and S11(6) motifs and forming a three-dimensional network. A Hirshfeld surface analysis indicated the contributions of various contacts: H...H (71.8%), O...H/H...O (27.1%), and C...H/H...C (1.0%).

The title compound, [Co(SCN)2(C6H4N2O)4], was prepared by the reaction of cobalt(II)thiocyanate with 3-cyanopyridine N-oxide in ethanol. In the crystal, the cobalt(II) cations are octahedrally coordinated by two terminal N-bonded thiocyanate anions and four O-bonded 3-cyanopyridine N-oxide coligands, forming discrete complexes that are located on centers of inversion, hence forming trans-CoN2O4 octahedra. The structure refinement was performed in the monoclinic space group P21/n, for which a potential lattice translation and new symmetry elements with a fit of 100% is suggested. The structure can easily be refined in the space group I2/m, where the complexes have 2/m symmetry. However, nearly all of the reflections that violate the centering are observed with significant intensity and the refinement in P21/n leads to significantly lower R(F) values (0.027 versus 0.033). Moreover, in I2/m much larger components of the anisotropic displacement parameters are observed and therefore, the crystal structure is presented in the primitive unit cell. IR investigations confirm that the anionic ligands are only terminally bonded and that the cyano group is not involved in the metal coordination. PXRD investigations show that a pure crystalline phase has been obtained and measurements using simultaneously thermogravimetry and differential thermoanalysis reveal that the compound decomposes in an exothermic reaction upon heating, without the formation of a coligand-deficient intermediate phase.

3-Methylbenzoic acid (3-mbH) and 2,2′-bipyridine (bipy) reacted with a copper(II) salt forming a new mixed ligand complex, aqua(2,2′-bipyridine-κ2N,N′)bis(3-methylbenzoato)-κ2O,O′;κO-copper(II) 0.68-hydrate, [Cu(C8H7O2)2(C10H8N2)(H2O)]·0.68H2O or [Cu(3-mb)2(bipy)(H2O)]·0.68H2O. The coordination environment of CuII is a distorted octahedron. The metal atom is attached to two 3-mb moieties, which bind in monodentate and bidentate fashions. One of the 3-mb units is disordered. The coordination environment is completed by one bipy ligand and a water molecule. A second water molecule is outside the coordination sphere of the CuII atom and its occupancy refined to 0.68. The structure consists of chains along the b-axis direction formed by complex units joined via hydrogen bonds between the coordinated water molecule and an O atom of a coordinated 3-mb unit. Hirshfeld surface analysis indicates that the most abundant contacts are H...H (56.8%), H...C/C...H (21.7%) and H...O/O...H (13.7%).

The use of acetic acid (HOAc) in a reaction between CuCl2·2H2O and secnidazole, an active pharmaceutical ingredient useful in the treatment against a variety of anaerobic Gram-positive and Gram-negative bacteria, affords the title complex, [CuCl2(C7H11N3O3)2]. This compound was previously synthesized using ethanol as solvent, although its crystal structure was not reported [Betanzos-Lara et al. (2013). Inorg. Chim. Acta, 397, 94–100]. In the molecular complex, the Cu2+ cation is situated at an inversion centre and displays a square-planar coordination environment. There is a hydrogen-bonded framework based on intermolecular O—H...Cl interactions, characterized by H...Cl separations of 2.28 (4) Å and O—H...Cl angles of 175 (3)°. The resulting supramolecular network is based on R22(18) ring motifs, forming chains in the [010] direction.

The title complex, [Cu(C8H18NO5)Cl] or [Cu(H4bis-tris)Cl], was obtained starting from the previously reported [Cu(H5bis-tris)Cl]Cl compound. The deprotonation of the aminopolyol ligand H5bis-tris {[bis(2-hydroxyethyl)amino]tris(hydroxymethyl)methane, C8H19NO5} promotes the formation of a very strong O—H...O intermolecular hydrogen bond, characterized by an H...O separation of 1.553 (19) Å and an O—H...O angle of 178 (4)°. The remaining hydroxy groups are also engaged in hydrogen bonds, forming R22(8), R44(16), R44(20) and R44(22) ring motifs, which stabilize the triperiodic supramolecular network.

