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The efficacy of available treatments for melanoma is limited by side effects and the rapidly emerging resistance to treatment. In this context, the decavanadate compounds represent promising tools to design efficient therapeutic agents. In our study, we synthesized a dimagnesium disodium decavanadate icosahydrate compound (Mg 2 Na 2 V 10 O 28 ·20H 2 O) and investigated its structure stability as well as its antimelanoma effects. Results showed that the Mg 2 Na 2 V 10 O 28 ·20H 2 O compound is structured in a monoclinic system with the space group C2/c, stabilized by oxygen vertices, hydrogen bonds, and van der Waals interactions. Interestingly, we found that this newly synthesized compound reduced the viability of human (IGR39, IGR37, and SKMEL28) and murine (B16-F10) melanoma cells in a dose-dependent manner. The IC 50 values ranged from 7.3 to 18 μM after 24 h and decreased to 1.4 μM after 72 h of treatment. Notably, this effect was more important than that of cisplatin (IC 50  = 3 μM after 72 h of treatment), a chemotherapeutic agent, commonly used in the treatment of malignant melanoma. Furthermore, the cytotoxicity of the decavanadate compound was relatively weak on normal human keratinocytes (HaCaT), with a light effect (IC 50 >> 70 μM) observed after 24 h of treatment. Thus, the Mg 2 Na 2 V 10 O 28 ·20H 2 O compound displayed an advantage over cisplatin, which was reported to be much more aggressive to the keratinocyte cell line (IC 50  = 23.9 μM). Moreover, it inhibited dose-dependently the adhesion of IGR39 cells to collagen (IC 50  = 2.67 μM) and fibronectin, as well as their migration with an IC 50 value of 2.23 μM. More interestingly, its in vivo administration to B16-F10 allografted mice, at the nontoxic dose of 50 μg (2.5 mg/kg), prevented and suppressed by 70% the tumor growth, compared to the nontreated mice. Moreover, this compound has also allowed a recovery against inflammation induced in mice by a mixture of DMBA and croton oil. Thus, all our results showed the potential of the Mg 2 Na 2 V 10 O 28 ·20H 2 O compound to prevent and efficiently treat the growth and metastasis of melanoma., Competing Interests: The authors declare no conflicts of interest., (Copyright © 2025 Amine Essid et al. Bioinorganic Chemistry and Applications published by John Wiley & Sons Ltd.)

Melanoma is a skin cancer that arises from melanocytes and can spread quickly to the other organs of the body, if not treated early. Generally, melanoma shows an inherent resistance to conventional therapies. In this regard, new potential drugs are being developed as possible treatments for melanoma. In this paper, we report the synthesis of a new decavanadate compound with organic molecules for a potential therapeutic application. The tetra-[methylimidazolium] dihydrogen decavanadate(V) salt (C 4 H 7 N 2 ) 4 [H 2 V 10 O 28 ] is characterized by single-crystal X-ray diffraction, by FT-IR, UV-Vis and 51 V NMR spectroscopy, as well as by thermal analysis (TGA and DSC). The compound crystallizes in the monoclinic centrosymmetric space group P2 1 /c. Its formula unit consists of one dihydrogen decavanadate anion [H 2 V 10 O 28 ] 4- and four organic 4-methylimidazolium cations (C 4 H 7 N 2 ) + . Important intermolecular interactions are N-H···O and O-H···O hydrogen bonds and π-π stacking interactions between the organic cations, revealed by analysis of the Hirshfeld surface and its two-dimensional fingerprint plots. Interestingly, this compound inhibits the viability of IGR39 cells with IC 50 values of 14.65 μM and 4 μM after 24 h and 72 h of treatment, respectively. The analysis of its effect by flow cytometry using an Annexin V-FITC/IP cell labeling, showed that (C 4 H 7 N 2 ) 4 H 2 V 10 O 28 compound induced IGR39 cell apoptosis and necrosis. Molecular docking studies performed against TNFR1 and GPR40, as putative targets, suggest that the (C 4 H 7 N 2 ) 4 [H 2 V 10 O 28 ] compound may act as inhibitor of these proteins, known to be overexpressed in melanoma cells. Therefore, we could consider it as a new potential metallodrug against melanoma., Competing Interests: Declaration of competing interest The authors declare no conflicts of interest., (Copyright © 2024. Published by Elsevier Inc.)

Two bases-decavanadates coordination compounds [(C 6 H 13 N 4 ) 2 ][Mg(H 2 O) 6 ] 2 [O 28 V 10 ].6H 2 O (1) and [(C 7 H 11 N 2 ) 4 ][Mg(H 2 O) 6 ][O 28 V 10 ].4H 2 O (2) have been synthesized and well characterized using vibrational spectroscopy (infrared), UV-Visible analysis and single crystal X-ray diffraction technique. The formula unit, for both compounds, is composed by the decavanadate [V 10 O 28 ] 6- , hydrated magnesium ion, a counter anion and free water molecules. The transition metal adopts octahedral geometries in both compound (1) and (2). The existence of a multitude of hydrogen bonding interactions for both compounds provides a stable three-dimensional supramolecular structure. Optical absorption reveals a band gap energy indicating the semi-conductive nature of the compound. In this study, the cytotoxic and the anti-proliferative activities of compounds (1) and (2) on human cancer cells (U87 and MDA-MB-231) were investigated. Both compounds demonstrated dose-dependent anti-proliferative activity on U87 and MDA-MB-231 with respective IC 50 values of 0.82 and 0.31 μM and 1.4 and 1.75 μM. These data provide evidence on the potential anticancer activity of [(C 6 H 13 N 4 ) 2 ][Mg(H 2 O) 6 ] 2 [O 28 V 10 ].6H 2 O and [(C 7 H 11 N 2 ) 4 ][Mg(H 2 O) 2 ][O 28 V 10 ].4H 2 O. Molecular docking of the compounds was also examined. Molecular docking studies were performed for both compounds against four target receptors and revealed better binding affinity with these targets in comparison to Cisplatin. Moreover, molecular docking investigations suggest that these compounds may function as potential inhibitors of proteins in brain and breast cells, exhibiting greater efficiency compared to Cisplatin., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Inc. All rights reserved.)

