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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Inorganic Chemistry".

Deadline for manuscript submissions: closed (31 December 2024) | Viewed by 12122

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Prof. Dr. Giuseppe Cavallaro

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Dipartimento di Fisica e Chimica, Università degli Studi di Palermo, Viale delle Scienze, pad. 17, 90128 Palermo, Italy
Interests: bionanocomposite films based on sustainable polymers and nanoclay; nanomaterials for cultural heritage; nanocarriers for drug delivery; adsorbent nanomaterials for remediation
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Prof. Dr. Athanassios C. Tsipis

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Laboratory of Inorganic and General Chemistry, Department of Chemistry, University of Ioannina, 45110 Ioannina, Greece
Interests: DFT; catalysis; anticancer drugs; photodynamic therapy; photophysical properties; intermolecular interactions; metallaromaticity
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Dr. Carla Bazzicalupi

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Department of Chemistry, University of Florence, Via della Lastruccia, 3-13-50019 Sesto Fiorentino, Florence, Italy
Interests: X-ray diffraction; molecular modeling techniques; supramolecular chemistry; weak interactions; coordination of environmentally and/or biologically relevant species; non-B DNA foldings; DNA G-quadruplexes
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Special Issue Information

Dear Colleagues,

This Special Issue of Molecules is dedicated to recent advances in inorganic chemistry and mainly comprises a selection of exclusive papers by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section. While contributions from other authors will also be considered, this Special Issue focuses primarily on highlighting recent interesting investigations conducted in the laboratories of our Section’s EBMs, providing an attractive open access publishing platform for inorganic chemistry research data.

Prof. Dr. Giuseppe Cavallaro
Prof. Dr. Athanassios C. Tsipis
Dr. Carla Bazzicalupi
Guest Editors

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Keywords

coordination chemistry
main-group chemistry
bioinorganic chemistry
organometallic compounds
solid-state chemistry
inorganic cluster chemistry

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Published Papers (11 papers)

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Research

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16 pages, 4010 KiB

Open AccessArticle

Monitoring of Fe(II) Spin Transition in Cu(II)-Doped Spin-Crossover Nanoparticles

by Alexander Charitos, Vassilis Tangoulis, John Parthenios, Ondrej Malina, Radim Mach, Nikolaos Ioannidis and Nikolia Lalioti

Molecules 2025, 30(6), 1258; https://doi.org/10.3390/molecules30061258 - 11 Mar 2025

Viewed by 514

Abstract

Experimental protocols based on Electron Paramagnetic Resonance (EPR) and Raman spectroscopy are presented for the investigation of the Fe(II) spin transition in Cu(II)-doped 1-D spin-crossover (SCO) nanoparticles of the type [Fe_1−xCu_x(NH₂trz)₃]Br₂ where x = 0.03 and 0.06 and NH₂trz = 4-amino-1, 2, 4-triazole. The resulting nanoparticles were characterized using Transmission Electron Microscopy (TEM), Infrared (IR) spectroscopy, and powder X-ray diffraction (p-XRD). Magnetic susceptibility measurements revealed a dependence on the scan rate, with critical temperatures and hysteresis widths varying accordingly. EPR spectroscopy provided insights into the doped nanoparticles’ structural changes and spin-state transitions. The Cu(II) dopants exhibited significant g-factor anisotropy and hyperfine structure, indicative of a distorted octahedral coordination. The EPR spectra indicated that the spin transition occurs in domains populated by ions of the same spin state. Cu(II) ions show different spectral characteristics depending on whether they are in high-spin or low-spin domains of Fe(II). Changes in Raman bands induced by laser power reveal structural and electronic rearrangements during the LS to HS transition. The findings provide insights into metal–ligand interactions and the molecular mechanisms underlying the SCO process. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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12 pages, 2231 KiB