Proteases, that are able to hydrolyze the peptide bonds in proteins and polypeptides, occupy a key position in diverse fields, such as food, agriculture, animal feed. Considering the increasing demand for microbial proteases, identification of new way for improving the productivity of producers is of great importance. The aim of the present study was to evaluate the effect of a new coordination compound [Fe(H2L)(H2O)2](NO3)3∙2.5H2O (where H2L = 2,6-diacetylpyridine bis(picolinoylhydrazone)) on the activity of proteolytic complex synthesized by the micromycete Fusarium gibbosum CNMN FD 12 under the submerged fermentations in shake flask, as well as in lab-scale fermenter. It was found that [Fe(H2L)(H2O)2](NO3)3∙2.5H2O exerts a significant positive effect on proteolytic activity in F. gibbosum CNMN FD 12 both in flasks and bioreactor and can be used as stimulator and regulator of proteases activity. By varying the concentration of the coordination compound and the duration of cultivation, it is possible to obtain proteolytic complexes enriched in different types of proteases (acid, neutral or alkaline), depending on the practical needs.

The title compound, trans-dibromidotetrakis(5-methyl-1H-pyrazole-κN2)manganese(II), [MnBr2(C4H6N2)4] or [Mn(3-MePzH)4Br2] (1) crystallizes in the triclinic P\overline{1} space group with the cell parameters a = 7.6288 (3), b = 8.7530 (4), c = 9.3794 (4) Å and α = 90.707 (4), β = 106.138 (4), γ = 114.285 (5)°, V = 542.62 (5) Å3, T = 120 K. The asymmetric unit contains only half the molecule with the manganese atom is situated on a crystallographic inversion center. The 3-MePzH ligands are present in an AABB type manner with two methyl groups pointing up and the other two down. The supramolecular architecture is characterized by several intermolecular C—H...N, N—H...Br, and C—H...π interactions. Earlier, a polymorphic structure of [Mn(3-MePzH)4Br2] (2) with a similar geometry and also an AABB arrangement for the pyrazole ligands was described [Reedijk et al. (1971). Inorg. Chem. 10, 2594–2599; a = 8.802 (6), b = 9.695 (5), c = 7.613 (8) Å and α = 105.12 (4), β = 114.98 (4), γ = 92.90 (3)°, V = 558.826 (5) Å3, T = 295 K]. A varying supramolecular pattern was reported, with the structure of 1 featuring a herringbone type pattern while that of structure 2 shows a pillared network type of arrangement along the a axis. A nickel complex [Ni(3-MePzH)4Br2] isomorphic to 1 and the analogous chloro derivatives of FeII, CoII and CuII are also known.

The structure of the title compound, [RuCl2(C7H10N2)2(C2H6OS)2], has monoclinic (P21/n) symmetry. The Ru—N distances of the coordination compound are influenced by the trans chloride or dimethylsulfoxide-κS ligands. The molecular structure exhibits disorder for two of the terminal methyl groups of a dimethyl sulfoxide ligand.

The reaction of Co(NCS)2 with 4-methylpyridine N-oxide (C6H7NO) leads to the formation of two compounds, namely, tetrakis(4-methylpyridine N-oxide-O)bis(thiocyanato-N)cobalt(II), [Co(NCS)2(C6H7NO)4] (1), and tris(4-methylpyridine N-oxide-O)bis(thiocyanato-N)cobalt(II), [Co(NCS)2(C6H7NO)3] (2). The asymmetric unit of 1 consists of one CoII cation located on a centre of inversion, as well as one thiocyanate anion and two 4-methylpyridine N-oxide coligands in general positions. The CoII cations are octahedrally coordinated by two terminal N-bonding thiocyanate anions in trans positions and four 4-methylpyridine N-oxide ligands. In the extended structure, these complexes are linked by C--H...O and C--H...S interactions. In compound 2, two crystallographically independent complexes are present, which occupy general positions. In each of these complexes, the CoII cations are coordinated in a trigonal-bipyramidal manner by two terminal N-bonding thiocyanate anions in axial positions and by three 4-methylpyridine N-oxide ligands in equatorial positions. In the crystal, these complex molecules are linked by C--H...S interactions. For compound 2, a nonmerohedral twin refinement was performed. Powder X-ray diffraction (PXRD) reveals that 2 was nearly obtained as a pure phase, which is not possible for compound 1. Differential thermoanalysis and thermogravimetry data (DTA-TG) show that compound 2 start to decompose at about 518K. [ABSTRACT FROM AUTHOR]