Cis -2-iminothiazolidines and cis -thiazolidine-2-iminium tetrafluoroborates were successfully produced from trans - N -alkyl aziridine-2-carboxylates and phenyl/alkyl isothiocyanates mediated by zinc tetrafluoroborate in refluxing DCE. Reactions were performed via a complete regio- and stereoselective process to give the title iminothiazolidines and cis -thiazolidine-2-iminium salts in moderate to good yields (35 to 82%) with a wide substrate scope. In addition, the antibacterial activity evaluation of these compounds, as well as the minimum inhibitory concentration (MIC) determination, revealed that only four cis -thiazolidine-2-iminium salts showed growth inhibition against Bacillus cereus ., Competing Interests: The authors declare no competing financial interest., (© 2023 The Authors. Published by American Chemical Society.)

Two isomeric 2-bromomethylpyridine Cu(II) complexes [Cu(C 6 H 9 NBr) 2 (NO 3 ) 2 ] with 2-bromo-5-methylpyridine (L 1 ) and 2-bromo-4-methylpyridine (L 2 ) were synthesized as air-stable blue materials in good yields. The crystal structures were different with [Cu(L 1 ) 2 (NO 3 ) 2 ] ( CuL 1 ) crystallizing in the monoclinic space group P 2 1 /c, while the 4-methyl derivative CuL 2 was solved and refined in triclinic P 1¯. The orientation of the Br substituents in the molecular structure ( anti ( CuL 1 ) vs. syn ( CuL 2 ) conformations) and the geometry around Cu(II) in an overall 4 + 2 distorted coordination was very different with two secondary (axially elongated) Cu-O bonds on each side of the CuN 2 O 2 basal plane in CuL 1 or both on one side in CuL 2 . The two Br substituents in CuL 2 come quite close to the Cu(II) centers and to each other (Br⋯Br ~3.7 Å). Regardless of these differences, the thermal behavior (TG/DTA) of both materials is very similar with decomposition starting at around 160 °C and CuO as the final product. In contrast to this, FT-IR and Raman frequencies are markedly different for the two isomers and the UV-vis absorption spectra in solution show marked differences in the π-π* absorptions at 263 ( CuL 2 ) or 270 ( CuL 1 ) nm and in the ligand-to-metal charge transfer bands at around 320 nm which are pronounced for CuL 1 with the higher symmetry at the Cu(II) center, but very weak for CuL 2 . The T -dependent susceptibility measurements also show very similar results ( µ eff = 1.98 µ B for CuL 1 and 2.00 µ B for CuL 2 and very small Curie-Weiss constants of about -1. The EPR spectra of both complexes show axial symmetry, very similar averaged g values of 2.123 and 2.125, respectively, and no hyper-fine splitting.

The present paper described the first green synthesis of silver nanoparticles (AgNPs) from the extremophile plant Aeonium haworthii . The characterization of the biosynthesized silver nanoparticles was carried out by using UV-Vis, FTIR and STM analysis. The antioxidant, antidiabetic and antimicrobial properties were also reported. The newly described AgNPs were spherical in shape and had a size of 35-55 nm. The lowest IC50 values measured by the DPPH assay indicate the superior antioxidant behavior of our AgNPs as opposed to ascorbic acid. The silver nanoparticles show high antidiabetic activity determined by the inhibitory effect of α amylase as compared to the standard Acarbose. Moreover, the AgNPs inhibit bacterial growth owing to a bactericidal effect with the MIC values varying from 0.017 to 1.7 µg/mL. The antifungal action was evaluated against Candida albicans , Candida tropicalis , Candida glabrata , Candida sake and non-dermatophytic onychomycosis fungi. A strong inhibitory effect on Candida factors' virulence was observed as proteinase and phospholipase limitations. In addition, the microscopic observations show that the silver nanoparticles cause the eradication of blastospores and block filamentous morphogenesis. The combination of the antioxidant, antimicrobial and antidiabetic behaviors of the new biosynthesized silver nanoparticles highlights their promising use as natural phytomedicine agents.

Candida and dermatophyte infections are difficult to treat due to increasing antifungal drugs resistance such as fluconazole, as well as the emergence of multi-resistance in clinical bacteria. Here, we first synthesized silver nanoparticles using aqueous fruit extracts from Scabiosa atropurpurea subsp. maritima (L.). The characterization of the AgNPs by means of UV, XRD, FTIR, and TEM showed that the AgNPs had a uniform spherical shape with average sizes of 40-50 nm. The biosynthesized AgNPs showed high antioxidant activity when investigated using 1,1-diphenyl-2-picryl-hydrazyl (DPPH) and ferric reducing antioxidant power (FRAP) assays. The AgNPs displayed strong antibacterial potential expressed by the maximum zone inhibition and the lowest MIC and MBC values. The AgNPs revealed a significant antifungal effect against the growth and biofilm of Candida species. In fact, the AgNPs were efficient against Trichophyton rubrum, Trichophyton interdigitale, and Microsporum canis . The antifungal mechanisms of action of the AgNPs seem to be due to the disruption of membrane integrity and a reduction in virulence factors (biofilm and hyphae formation and a reduction in germination). Finally, the silver nanoparticles also showed important cytotoxic activity against the human multiple myeloma U266 cell line and the human breast cancer cell line MDA-MB-231. Therefore, we describe new silver nanoparticles with promising biomedical application in the development of novel antimicrobial and anticancer agents.