Open AccessArticle

An In-Plane Heterostructure Ni₃N/MoSe₂ Loaded on Nitrogen-Doped Reduced Graphene Oxide Enhances the Catalyst Performance for Hydrogen Oxidation Reaction

by Abrar Qadir, Peng-Peng Guo, Yong-Zhi Su, Kun-Zu Yang, Xin Liu, Ping-Jie Wei and Jin-Gang Liu

Molecules 2025, 30(3), 488; https://doi.org/10.3390/molecules30030488 - 22 Jan 2025

Viewed by 852

Abstract

Non-noble metal electrocatalysts for the hydrogen oxidation reaction (HOR) that are both highly active and low-cost are essential for the widespread use of fuel cells. Herein, a simple two-step method for creating an in-plane heterostructure of Ni₃N/MoSe₂ loaded on N-doped reduced graphene oxide (Ni₃N/MoSe₂@N-rGO) as an effective electrocatalyst for the HOR is described. The process involves hydrothermal treatment of the Ni and Mo precursors with N-doped reduced graphene oxide, followed by the annealing with urea. The Ni₃N/MoSe₂@N-rGO catalyst exhibits high activities for the HOR, with current densities of 2.15 and 3.06 mA cm⁻² at 0.5 V vs. the reversible hydrogen electrode (RHE) in H₂-saturated 0.1 M KOH and 0.1 M HClO₄ electrolytes, respectively, which is comparable to a commercial 20% Pt/C catalyst under similar experimental conditions. Furthermore, the catalyst demonstrates excellent durability, maintaining its performance during accelerated degradation tests for 5000 cycles. This work offers a practical framework for the designing and preparing of non-precious metal electrocatalysts for the HOR in fuel cells. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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19 pages, 6149 KiB

Open AccessArticle

Coordination Chemistry of Mixed-Donor Pyridine-Containing Macrocyclic Ligands: From Optical to Redox Chemosensors for Heavy Metal Ions

by Alessandra Garau, Alexander J. Blake, Maria Carla Aragoni, Massimiliano Arca, Claudia Caltagirone, Francesco Demartin, Vito Lippolis, Giacomo Picci and Enrico Podda

Molecules 2025, 30(1), 130; https://doi.org/10.3390/molecules30010130 - 31 Dec 2024

Viewed by 818

Abstract

2,8-Dithia-5-aza-2,6-pyridinophane (L1) has been used as a receptor unit in the construction of the conjugated redox chemosensor 5-ferrocenylmethyl-2,8-dithia-5-aza-2,6-pyridinophane (L3). In order to further explore the coordination chemistry of L1, and comparatively, that of its structural analogue 2,11-dithia-5,8-diaza-2,6-pyridinophane (L2), featuring two secondary nitrogen atoms in the macrocyclic unit, the crystal structures of the new synthesised complexes [Pb(L1)(ClO₄)₂]·½CH₃CN, [Cu(L2)](ClO₄)₂·CH₃CN and [Cd(L2)(NO₃)]NO₃ were determined by X-ray diffraction analysis. The electrochemical response of L3 towards the metal ions Cu²⁺, Zn²⁺, Cd²⁺, Hg²⁺, and Pb²⁺ was investigated by cyclic voltammetry (CV) in CH₂Cl₂/CH₃CN 0.25:1 (v/v) mixture. Upon addition to L3 of increasing amounts of the aforementioned metal cations, the wave corresponding to the Fc⁺/Fc redox couple of the un-complexed L3 was gradually replaced by a new reversible wave at more positive potentials and corresponding to the Fc⁺/Fc redox couple of the complexed ligand. The maximum anodic shift of the ferrocene oxidation wave is observed in the presence of Pb²⁺ (230 mV), to which corresponds a reaction coupling efficiency (RCE) value as large as 7.9 × 10³. The response selectivity of L3 is discussed in reference to the optical selectivity observed for conjugated chemosensors featuring L1 as receptor unit and different fluorogenic fragments as signalling units. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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22 pages, 4654 KiB