Background. Coordination compounds can exhibit phase transitions: dissolution, solvation loss, desolvation, dehydration, and polymorphic transitions. Understanding them is important for optimizing the synthesis process, controlling crystal growth, and studying the state of coordination compounds in various environments. Purpose. Synthesis of a complex compound containing [Mn(BZA)4Cl2], its thermogravimetric and differential thermal analysis. Methodology. During the synthesis process, a magnetic stirrer was used and studied by thermogravimetric and differential thermal analysis (Model: KL-JS-100A). Originality. The conditions for the synthesis of coordination compounds with the general formula [Mn(BZA)4Cl2] were identified and their structure was determined by physical research methods. Findings. Having performed TGA and DTA of the metal complex, we gained an understanding of its thermal stability, behavior during decomposition and thermal phenomena, which can be used to determine the properties of the complex and prospects for use. [ABSTRACT FROM AUTHOR]

Background. Studying the structures of coordination compounds, including organometallic ones, is an important condition for the synthesis of biopharmaceuticals with predetermined properties. Purpose. Synthesis of the [(Cu(CH3COO)2)4(EDA)2(H2O)2](PNA)2 complex and identification of its composition and structure by physical research methods. Methodology. The structure of complex compounds was studied using X-ray diffraction analysis, infrared (Bruker Invenio S-2021), ultraviolet (Specord 200 Plus), spectroscopic, thermogravimetric and differential thermal analysis (KL-JS-100A). Originality. The optimal conditions for the synthesis of coordination compounds [(Cu(CH3COO)2)4(EDA)2(H2O)2](PNA)2 were identified and their structure was determined by physical research methods. Findings. A successful result was noted in the synthesis of a new copper acetate complex containing the ligands: ethylenediamine EDA and p-nitroaniline (PNA), as well as the formation of coordination bonds with four monodentate ligands (CH3COO-), EDA serve as bidentate ligands forming coordination bonds with the copper ion through nitrogen atoms . [ABSTRACT FROM AUTHOR]

The reactions in the Cu(OAc)2⋅H2O–phytic acid–2,2'-bipyridine (bpy) system in aqueous methanol solutions resulted in the formation of a molecular different-ligand tetranuclear complex [(Cu4(bpy)4(PO4)2(CO3)(H2O)2]⋅13H2O (I), the structure of which was established from the X-ray diffraction data (CCDC no. 2262998). The molecule of complex I contains four non-equivalent Cu2+ cations, coordinating each two phosphate anions ( remaining after the transformation of the phytate ring), four neutral bpy molecules, two water molecules, and one carbonate anion (). The presence of a large number of solvate water molecules in the outer coordination sphere gives rise to a hydrogen-bonded framework involved in stabilization of the crystal packing. Study of the antimycobacterial activity of I against non-pathogenic Mycolicibacterium smegmatis strain revealed high biological efficacy. [ABSTRACT FROM AUTHOR]

A set of substituted 1,4,7-triazacyclononane ligands was synthesised, including a wide series of novel derivatives bearing a thiazole or thiophene side group, with the potential to incorporate these derivatives into a polymeric material; some previously known/studied ligands were also synthesised for comparative purposes. The corresponding copper(II) complexes were prepared, and their ability to mediate the hydrolysis of phosphate ester bonds was studied via UV-Vis spectrophotometry, using bis(p-nitrophenyl)phosphate as a model substrate. Some of the prepared complexes showed a considerable enhancement of the phosphate ester hydrolysis in comparison with previously studied systems, which makes them some of the most effective complexes ever tested for this purpose. Therefore, these novel, potentially bifunctional systems could provide the possibility of creating new coating materials for medicinal devices that could prevent biofilm formation. [ABSTRACT FROM AUTHOR]

The title coordination compound, [Cd(C2H3O2)2(C6H14N2O)2]⋅4H2O, was synthesized by mixing 2 moles of 4-(2-aminoethyl)morpholine and 1 mole of cadmium acetate in double-distilled water. The Cd atom is octahedrally coordinated by two N,N'-bidentate ligands [4-(2-aminoethyl)morpholine] and two trans-located acetate molecules. The Cd atom is located on a center of inversion, whereas the 4-(2-aminoethyl)morpholine and four water molecules are adjacent to the acetate molecules. The chair conformation of the morpholine molecules is confirmed. In the crystal, adjacent metal complexes and uncoordinated water molecules are linked via N--H⋯O and O--H⋯O hydrogenbonding interactions, generating R2²(6), R66(16), R66(20) and S1¹(6) motifs and forming a three-dimensional network. A Hirshfeld surface analysis indicated the contributions of various contacts: H⋯H (71.8%), O⋯H/H⋯O (27.1%), and C⋯H/H⋯C (1.0%). [ABSTRACT FROM AUTHOR]