In this study, a successfully rapid, simple approach was applied for biosynthesis of silver nanoparticles AgNPs using for the first time the mixed leaves extract of Olea europaea subsp. europaea var. sylvestris and Pistacia lentiscus from natural association aimed to enhance their antimicrobial potential. The plant extract acts both as reducing and capping agents. When the aqueous extract was added to AgNO 3 solution, the color was changed from pale to yellow to brown indicating the reduction of Ag ions and synthesis of silver nanoparticles (AgNPs) without any solvent or hazardous reagents. The green synthesized AgNPs were characterized by UV-Vis spectrophotometer, FTIR spectrum and the X-ray crystallography. The AgNPs showed superior antioxidant activity measured by DPPH, Ferric Antioxidant Reducing Power (FRAP) as well as the total antioxidant activity methods. Moreover, the analysis of phytochemical constituents including flavonoids, tannins, alkaloids and total polyphenols contents mentioned the most richness of the silver nanoparticles compared to plant extract. The new synthesized AgNPs demonstrated the bactericidal and fungicidal effects against all the tested bacterial and fungal strains and found to limit the spore germination of filamentous fungi. AgNPs also gave an anti-biofilm activity and synergistic effect with the conventional antibiotic's drugs. Here we firstly describe the silver nanoparticles effect on virulence factors of Candida species by reduction of enzymes like proteinase and phospholipase, inhibition of morphogenesis of Candida albicans cells. This natural product, acquiring these properties, should be promoted to be used in pharmaceutical and medical industries in future., (© 2022. The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature.)

The title mol-ecular salt, (C 7 H 11 N 2 ) 2 [Hg 2 Cl 6 ], crystallizes with two 4-(di-methyl-amino)-pyridinium cations ( A and B ) and two half hexa-chlorido-dimercurate(II) anions in the asymmetric unit. The organic cations exhibit essentially the same features with an almost planar pyridyl ring (r.m.s. deviations of 0.0028 and 0.0109 Å), which forms an inclined dihedral angle with the dimethyamino group [3.06 (1) and 1.61 (1)°, respectively]. The di-methyl-amino groups in the two cations are planar, and the C-N bond lengths are shorter than that in 4-(di-methyl-amino)-pyridine. In the crystal, mixed cation-anion layers lying parallel to the (010) plane are formed through N-H⋯Cl hydrogen bonds and adjacent layers are linked by C-H⋯Cl hydrogen bonds, forming a three-dimensional network. The analyses of the calculated Hirshfeld surfaces confirm the relevance of the above inter-molecular inter-actions, but also serve to further differentiate the weaker inter-molecular inter-actions formed by the organic cations and inorganic anions, such as π-π and Cl⋯Cl inter-actions. The powder XRD data confirms the phase purity of the crystalline sample. Furthermore, the vibrational absorption bands were identified by IR spectroscopy and the optical properties were studied by using optical UV-visible absorption spectroscopy., (© Garci et al. 2019.)

Mercerized cellulose (alkali cellulose C 6 H 10 O 5 * NaOH) was obtained by treatment of cotton linters (cellulose) with aqueous sodium hydroxide. Cellulose and alkali-cellulose samples with relative density of 78% and 79% were obtained after sintering the material in air at optimal sintering temperatures of 423 K and 473 K, respectively. The electrical properties of the samples were studied by impedance spectroscopy in the frequency range from 13 MHz to 50 Hz at temperatures between 393 K and 493 K. The influence of cellulose mercerization on electrical properties of cotton linters was observed. The cellulose behaves like an electrical insulator. Contrariwise, the alkali-cellulose is a fast-ionic conductor with a conductivity value of σ 473 K = 3.22 × 10 -6 S cm -1 having activation energies of 0.49 eV and 0.68 eV at temperature range of 393 K-458 K and 459 K-500 K, respectively. The change of activation energy value has been discussed in relation to thermal stability., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Crystals of the title compound, (C 5 H 8 N 3 ) 3 [VO 2 (C 2 O 4 ) 2 ]·2.5H 2 O, a mononuclear V V complex, were obtained by slow evaporation at room temperature of an aqueous solution containing vanadium pentoxide, oxalic acid and 2,6-di-amino-pyridine. The asymmetric unit contains one bis-(oxalato)dioxovanadate(V) anionic complex, three 2,6-di-amino-pyridinium cations and two and a half uncoordinated water mol-ecules. The mononuclear vanadium(V) anions are connected to the organic cations and water mol-ecules through a strong N-H⋯O and O-H⋯O hydrogen-bond network, consolidated by π-π stacking inter-actions, to form a three-dimensional structure.

The title salt, C 8 H 20 N 2 2+ ·2NO 3 - , was obtained by a reaction between 1,3-cyclohexa-nebis(methyl-amine) and nitric acid. The cyclo-hexane ring of the organic cation is in a chair conformation with the methyl-ammonium substituents in the equatorial positions and the two terminal ammonium groups in a trans conformation. In the crystal, mixed cation-anion layers lying parallel to the (010) plane are formed through N-H⋯O hydrogen-bonding inter-actions; these layers are formed by infinite undulating chains running parallel to the [001] direction. The overall inter-molecular inter-actions involved in the structure were qu-anti-fied and fully described by Hirshfeld surface analysis. In addition, energy-framework calculations were used to analyse and visualize the three-dimensional topology of the crystal packing. The electrostatic energy framework is dominant over the dispersion energy framework.

In the title mol-ecular salt, (C 5 H 8 N 3 ) 2 [CoCl 4 ], the cations are protonated at their pyridine N atoms and the anion is an almost regular tetra-hedron. The crystal structure consists of alternating inorganic layers, built from tetra-chlorido-cobaltate anions, and organic layers formed by protonated cations of 2,6-di-amino-pyridinium. The crystal packing is governed by C/N-H⋯Cl hydrogen-bonding inter-actions between the organic and the inorganic ions and Cl⋯Cl inter-actions. Moreover, the cations show a π-π stacking inter-action [inter-centroid distance = 3.763 (2) Å]. The prevalence of these inter-actions is illustrated by an analysis of the three-dimensional Hirshfeld surface and by two-dimensional fingerprint plots.

The title compound, sodium chromium/aluminium molybdenum/aluminium dodeca-oxide, Na 0.72 Cr 0.48 Al 1.74 Mo 2.77 O 12 , was prepared by solid-state reaction. Its crystal structure is related to NaSICON-type compounds. The framework is built up from M 1O 6 ( M 1 = Cr/Al) octa-hedra and M 2O 4 ( M 2 = Mo/Al) tetra-hedra inter-connected by corners. The three-dimensional framework contains cavities in which sodium cations are located. Two validation models (BVS and CHARDI) were used to confirm the proposed structural model. The mobility of Na + ions in the structure has been investigated by theoretical means.