Open AccessArticle

Synthesis, Characterization and Antimicrobial Activity of Trimethylantimony(V) Biscyanoximates, a New Family of Antimicrobials

by Seth A. Amankrah, Tarosha Salpadoru, Kaitlyn Cotton, Marianna A. Patrauchan, Karen L. Wozniak and Nikolay Gerasimchuk

Molecules 2024, 29(23), 5779; https://doi.org/10.3390/molecules29235779 - 6 Dec 2024

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Abstract

Antimicrobial compounds play a critical role in combating microbial infections. However, the emergence of antibiotic and antifungal resistance and the scarcity of new antibiotic developments pose a significant threat and demand the discovery of new antimicrobials for both bacterial and fungal pathogens. Our previous work described the first generation (G1) of organoantimony-based compounds that showed antimicrobial activity against several bacterial and fungal pathogens. Here, we present our efforts in modifying these compounds by replacing the tetraphenyl backbone in G1 compounds with a trimethyl group, thereby generating a new series of compounds we refer to as “generation 2”, G2. In addition to the novel backbone structure, we introduced three new anionic chloro-cyanoxime ligand groups, namely 2,4-diCl-PhCO⁻, 2,6-diCl-PhCO⁻ and 2Cl-PhCO⁻, which were found to be biologically active in the past. Nine new compounds of SbMe₃L₂ composition were obtained in high yields and characterized by NMR, IR spectroscopies, thermogravimetric TG/DSC and X-ray single crystal analyses. The antibacterial activity of the cyanoximates was tested against three bacterial (Pseudomonas aeruginosa PAO1, Escherichia coli S17 and methicillin-resistant Staphylococcus aureus (MRSA) NRS70) and two fungal (Candida albicans strain SC5314 and Cryptococcus neoformans strain H99) pathogens. Two compounds, SbMe₃(MCO)₂ and SbMe₃(2,4-diClPhCO)₂, were active against bacterial strains and inhibited the growth of PAO1 and MRSA with MICs of 50 and 100 µg/mL, respectively. Three compounds, SbMe₃(MCO)₂, SbMe₃(ECO)₂ and SbMe₃(TCO)₂, were active against fungal strains and inhibited either one of or both C. albicans and C. neoformans at MICs of 2.6–66.67 μg/mL. In addition, SbMe₃(TCO)₂ and SbMe₃(MCO)₂ were fungicidal at MFC 33.33–66.67 μg/mL. Ultra-thin-layer TEM imaging suggested that SbMe₃(MCO)₂ targets the integrity of bacterial membranes. Overall, four of the studied G2 series compounds possess antimicrobial activity against a broad range of microbial pathogens, with particular potential against fungal pathogens, which will be explored in further studies. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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12 pages, 3910 KiB

Open AccessArticle

Fast and Sensitive Determination of Iodide Based on Ternary Chalcogenides Nanoparticles

by Zhitai Wang, Nengtao Wu, Weihao Wang, Yaozheng Hu, Zhijie Luo, Yuhui Zheng and Qianming Wang

Molecules 2024, 29(19), 4751; https://doi.org/10.3390/molecules29194751 - 8 Oct 2024

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Abstract

A fluorescent probe based on ternary AgFeS₂ quantum dots has been prepared for the design of ternary chalcogenides. The nanoparticles are synthesized with oleylamine as a stabilizer at a low temperature (particle size in the range of 2 to 3 nm) and they exhibit an intense blue emission in aqueous media. As for their internal structure, each nanoparticle’s relative stoichiometric ratio (AgFe_1.01S_1.91) is very close to the theoretical value of 1:1:2. Their magnetic properties have been studied with a vibrating sample magnetometer and they have ferromagnetism between 4 K and 298 K (applied magnetic field ranging between −10,000 and 10,000 Oe). In the presence of iodide ions, the emission at 458 nm derived from AgFeS₂ QDs has been observed to give rise to fluorescence quenching. The detection system is based on a static quenching process and morphological change between iodide ions and AgFeS₂, which has a good linear range from 0 to 37.5 μmol/L, with a limit of detection of 0.99 μM. The nanoprobe responds within 30 s for the efficient detection of iodide. Such functional quantum dots will provide a powerful indicator in environmental and bio-sensing applications. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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20 pages, 3981 KiB