For the first time, a thiosemicarbazone-type ligand containing a paracetamol structural unit was synthesized. Five new coordination compounds based on copper(II) salts: [Cu(L)CH3COO] (1), [{Cu(L)Cl}2]·H2O (2), [Cu(L)H2O·DMF]NO3 (3), [Cu(L)Br] (4), [Cu(L)H2O]ClO4 (5), were obtained, where HL is N-[4-({2-[1-(pyridin-2-yl)ethylidene]hydrazinecarbothioyl}amino)phenyl]acetamide. The new HL was characterized by NMR, FTIR, spectroscopy, and X-ray crystallography. All copper(II) coordination compounds were characterized by elemental analysis, FTIR, EPR spectroscopy, and molar electrical conductivity. Furthermore, single crystal X-ray diffraction analysis elucidated the structures of thiosemicarbazone HL as well as complexes 1–3. All compounds were tested for antimicrobial, antifungal, and antioxidant activities, and their toxicity to Daphnia magna was studied. Biological evaluation has revealed that most of the synthesized compounds demonstrate promising antibacterial, antifungal, and antioxidant activities. In many cases, their antibacterial/antifungal activity is comparable to that of certain drugs used in medicine for these purposes, and in some cases, even surpasses them. HL and complexes 2–5 exhibit antioxidant activity that surpasses that of Trolox. Furthermore, HL and complex 2 display virtually no toxicity to D. magna. [ABSTRACT FROM AUTHOR]

The title compound, [Co(SCN)2(C6H4N2O)4], was prepared by the reaction of cobalt(II)thiocyanate with 3-cyanopyridine N-oxide in ethanol. In the crystal, the cobalt(II) cations are octahedrally coordinated by two terminal N-bonded thiocyanate anions and four O-bonded 3-cyanopyridine N-oxide coligands, forming discrete complexes that are located on centers of inversion, hence forming trans-CoN2O4 octahedra. The structure refinement was performed in the monoclinic space group P21/n, for which a potential lattice translation and new symmetry elements with a fit of 100% is suggested. The structure can easily be refined in the space group I2/m, where the complexes have 2/m symmetry. However, nearly all of the reflections that violate the centering are observed with significant intensity and the refinement in P21/n leads to significantly lower R(F) values (0.027 versus 0.033). Moreover, in I2/m much larger components of the anisotropic displacement parameters are observed and therefore, the crystal structure is presented in the primitive unit cell. IR investigations confirm that the anionic ligands are only terminally bonded and that the cyano group is not involved in the metal coordination. PXRD investigations show that a pure crystalline phase has been obtained and measurements using simultaneously thermogravimetry and differential thermoanalysis reveal that the compound decomposes in an exothermic reaction upon heating, without the formation of a coligand-deficient intermediate phase. [ABSTRACT FROM AUTHOR]

A europium(III) coordination compound based on thiopheneacrylic acid (Htpa), triaquatris[3-(thiophen-2-yl)prop-2-enoato-κ2O,O′]europium(III)–3-(thiophen-2-yl)prop-2-enoic acid (1/3), [Eu(C7H5O2S)3(H2O)3]·3C7H6O2S or [Eu(tpa)3(H2O)3]·3(Htpa) (1), where tpa is the conjugate base of Htpa, has been synthesized and structurally characterized. Compound 1 crystallizes in the trigonal space group R3. The structure of 1 consists of a discrete molecular complex [Eu(tpa)3(H2O)3] species and the Htpa molecule. In the crystal, the two components are involved in O—H...O [ring motif R22(8)] and C—H...π hydrogen-bonding interactions. These interactions were further investigated by Hirshfeld surface analysis, which showed high contributions of H...H, H...C/C...H and H...O/O...H contacts to the total Hirshfeld surfaces.