The synthesis of p -toluidinium perchlorate (systematic name: 4-methyl-anilinium perchlorate), C 7 H 10 N + ·ClO 4 - , was carried out from an aqueous reaction of perchloric acid with p -toluidine. This compound was characterized by powder XRD, IR and UV-Vis spectroscopy. The structure was further confirmed by a single-crystal X-ray diffraction study. The crystal structure is formed by a succession of two-dimensional mol-ecular layers consisting of perchlorate anions and organic cations parallel to the (100) plane and located at x = 2 n  + ½ ( n ∈ Z ). Each mixed layer is formed by infinite chains {C 7 H 10 N + ·ClO 4 - } n parallel to the [010] direction and developing along the c axis, generating R 2 4 (8), R 2 2 (4) and R 4 4 (12) graph-set motifs. The results of a theoretical study using the DFT method at the B3LYP/6-311++G(d,p) level are in good agreement with the experimental data. Hirshfeld surface and fingerprint plots reveal that the structure is dominated by O⋯H/H⋯O (54.2%), H⋯H (26.9%) and C-H ⋯π (14.3%) contacts. The studied crystal was refined as a two-component twin.

Since the discovery of electrochemically active LiFePO 4 , materials with tunnel and layered structures built up of transition metals and polyanions have become the subject of much research. A new quaternary arsenate, sodium calcium trinickel aluminium triarsenate, NaCa 1-x Ni 3-2x Al 2x (AsO 4 ) 3 (x = 0.23), was synthesized using the flux method in air at 1023 K and its crystal structure was determined from single-crystal X-ray diffraction (XRD) data. This material was also characterized by qualitative energy-dispersive X-ray spectroscopy (EDS) analysis and IR spectroscopy. The crystal structure belongs to the α-CrPO 4 type with the space group Imma. The structure is described as a three-dimensional framework built up of corner-edge-sharing NiO 6 , (Ni,Al)O 6 and AsO 4 polyhedra, with channels running along the [100] and [010] directions, in which the sodium and calcium cations are located. The proposed structural model has been validated by bond-valence-sum (BVS) and charge-distribution (CHARDI) tools. The sodium ionic conduction pathways in the anionic framework were investigated by means of the bond-valence site energy (BVSE) model, which predicted that the studied material will probably be a very poor Na + ion conductor (bond-valence activation energy ∼7 eV).

The synthesis of 4-aza-niumyl-2,2,6,6-tetra-methyl-piperidin-1-ium diperchlorate, C 9 H 22 N 2 2+ ·2ClO 4 - , was carried out from an aqueous reaction of perchloric acid with 4-amino-2,2,6,6-tetra-methyl-piperidine. This compound was characterized by TGA-DSC analysis and single-crystal X-ray diffraction. The piperidine ring of the dication adopts a chair conformation and the orientation of the C-NH 3 bond is equatorial. One of the two crystallographically independent perchlorate anions exhibits disorder [occupancies 0.625 (7) and 0.375 (7)]. The crystal packing is constituted by a succession of mixed layers parallel to the (-102) plane, made up of C 9 H 22 N 2 2+ dications and ClO 4 - anions. These ions are linked by normal and bifurcated N-H⋯O hydrogen bonds with R 4 4 (12) graph-set motifs, generating a two-dimensional network. The inter-molecular inter-actions in the crystal structure were qu-anti-fied and analysed using Hirshfeld surface analysis.

A new arsenate K 1+2 x Ni 1- x Fe 2 (AsO 4 ) 3 ( x = 1/8) {potassium nickel diiron(III) tris-[arsenate(V)]} was synthesized using a flux method and its crystal structure was determined from single-crystal X-ray diffraction data. This material was also characterized by qualitative energy dispersive X-ray spectroscopy (EDS) analysis. The crystal structure belongs to the α-CrPO 4 -structure type, space group Imma . It consists of a three-dimensional-framework built up from FeO 6 and Ni 0.875 □ 1.25 O 6 -octa-hedra and AsO 4 -tetra-hedra that are sharing corners and/or edges, generating tunnels running along the [010] and [001] directions in which the potassium cations are located. The proposed structural model was validated by bond-valence-sum calculations, charge-distribution (CHARDI) and Madelung energy analyses.

Single crystals of a new variety of tetra-sodium copper(II) tris-[molybdate(VI)], Na4Cu(MoO4)3, have been synthesized by solid-state reactions and characterized by single-crystal X-ray diffraction. This alluaudite structure-type is characterized by the presence of infinite layers of composition (Cu/Na)2Mo3O14 parallel to the (100) plane, which are linked by MoO4 tetra-hedra, forming a three-dimensional framework containing two types of hexa-gonal channels in which Na(+) cations reside. The Cu(2+) and Na(2+) cations are located at the same general site with occupancies of 0.5. All atoms are on general positions except for one Mo, two Na (site symmetry 2) and another Na (site symmetry -1) atom. One O atom is split into two separate positions with occupancies of 0.5. The title compound is isotypic with Na5Sc(MoO4)4 and Na3In2As3O12. The structure model is supported by bond-valence-sum (BVS) and charge-distribution CHARDI methods. β-Na4Cu(MoO4)3 is compared and discussed with the K4Cu(MoO4)3 and α-Na4Cu(MoO4)3 structures.

The title organic-inorganic hybrid salt, (C7H11N2)2[V(C2O4)2O(H2O)]·2H2O, shows a distorted octa-hedral coordination environment for the vanadium(IV) atom in the anion (point group symmetry 2), with four O atoms from two symmetry-related chelating oxalate dianions and two O atoms in trans configuration from a coordinating water mol-ecule and a terminal vanadyl O atom. In the crystal, (001) layers of cations and anions alternate along [001]. The anionic layers are built up by inter-molecular O-H⋯O hydrogen bonds involving the coordinating and solvent water mol-ecules. The cationic layers are linked to the anionic layers via N-H⋯O hydrogen bonds between the pyridinium group and the non-coordinating O atoms of the oxalate group. The 4-(di-methyl-amino)-pyridinium cations are also engaged in π-π stacking with their anti-parallel neighbours [centroid-to-centroid distance = 3.686 (2) Å]. Considering all supra-molecular features, a three-dimensional network structure is accomplished.