Rare-earth (RE, Ln) carboxylates are widely studied as precursors of RE oxide-based nanomaterials; however, no systematic studies of RE L-lactates (HLact = 2-hydroxypropanoic acid) have been reported to date. In the present work, a profound structural investigation of RE L-lactates is carried out. A family of RE lactate complexes of the general formula LnLact3∙nH2O (Ln = La, Ce–Nd, Sm–Lu, Y; n = 2–3) are synthesized and characterized by CHN, TGA, and FTIR as well as by powder and single-crystal XRD methods.The existence of four novel structural types (1-Ln–4-Ln) is revealed. Compounds of the 1-Ln type (Ln = La, Ce, Pr) exhibit a chain polymeric structure, whereas 2-Ln–4-Ln compounds are molecular crystals consisting of dimeric (2-Ln; Ln = La, Ce–Nd) or monomeric (3-Ln–Ln = Sm–Lu, Y; 4-Ln–Ln = Sm–Gd, Y) species. The crystal structures of 1-Ln–4-Ln compounds are discussed in terms of their coordination geometry and supramolecular arrangement. Solutions of yttrium and lanthanum lactates with diethylenetriamine are applied for the chemical deposition of Y2O3 and La2O3 thin films. [ABSTRACT FROM AUTHOR]

3-Methylbenzoic acid (3-mbH) and 2,2'-bipyridine (bipy) reacted with a copper(II) salt forming a new mixed ligand complex, aqua(2,2'-bipyridine-k²N,N')bis(3-methylbenzoato)-k²O,O';kO-copper(II) 0.68-hydrate, [Cu(C8H7O2)2(C10H8N2)(H2O)]·0.68H2O or [Cu(3-mb)2(bipy)(H2O)].0.68H2O. The coordination environment of CuII is a distorted octahedron. The metal atom is attached to two 3-mb moieties, which bind in monodentate and bidentate fashions. One of the 3-mb units is disordered. The coordination environment is completed by one bipy ligand and a water molecule. A second water molecule is outside the coordination sphere of the CuII atom and its occupancy refined to 0.68. The structure consists of chains along the b-axis direction formed by complex units joined via hydrogen bonds between the coordinated water molecule and an O atom of a coordinated 3-mb unit. Hirshfeld surface analysis indicates that the most abundant contacts are H...H (56.8%), H...C/C...H (21.7%) and H...O/O...H (13.7%). [ABSTRACT FROM AUTHOR]

The article includes experimental results related to the productivity of the Spirulina platensis (Nordst.) Geitl - CALU - 835 strain, which was cultivated for 8 days on modified nutrient media supplemented with two coordination compound containing Ca and Ba. A greater amount of biomass was recorded when growing spirulina on the Zarrouk culture medium supplemented with these coordination compounds in a concentration of 5 mg/L, accumulating a fresh biomass of about 13,3 g/L and 12,8 g/L, respectively, or about 14,5% and 9,9% higher than that accumulated by the witness.

The growing worldwide cancer incidence, coupled to the increasing occurrence of multidrug cancer resistance, requires a continuous effort towards the identification of new leads for cancer management. In this work, two C-scorpionate complexes, [FeCl2(κ3-Tpm)] (1) and [Co(κ3-TpmOH)2](NO3)2 (2), (Tpm = hydrotris(pyrazol-1-yl)methane and TpmOH = 2,2,2-tris(pyrazol-1-yl)ethanol), were studied as potential scaffolds for future anticancer drug development. Their cytotoxicity and cell migration inhibitory activity were analyzed, and an untargeted metabolomics approach was employed to elucidate the biological processes significantly affected by these two complexes, using two tumoral cell lines (B16 and HCT116) and a non-tumoral cell line (HaCaT). While [FeCl2(κ3-Tpm)] did not display a significant cytotoxicity, [Co(κ3-TpmOH)2](NO3)2 was particularly cytotoxic against the HCT116 cell line. While [Co(κ3-TpmOH)2](NO3)2 significantly inhibited cell migration in all tested cell lines, [FeCl2(κ3-Tpm)] displayed a mixed activity. From a metabolomics perspective, exposure to [FeCl2(κ3-Tpm)] was associated with changes in various metabolic pathways involving tyrosine, where iron-dependent enzymes are particularly relevant. On the other hand, [Co(κ3-TpmOH)2](NO3)2 was associated with dysregulation of cell adhesion and membrane structural pathways, suggesting that its antiproliferative and anti-migration properties could be due to changes in the overall cellular adhesion mechanisms. [ABSTRACT FROM AUTHOR]

A new trinuclear CuII compound {[Cu3(HL′)2(H2O)2](ClO4)4}·(H2O)4 (1) was obtained and presented a trapped chiral hemiaminal (HL2′ = [(5-amino-4H-1,2,4-triazol-3-yl)amino](1H-imidazol-4-yl)methanol)). Compound 1 shows an almost flat cationic structure [Cu3(HL′)2(H2O)2]4+ with a Cu3 linear core reached by the double Cu-OR/NN-Cu triazole/alkoxo bridge of the hemiaminal molecule. The CuII spin carriers are antiferromagnetically coupled, presenting a spin doublet ground state (S = 1/2) with a magnetic coupling constant of −179 cm−1. Moreover, DTF calculations show that the planarity of the compound permits a sigma-type overlapping between the unpaired electrons of the spin carriers and the p-type orbitals of the coordinated N and O atoms producing an electronic delocalization through the bridging ligand responsible for the strong antiferromagnetic interactions observed experimentally. [ABSTRACT FROM AUTHOR]

A three-dimensional (3-D) 3d-4f polyoxometalate (POM), [Gd2Cu(SiW12O40)(Hpca)4(pca)4(H2O)3]·(Hpca)2·H2O (1) (Hpca = isonicotinic acid, abbreviated as Cu-Gd-CP), was synthesized by hydrothermal method and characterized by XRD, TG, IR, and Ultraviolet–visible (UV–vis) spectra. The Gd3+ ions have two different coordination modes, which correspond to distinct kinds of dinuclear secondary building units, ([Gd12(Hpca)4(pca)4(H2O)2] and [Gd22(Hpca)4(pca)4(H2O)4]). Thus, there are two different types of pores (pore A and pore B) filled by free Hpca molecules in Cu-Gd-CP. The Hpac molecules in pore A are oriented perpendicular to each other in pore B. The electrochemical potential of Cu-Gd-CP is explored. [ABSTRACT FROM AUTHOR]

In order to explore the electrochemical reduction reaction process of trivalent chromium ions, ultraviolet visible spectrophotometry (UV - Vis), linear sweep voltammetry (LSV), cyclic voltammetry (CV) and other methods were used to study the existing forms of the coordination compounds at the initial reduction stage of Cr (Ⅲ) ions in choline chloride - ethylene glycol (ChCl - EG) deep eutectic solvent system, the electrochemical reduction reaction process of Cr (Ⅲ) ions, the apparent activation energy of the reduction process of Cr (Ⅲ) ions in the electrolyte and the control steps of the reduction process. Results showed that at the initial reduction stage of Cr (Ⅲ) in deep eutectic solvent, the coordination compounds of [Cr(H2O)3Cl3] and [Cr(H2O)2Cl4 ]- would be preferentially formed, and the [Cr(H2O)2Cl4]- was the main coordination compound. With the increase of the concentration of CrCl3·6H2O, the form of coordination compound had a tendency to partially convert from [Cr(H2O)2Cl4]- to [Cr(H2O)3Cl3], and through an analysis taking into account both this tendency and the dissociation energy, it could be found that the transformation of the coordination compound made the reduction of Cr3+→Cr2+ easier. The reduction of trivalent chromium ions in ChCl - EG deep eutectic solvent was a two - step process: Cr3+→Cr2+→Cr. In the first step, the apparent activation energy was in the range of 12～16 kJ/mol and controlled by the diffusion step. In the second step, the apparent activation energy was in the range of 16～40 kJ/mol and controlled by both electrochemical and diffusion steps.

The aim of this study was to evaluate phagocytic and oxidative activities of monocytes and granulocytes during combined therapy of mice infected by drug-resistant Staphylococcus aureus SCAID OTT1-2022. The treatment of the infected mice was conducted by using an iodine-containing coordination compound CC-195, antibiotic cefazolin and by a combined therapy with CC-195 and cefazolin. The PHAGOTEST and BURSTTEST kits (BD Biosciences, USA) were used to determine the phagocytic and oxidative activities. The samples were analyzed on a FACSCalibur flow cytometer (BD Biosciences, United States). It was found that the different treatment regiments applied on the infected animals caused a statistically significant differentiation in numbers and activity of monocytes and granulocytes in comparison to the negative and positive control animals (intact and infected but untreated mice, respectively).