The title compound, nonasodium chromium(III) hexakis[molybdate(VI)], β-Na9CrMo6O24, was prepared by solid-state reactions. This alluaudite-type structure is constituted of infinite layers formed by links between M 2O10 (M = C/Na) dimers and MoO4 tetra-hedra. The Na(+) and Cr(3+) cations are located in the same site with, respectively, 0.25 and 0.75 occupancies. The layers are connected to each other through MoO4 sharing corners, resulting an in open three-dimensional framework with hexa-gonal-form cavities occupied by Na(+) cations. The proposed structural model is supported by charge-distribution (CHARDI) and bond-valence-sum (BVS) analysis. All atoms are on general positions except for one Mo, two Na (site symmetry 2) and another Na site (site symmetry -1). A comparison is made with the similar structures Na4Co(MoO4)3, Na2Ni(MoO4)2, Cu1.35Fe3(PO4)3 and NaAgFeMn2(PO4)3.

As part of our studies on the synthesis and the characterization of oxalate-bridged compounds M-ox-M (ox = oxalate dianion and M = transition metal ion), we report the crystal structure of a new oxalate-bridged Mn(II) phase, {(CH6N3)[Mn(C2O4)Cl(H2O)]·H2O} n . In the compound, a succession of Mn(II) ions (situated on inversion centers) adopting a distorted octa-hedral coordination and bridged by oxalate ligands forms parallel zigzag chains running along the c axis. These chains are inter-connected through O-H⋯O hydrogen-bonding inter-actions to form anionic layers parallel to (010). Individual layers are held together via strong hydrogen bonds involving the guanidinium cations (N-H⋯O and N-H⋯Cl) and the disordered non-coordinating water mol-ecule (O-H⋯O and O-H⋯Cl), as well as by guanidinium π-π stacking. The structural data were confirmed by IR and UV-Visible spectroscopic analysis.

The title compound, Ag0.60Na0.40Fe(MoO4)2 {silver sodium iron(III) bis-[molyb-date(VI)]}, was synthesized by a solid-state reaction. The structure is built up from FeO6 octa-hedra and MoO4 tetra-hedra sharing corners to form a two-dimensional framework parallel to the (001) plane. The occupationally disordered (Ag/Na)(+) cations are located in the inter-layer space. These [Fe(MoO4)2 (-)] n layers are similar to those in the isotypic yavapaiite-related structure of NaFe(MoO4)2. All atoms are on general positions except for Fe (site symmetry -1) and Ag/Na (site symmetry 2). The Ag/Na occupancies of the latter site were refined to 0.597 (4):0.403 (5). The title structure is compared to similar structures.

The new compound (Na0.4,Li0.6)(Fe,Li2)(MoO4)3 was synthesized by cooling from the melt. Its anionic framework is built up from two distinct MO6 octa-hedra, each containing disordered Li(+) and Fe(3+) ions in 0.6:0.4 and 0.7:0.3 ratios, and two MoO4 tetra-hedra, which link by vertex-sharing of their O atoms. These tetra-meric units are further linked by sharing edges between octa-hedra and by formation of M-O-Mo (M = Fe/Li) bridges, forming ribbons propagating in the [100] direction. The ribbons are cross-linked in both the b- and c-axis directions, giving rise to a three-dimensional framework having [100] tunnels in which the monovalent Na(+)/Li(+) cations (0.4:0.6 ratio) lie. Bond-valence calculations are consistent with the disorder model for the cations. The structure of the title compound, which is isotypic with Li3Fe(MoO4)3 and Li3Ga(MoO4)3, is compared briefly with those of LiFeMo2O8 and Li1.6Mn2.2(MoO4)3.

The title compound, nona-sodium chromium(III) hexa-kis[molybdate(VI)], Na9Cr(MoO4)6 was prepared by solid-state reactions. The basic structure units are isolated polyhedral clusters composed of a central CrO6 octa-hedron sharing vertices with six MoO4 tetrahedra to form an open framework in which the Na(+) cations are bound to the free vertices of the MoO4 tetra-hedra. The Cr(3+) cation has site symmetry of 32 (6a), one Na atom sits on a twofold axis (18e), and all other atoms are at general positions. The bond-valance-sum model confirms the expected values of ion charges. The title compound is isotypic with Na9Sc(MoO4)6 and Na9Fe(MoO4)6. It is compared and discussed with similar structures.

Silver(I) aluminiun tricobalt(II) penta-kis-[tetra-oxidomolybdate(VI)], Ag0.90Al1.06Co2.94(MoO4)5, was synthesized using a solid-state reaction at 845 K. The structure can be described as a three-dimensional framework formed from dimeric M 2O10 (M = Co/Al) and trimeric M 3O14 units linked to MoO4 tetra-hedra by sharing corners, with the cavities occupied by disordered Ag(+) cations. It is shown that the Co and Al atoms occupy common positions with different occupancies. The Ag(+) cations are located at two different sites with occupancies of 0.486 (1) and 0.408 (1). The title coumpond is isotypic with NaMg3Al(MoO4)5 and NaFe4(MoO4)5. Differences and similarities with other related structures are discussed.

A new silver aluminium trimangan-ese penta-molybdate {silver(I) trimanganese(II) aluminium penta-kis-[tetra-oxidomolybdate(VI)]}, AgMn(II) 3(Mn(III) 0,26Al0,74)(MoO4)5, has been synthesized using solid-state methods. The structure is composed of M 2O10 dimers, M 3O14 (M = Mn, Al) trimers and MoO4 tetra-hedra sharing corners and forming three types of layers A, B and B'. The sequence of the constituting layers is A-BB'-A-BB', with B' obtained from B by inversion symmetry, forming a three-dimensional structure with large channels in which the positionally disordered and partially occupied Ag(+) ions reside. The Mn(III) and Al(III) atoms share the same site, M. AgMn(II) 3(Mn(III) 0,26Al0,74)(MoO4)5 is isotypic with the NaMg3 X(MoO4)5 (X = Al, In) family and with NaFe4(MoO4)5. A comparative structural description is provided between the structure of the title compound and those of related phases containing dimers, trimers and tetra-mers.