The reaction of magnesium turnings and 6,6‐di‐para‐tolylpentafulvene was investigated. Under mild conditions, the magnesium dissolves, forming the MgII complex 1 with a π‐η5 : σ‐κ1 coordinating ligand of the dimerized pentafulvene, analyzed by NMR and XRD investigations. As a magnesium pentafulvene complex was a possible intermediate, amines were employed as intercepting agents. Thereby, the amines were formally deprotonated by elemental magnesium, yielding the first examples of Cp'Mg(THF)2NR2 complexes. This reaction competes with the formation of 1 and a consecutive formal [1,5]‐H‐shift forming an ansa‐magnesocene. Employing amines with low basicity gave quantitative conversion to the amide complexes. [ABSTRACT FROM AUTHOR]

A study was carried out on the effect of a heavy chlorine atom introduced into the aromatic fragment of a 1,3-diketone ligand in Eu3+ coordination compounds on the spectral and luminescent properties of complex compounds. The data obtained from the absorption, optical excitation, fluorescence, and phosphorescence spectra as well as from the kinetics of the luminescence intensity permit estimation of the efficiency of energy transfer processes within the compounds studied. Introduction of a heavy chlorine atom was found to raise the energy of the first excited singlet state from 24,500 to 26,000 cm–1 but not affect the energy of the triplet level of the ligand. Furthermore, introduction of a chlorine atom leads to a decrease in the nonradiative relaxation constant (from 1290 to 840 s–1) and thereby triples the luminescence quantum yield from 23 to 64%. Hence, a new approach for the rational construction of useful coordination compounds of Eu3+ ions with 1,3-diketone ligands has been developed consisting of the substitution of a hydrogen atom by a heavy chlorine atom in the aromatic fragment of the ligand. [ABSTRACT FROM AUTHOR]

A new molecular binuclear vanadium(V) complex [VO(L)(OCH3)]2 (I) is synthesized in which ligand H2L is prepared by the reaction of isonicotinic acid hydrazide (INAH, isoniazide) with 1-phenyl-1,3-butanedione. Ligand H2L and complex I are studied by elemental analysis, IR spectroscopy, mass spectrometry, and X-ray diffraction (XRD) (CIF files CCDC nos. 2172124 and 2172125, respectively). The composition and structure of the ligand in the free state is additionally studied by NMR spectroscopy. The bideprotonated organic ligand L2– coordinates to the metal atom via the tridentate mode through a set of donor atoms ONO to form two conjugated metallocycles. Different tautomeric forms are stabilized in H2L and in the corresponding coordinated ligand. [ABSTRACT FROM AUTHOR]

Two coordination compounds of Cu(II), namely, [Cu (phen)2Cl](NO3)·H2O (compound 1) and [Cu2(µ-Cl2)Cl2(Hdmpz)4] (compound 2), where phen = 1,10-phenanthroline and Hdmpz = 3,5-dimethylpyrazole, were synthesized at room temperature and characterized using elemental analysis, TGA, spectroscopic techniques (FT-IR and electronic) and single-crystal X-ray diffraction studies. The cooperative anion–π/π–π/anion–π assemblies involving the coordinated phen, along with the uncoordinated nitrate moieties, played pivotal roles in the stabilization of the crystal structure of compound 1. Unconventional type I Cl⋯Cl interactions involving the coordinated Cl atoms provided reinforcement to the crystal structure of compound 2. We theoretically explored the supramolecular assemblies observed in the crystal structures of compounds 1 and 2 using DFT calculations, MEP surface analysis and combined NCI plot/QTAIM computational tools. Theoretical analysis revealed that the antiparallel π-stacking interactions in compound 1 and the N–H···Cl H-bonds in compound 2 were the strong structure-guiding non-covalent synthons which stabilized the compounds. In the anion–π/π–π/anion–π assembly observed in compound 1, the anion–π interaction reinforced the π-stacking by reducing the electrostatic repulsion between the metal-coordinated electron-deficient phen rings. [ABSTRACT FROM AUTHOR]

Enhancing carrier separation and transport efficiency to achieve efficient water oxidation reaction is an important issue in photoelectrochemical (PEC) water splitting field, and introducing hole transfer layer (HTL) is an effective strategy to improve it. However, the difficulty of charge transfer between HTL and oxygen evolution catalyst (OEC) is a problem unresolved. To ameliorate the situation, we choose CoOOH as HTL and the metal–organic coordination compound constructed by 4,5-Imidazoledicarboxylic acid (IA) and Co/Ni ions as OEC. Using the interfacial coordination bonds as carrier transfer channels, the holes were rapidly extracted from HTL to OEC containing abundant active sites and participate in oxidation reaction. In consequence, the unique design results in a photocurrent density of 2.97 times that of α-Fe 2 O 3 at 1.23 V RHE for the IACN/CoOOH/Fe 2 O 3. This study reveals how the advisable design of photoanode promotes interfacial charge transfer and provides a valuable reference for the design of composite photoanode. [Display omitted] • A highly efficient PEC composite photoanode IACN/CoOOH/Fe 2 O 3 was fabricated by simple methods. • CoOOH was introduced as hole transfer layer to improve charge separation and extraction efficiency. • The holes transfer channels constructed by the interfacial coordination bonds improve the hole transport from HTL to IACN. • The active sites and hydrophilicity of IACN can promote the adsorption and catalysis of active species in the electrolyte. [ABSTRACT FROM AUTHOR]