A new triple molybdate, potassium sodium cobalt tris-(molybdate), K0.4Na3.6Co(MoO4)3, was synthesized using solid-state reactions. The Co(2+) and one Na(+) cation are located at the same general site, each with occupancy 0.5. Another site (site symmetry 2) is occupied by Na(+) and K(+) cations, with occupancies of 0.597 (7) and 0.402 (6), respectively. The other two Na(+) cations and one of the two Mo atoms lie on special positions (site symmetries -1, 2 and 2, respectively). The structure is characterized by M 2O10 (M = Co/Na) dimers, which are linked by MoO4 tetra-hedra, forming infinite layers. The latter are connected firstly by insertion of one type of MoO4 tetra-hedra and secondly by sharing corners with the other type of MoO4 tetra-hedra. This results in an open three-dimensional framework with the cavities occupied by the Na(+) and K(+) cations. The structure is isotypic with Na3In2As3O12 and Na3In2P3O12. A comparison is made with structures such as K2Co2(MoO4)3 and β-NaFe2(MoO4)3 and their differences are discussed.

The new phase potassium penta-sodium trimanganese hexa-kis(molybdate), KNa5Mn3Mo6O24, has been synthesized using solid-state methods. The structure is composed of M 2O10 (M = Mn, Na) dimers and MoO4 tetra-hedra (point group symmetry 2) sharing corners and forming layers parallel to (100), which are linked via common corners of another type of MO4 tetra-hedra, forming a three-dimensional structure with two types of large channels along [001] in which two types of Na(+) cations (one with site symmetry 2, one with -1) and K(+) cations (site symmetry 2, half-occupation) are located. Mn(2+) and the third type of Na(+) cations are located at the same site M with occupancies of 0.75 and 0.25, respectively. A comparative structural description is provided between the structure of the title compound and those of the related phases Cu1.35Fe3(PO4)3 and NaAgFeMn2(PO4)3.

The title compound, tetra-sodium cobalt(II) tris-[molyb-date(IV)], was prepared by solid-state reactions. The structure is isotypic with Na3In2(AsO4)3 and Na3In2(PO4)3. The main structural feature is the presence of infinite chains of edge-sharing X 2O10 (X = Co/Na) dimers, which are linked by MoO4 tetra-hedra, forming a three-dimensional framework enclosing two types of hexa-gonal tunnels in which Na(+) cations reside. In this alluaudite structure, Co and Na atoms are located at the same general site with occupancies of 0.503 (5) and 0.497 (6), respectively. The other three Na and one of the two Mo atoms lie on special positions (site symmetries 2, -1, 2 and 2, respectively). The structure is compared with similar structures and other members of alluaudite family.

A new organic-inorganic hybrid SO4[C6H9N2O2S]2, has been synthesized and characterized by X-ray diffraction. This compound crystallizes in the orthorhombic system, spaces group Pbcn. In the title compound, the packing is stabilized by intermolecular N-H⋯O hydrogen bonds and π-π stacking interactions between the phenyl rings, linking the molecules into three-dimensional network. The in vitro antimicrobial activity of di (4-sulfamoyl-phenyl-ammonium) sulphate was determined by the broth dilution method against several strains selected to define their spectrum and potency. Here we show that the synthetic sulfanilamide exhibits promising antibacterial potency. High inhibition was also detected against Candida albicans. In this paper we firstly showed the antifungal activity of the sulfanilamide against two serious phytopathogenic fungi. Interestingly, the new compound was able to suppress mycelial growth as well as the spores germination of tested fungi, values of spore germination vary from 97.6% to 37.5%, respectively for Botrytis cinerea and Fusarium species. The minimal inhibitory concentrations (MIC) ranging from 8 to 100 μg ml(-1) and IC50 values varying from 5.81 to less than 100 μg ml(-1)), showed that the sulfanilamide sulphate had high activity against bacteria, yeast and fungi, compared to others published antifungal compounds., (Copyright © 2013 Elsevier GmbH. All rights reserved.)

The title compound, dirubidium dimanganese(II) tris-(tetra-oxo-molyb-date), Rb2Mn2(MoO4)3, was prepared by solid-state reactions. The structure can be described as being composed of MnO6 octa-hedra sharing corners with MoO4 tetra-hedra. The three-dimensional framework contains cavities in which the rubidium ions are located. The Rb(+) cations are within distorted nine- and 12-vertex polyhedra. The pairs of different Mn(2+) and Rb(+) cations are each located on threefold rotation axes.. Rb2Mn2(MoO4)3 is isotypic with compounds of the Cs2 M 2Mo3O12 (M = Ni, Fe) family. A comparative structural description is provided between the structure of the title compound and those of related phases. Differences with structures such as alluaudite are discussed.

The title compound, tripotassium iron(III) bis-(ortho-molyb-date) dimolybdate, was obtained by a solid-state reaction. The main structural building units are one FeO6 octa-hedron, two MoO4 tetra-hedra and one Mo2O7 dimolybdate group, all with point group symmetries m. These units are linked via corner-sharing to form ribbons parallel to [010]. The three K(+) cations are located between the ribbons on mirror planes and have coordination numbers of 10 and 12. Two O atoms of one of the MoO4 tetra-hedra of the dimolybdate group are disordered over two positions in a 0.524 (11):0.476 (11) ratio. The structure of the title compound is compared briefly with that of Rb3FeMo4O15.

In the crystal structure of the title salt, C9H22N2 (2+)·2NO3 (-), the piperidine ring of the dication adopts a chair conformation and the orientation of the C-NH3 bond is equatorial. The ions are linked by normal and bifurcated N-H⋯O hydrogen bonds in R 2 (2)(6), two R 4 (2)(8) and R 3 (4)(14) graf-set motifs, generating a three-dimensional network.