An europium(III) coordination binuclear compound [Eu 2 (o -MBA) 6 (phen) 2 ] (o -MBA = ortho -methylbenzoate, phen = 1,10-phenantroline) has been synthesized and investigated by X-ray diffraction method, thermogravimetric analysis (TGA), infrared (IR) and photoluminescence (PL) spectroscopy. The single crystal X-Ray diffraction measurements show that the compound crystallizes in the triclinic centrosymmetric space group P -1. The PL excitation spectrum displays a broad band between 300 and 420 nm and a number of sharp transitions between 384 and 590 nm, which can be attributed to the Eu3+ 4 f 6 intra-shell excitation transitions. The complex exhibits characteristic narrow, metal-centred emission bands, which are determined by the radiative transitions of the Eu3+ ion, from the first excited non-degenerate 5 D 0 level to the 7 F J (J = 0–4) manifold. The compound shows intense hypersensitive transition 5 D 0 →7 F 2 which dominates the PL emission spectrum. The dipole strengths of the transitions were determined from the emission spectra in terms of Judd-Ofelt (JO) intensity parameters Ω λ (λ = 2, 4). The high intensity bright-red emission of the complex can be attributed to highly polarizable ligands environment and the low site symmetry (Ci) around the lanthanide ions. We suppose that the J -mixing effect in the Eu(III) ions is responsible for enhanced peak maximum of the 5 D 0 →7 F 0 transition. [Display omitted] • A binuclear complex [Eu 2 (o-MBA) 6 (phen) 2 ] has been prepared and characterized by XRD, TGA, IR and PL spectroscopy. • A grown crystals comprise two centrosymmetric similar types binuclear molecules with Ci molecular symmetry. • The Eu 2 (o -MBA) 6 (phen) 2 compound shows a pure bright-red luminescence with the intrinsic quantum yield about 75 %. • The radiative parameters of the complex indicate on a significant potential for applications in photonics. [ABSTRACT FROM AUTHOR]

Bis(η5:η1‐(di‐para‐tolyl)pentafulvene)niobium chloride (1) reacts with methyl lithium via salt metathesis to the methylated bis(pentafulvene)niobium complex 2, and with lithium 2,6‐diisopropylanilide addition and subsequent N−H bond activation to the imido mono(pentafulvene)niobium complex 3. Avoiding the competing protonation of the chloride, bis(pentafulvene)niobium complex 2 reacts with primary aromatic and aliphatic amines to form terminal niobocene imido complexes, and with water to form the analog terminal oxo complex. Secondary methyl amines undergo a simultaneous N−H and C−H activation to form niobaaziridines under mild conditions. In contrast to other reported examples, 3 can be employed to investigate the uncontested reactivity of mono(pentafulvene)niobium complexes. Reaction with 4‐tert‐butylphenol selectively yields a niobocene phenolate complex. Unprecedented for mono(pentafulvene)niobium complexes, treating 3 with multiple‐bond‐containing substrates (nitriles, isocyanates) smoothly results the insertion into the Nb‐Cexo σ‐bond, forming the corresponding alkylidene amido and imidato complexes. [ABSTRACT FROM AUTHOR]

A novel lead coordination compound based on an extend viologen derivated ligand, [Pb4(TTVTC)Cl6(H2O)2] was successfully assembled under solvothermal condition and characterized. Single crystal structure study reveals that compound 1 is a 2D layer. Adjacent Pb2+ ions are doubly bridged by isophthalates and µ2-Cl ions to form an infinite one dimensional (1D) ladder-like chain. The chains are further interlinked by the TTV moieties to generate a 2D layer. And hydrogen bond interaction based on C–H···Cl and C–H···O forms the supramolecular 3D structure. Additionally, Solid- state fluorescence shows that 1 emits pale green fluorescence, which can be assigned to the inter-ligand π*–π and/or π*–n transitions. [ABSTRACT FROM AUTHOR]