The title compound α-ammonium iron(III) bis-[hydro-gen arsenate(V)], α-NH4Fe(HAsO4)2 (or poly[ammonium bis-(μ-hydro-gen arsenato)ferrate(III)], {NH4[Fe(HAsO4)2]} n ), syn-the-sized hydro-thermally, is isostructural with NH4Fe(HPO4)2. Condensation of the hydro-gen arsenate groups with FeO6 coordination octa-hedra via common corners results in an overall three-dimensional framework containing inter-connected channels parallel to the a-, b- and c-axis directions. The NH4 (+) cations are located in three inter-secting tunnels, which is promising as an ion exchange. Hydrogen bonding of the types O-H⋯O and N-H⋯O consolidates the packing of the structure. The distortion of the coordination polyhedra is analyzed by means of the effective coordination number and distortion indices. Structural relationships with other compounds of general formula M (I) M (III)[HXO4)]2 (X = P, As) are discussed.

The title compound, nona-niobium vanadium penta-cosa-oxide, was prepared by a solid-state reaction at 1198 K. It is isotypic with Nb9AsO25, Nb9PO25 and Ta9VO25. The structure consists of NbO6 octa-hedra (one with 4/m.. and two with m.. symmetry) and VO4 tetra-hedra (-4.. symmetry) sharing corners and edges to form a three-dimensional framework. This framework can be considered as a junction between ribbons made up from NbO6 octa-hedra and chains of NbO6 octa-hedra and chains of VO4 tetra-hedra. The V site shows half-occupancy, hence one half of the VO4 tetra-hedra is unoccupied. The structural differences with α-Nb9VO25, VOSO4, SbOPO4 and NbOPO4 oxides are discussed.

The title compound, disodium dimanganese(II) tris-[ortho-molybdate(VI)], was prepared by solid-state reactions. The structure can be described as being composed of Mn2Mo2O14 double-chains that are inter-connected by corner-sharing with MoO4 tetra-hedra, leading to a three-dimensional framework with channels propagating in [100] and [001] in which the Na(+) counter-cations are located. One of these Na sites is located on an inversion centre, one is partially occupied [occupancy 0.341 (9)], and one is statistically occupied by Na and Mn in a ratio of 0.829 (5):0.171 (5). Na1.67Mn2.17(MoO4)3 is isotypic with structures of the Ag2 M 2(MoO4)3 (M = Zn, Mg, Co, Mn) family. A comparative structural description is provided between the structure of the title compound and those of related phases containing (MXO8) n chains (M = Mo, Mn and X = As) or M 2O10 (M = Mo, Mn, Nb, V) dimers.

The title compound, lithium/sodium iron(III) bis-[ortho-molyb-date(VI)], was obtained by a solid-state reaction. The main structure units are an FeO6 octa-hedron, a distorted MoO6 octa-hedron and an MoO4 tetra-hedron sharing corners. The crystal structure is composed of infinite double MoFeO11 chains along the b-axis direction linked by corner-sharing to MoO4 tetra-hedra so as to form Fe2Mo3O19 ribbons. The cohesion between ribbons via mixed Mo-O-Fe bridges leads to layers arranged parallel to the bc plane. Adjacent layers are linked by corners shared between MoO4 tetra-hedra of one layer and FeO6 octa-hedra of the other layer. The Na(+) and Li(+) ions partially occupy the same general position, with a site-occupancy ratio of 0.631 (9):0.369 (1). A comparison is made with AFe(MoO4)2 (A = Li, Na, K and Cs) structures.

The title compound, trisodium dicobalt(II) (arsenate/phosphate) (diarsenate/diphosphate), was prepared by a solid-state reaction. It is isostructural with Na3Co2AsO4As2O7. The framework shows the presence of CoX22O12 (X2 is statistically disordered with As0.95P0.05) units formed by sharing corners between Co1O6 octa-hedra and X22O7 groups. These units form layers perpendicular to [010]. Co2O6 octa-hedra and X1O4 (X1 = As0.54P0.46) tetra-hedra form Co2X1O8 chains parallel to [001]. Cohesion between layers and chains is ensured by the X22O7 groups, giving rise to a three-dimensional framework with broad tunnels, running along the a- and c-axis directions, in which the Na(+) ions reside. The two Co(2+) cations, the X1 site and three of the seven O atoms lie on special positions, with site symmetries 2 and m for the Co, m for the X1, and 2 and m (× 2) for the O sites. One of two Na atoms is disordered over three special positions [occupancy ratios 0.877 (10):0.110 (13):0.066 (9)] and the other is in a general position with full occupancy. A comparison between structures such as K2CdP2O7, α-NaTiP2O7 and K2MoO2P2O7 is made. The proposed structural model is supported by charge-distribution (CHARDI) analysis and bond-valence-sum (BVS) calculations. The distortion of the coordination polyhedra is analyzed by means of the effective coordination number.

In the title hydrated mol-ecular salt, (C3H5N2)[Cr(C2O4)2(H2O)2]·2H2O, the complete cation is generated by a crystallographic twofold rotation axis, with one C atom lying on the rotation axis. The complete anion is generated by crystallographic inversion symmetry (Cr(III) site symmetry -1), to generate a slightly distorted CrO6 octa-hedron with trans water mol-ecules and chelating oxalate dianions. The oxalate ion is almost planar (r.m.s. deviation = 0.017 Å) and the five-membered chelate ring is a shallow envelope with the metal ion displaced by 0.126 (1) Å from the ligand atoms. The crystal structure features O-H⋯O, N-H⋯O and C-H⋯O hydrogen bonds, which link the components into a three-dimensional network.

The title compound, tetrasodium lithium cobalt aluminium hexa-(orthoarsenate), was synthesized by a solid state reaction route. In the crystal structure, Co(2+) ions are partially substituted by Al(3+) in an octa-hedral environment [M1 with site symmetry 2/m; occupancy ratio Co:Al = 0.286 (10):0.714 (10)]. The charge compensation is ensured by Li(+) cations sharing a tetra-hedral site with Co(2+) ions [M2 with site symmetry 2; occupancy ratio Co:Li = 0.690 (5):0.310 (5)]. The anionic unit is formed by two octa-hedra and three tetra-hedra linked only by corners. The CoM1M2As2O19 units associate to an open three-dimensional framework containing tunnels propagating along the a-axis direction. One Na(+) cation is located in the periphery of the tunnels while the other two are situated in the centres: all Na(+) cations exhibit half-occupancy. The structure of the studied material is compared with those of various related minerals reported in the literature.

Brannerite-type Li[VMoO6] has been synthesized by a solid state reaction route. The V and Mo atoms statistically occupy the same site with mirror symmetry and are octa-hedrally surrounded by O atoms. The framework is two-dimensional and is built up from edge-sharing (V,Mo)O6 octa-hedra forming (VMoO6)∞ layers that run parallel to the (001) plane. Li(+) ions are situated in position with symmetry 2/m in the inter-layer space. The bond-valence analysis reveals that the Li(+) ionic conductivity is along the [010] and [110] directions, and shows that this material may have inter-esting conduction properties. This simulation proposes a model of the lithium conduction pathways.

The title compound, lithium/aluminium dimagnesium tetra-kis-[orthomolybdate(VI)], was prepared by a solid-state reaction route. The crystal structure is built up from MgO6 octa-hedra and MoO4 tetra-hedra sharing corners and edges, forming two types of chains running along [100]. These chains are linked into layers parallel to (010) and finally linked by MoO4 tetra-hedra into a three-dimensional framework structure with channels parallel to [001] in which lithium and aluminium cations equally occupy the same position within a distorted trigonal-bipyramidal coordination environment. The title structure is isotypic with LiMgIn(MoO4)3, with the In site becoming an Mg site and the fully occupied Li site a statistically occupied Li/Al site in the title structure.

In the title compound, (C6H9N2)[Cr(C2O4)2(H2O)2]·H2O, the Cr(III) atom adopts a slightly distorted octa-hedral coordination environment defined by two chelating oxalate ligands in the equatorial plane and two water mol-ecules in axial positions. A three-dimensional network is generated by inter-molecular N-H⋯O and O-H⋯O hydrogen-bonding interactions involving the cation, the complex anion and the lattice water molecule.

The title compound, potassium sodium dioxidomolybden-um(VI) arsenate, K0.78Na0.22MoO2AsO4, was synthesized by a solid-state reaction route. The structure is built up from corner-sharing MoO6 octa-hedra and AsO4 tetra-hedra, creating infinite [MoAsO8]∞ chains running along the b-axis direction. As, Mo and all but one O atom are on special positions (4c) with m symmetry and K (occupancy 0.78) is on a position (4a) of -1 in the tunnels. The possible motion of the alkali cations has been investigated by means of the bond-valance sum (BVS) model. The simulation shows that the Na(+) motion appears to be easier mainly along the b-axis direction. Structural relationships between the different compounds of the AMoO2AsO4 (A = Ag, Li, Na, K, Rb) series and MXO8 (M = V; X = P, As) chains are discussed.

A new compound with a non-centrosymmetric structure, potassium tetra-kis-[dioxomolybdenum(IV)] arsenate trioxide, K(MoO2)4O3(AsO4), has been synthesized by a solid-state reaction. The [(MoO2)4O3(AsO4)](+) three-dimensional framework consists of single arsenate AsO4 tetra-hedra, MoO6 octa-hedra, MoO5 bipyramids and bi-octa-hedral units of edge-sharing Mo2O10 octa-hedra. The [Mo2O8]∞ octa-hedral chains running along the a-axis direction are connected through their corners to the AsO4 tetra-hedra, MoO6 octa-hedra and MoO5 bipyramids, so as to form large tunnels propagating along the a axis in which the K(+) cations are located. This structure is compared with compounds containing M 2O10 (M = Mo, V, Fe) dimers and with those containing M 2O8 (M = V) chains.

The title compound, hepta-sodium tetra-chromium(III) tetra-kis-(diphosphate) orthophosphate, was synthesized by solid-state reaction. Its structure is isotypic with that of Na7 M 4(P2O7)4PO4 (M = In, Al) compounds and is made up from a three-dimensional [(CrP2O7)4PO4](7-) framework with channels running along [001]. The three Na(+) cations are located in the voids of the framework. One of the cations is situated on a general position, one is equally disordered around a twofold rotation axis and one is on a fourfold rotoinversion axis. The isolated PO4 tetra-hedron of the anionic framework is also situated on the -4 axis. Structural relationships between the title compound and different diphosphates containing MP2O11 units (M = Mo, V) are discussed.

The structure of the title compound tris-odium aluminium bis-(arsenate), Na(3)Al(AsO(4))(2), is built up from AlO(4) and AsO(4) corner-sharing tetra-hedra, forming an undulating two-dimensional framework parallel to (100). The layers are constituted of large Al(6)As(6)O(36) rings made up from six AlO(4) and AsO(4) tetra-hedra in which two sodium cations are situated, the third sodium cation being located in the inter-layer space. The structural relationships between the title compound and Na(3)Fe(PO(4))(2), NaAlCo(PO(4))(2) and Al(5)Co(3)(PO(4))(8) are discussed.

A new vanadium oxide, potassium bis-(dioxovanad-yl) phosphate, β-K(VO2)2(PO4), has been synthesized by a solid-state reaction. In the title compound, the [V2PO8] framework is built up from infinite pyramidal [V2O8]∞ and [VPO7]∞ chains linked together by V-O-P bridges, leading to a three-dimensional framework which delimits two types of inter-secting tunnels running along [100] and [010] in which the four unique K(+) ions, showing coordination numbers of nine and ten, are located.

Disodium molybdenum dioxide diarsenate, Na2MoO2As2O7, has been synthesized by a solid-state reaction. The structure is built up from MoAs2O12 linear units sharing corners to form a three-dimensional framework containing tunnels running along the a-axis direction in which the Na(+) cations are located. In this framework, the As(V) atoms are tetra-hedrally coordinated and form an As2O7 group. The Mo(VI) atom is displaced from the center of an octa-hedron of O atoms. Two Na(+) cations are disordered about inversion centres. Structural relationships between different compounds: A2MoO2As2O7 (A = K, Rb), AMOP2O7 (A = Na, K, Rb; M = Mo, Nb) and MoP2O7 are discussed.