Open AccessArticle

Functionalizing Thiosemicarbazones for Covalent Conjugation

by Johannes Hohnsen, Lukas Rryci, Diana Obretenova, Joshua Friedel, Shahab Jouchaghani and Axel Klein

Molecules 2024, 29(15), 3680; https://doi.org/10.3390/molecules29153680 - 3 Aug 2024

Viewed by 1435

Abstract

Thiosemicarbazones (TSCs) with their modular character (thiosemicarbazides + carbonyl compound) allow broad variation of up to four substituents on the main R¹R²C=N(1)–NH–C(S)–N(4)R³R⁴ core and are thus interesting tools for the formation of conjugates or the functionalization of nanoparticles (NPs). In this work, di-2-pyridyl ketone was introduced for the coordination of metals and 9-anthraldehyde for luminescence as R¹ and R² to TSCs. R³ and R⁴ substituents were varied for the formation of conjugates. Amino acids were introduced at the N4 position to produce [R¹R²TSC–spacer–amino acid] conjugates. Further, functions such as phosphonic acid (R–P(O)(OH)₂), D-glucose, o-hydroquinone, OH, and thiol (SH) were introduced at the N4 position producing [R¹R²TSC–spacer–anchor group] conjugates for direct NP anchoring. Phenyl, cyclohexyl, benzyl, ethyl and methyl were used as spacer units. Both phenyl phosphonic acid TSC derivatives were bound on TiO₂ NPs as a first example of direct NP anchoring. [R¹R²TSC–spacer–end group] conjugates including OH, S–Bn (Bn = benzyl), NH–Boc (Boc = tert-butyloxycarbonyl), COOtBu, C≡CH, or N₃ end groups were synthesized for potential covalent binding to functional molecules or functionalized NPs through amide, ester, or triazole functions. The synthesis of the thiosemicarbazides H₂NNH–C(S)–NR₃R₄ starting from amines, including amino acids, SCCl₂ or CS₂, and hydrazine and their condensation with dipyridyl ketone and anthraldehyde led to 34 new TSC derivatives. They were synthesized in up to six steps with overall yields ranging from 10 to 85% and were characterized by a combination of nuclear magnetic resonance spectroscopy and mass spectrometry. UV-vis absorption and photoluminescence spectroscopy allowed us to easily trace the dipyridyl imine and anthracene chromophores. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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17 pages, 2271 KiB

Open AccessArticle

Systematic Study of Different Types of Interactions in α-, β- and γ-Cyclodextrin: Quantum Chemical Investigation

by Imre Bakó, László Jicsinszky and Szilvia Pothoczki

Molecules 2024, 29(10), 2205; https://doi.org/10.3390/molecules29102205 - 8 May 2024

Cited by 2 | Viewed by 1354

Abstract

In this work, comprehensive ab initio quantum chemical calculations using the DFT level of theory were performed to characterize the stabilization interactions (H-bonding and hyperconjugation effects) of two stable symmetrical conformations of α-, β-, and γ-cyclodextrins (CDs). For this purpose, we analyzed the electron density using “Atom in molecules” (AIM), “Natural Bond Orbital” (NBO), and energy decomposition method (CECA) in 3D and in Hilbert space. We also calculated the H-bond lengths and OH vibrational frequencies. In every investigated CD, the quantum chemical descriptors characterizing the strength of the interactions between the H-bonds of the primary OH (or hydroxymethyl) and secondary OH groups are examined by comparing the same quantity calculated for ethylene glycol, α-d-glucose (α-d-Glcp) and a water cluster as reference systems. By using these external standards, we can characterize more quantitatively the properties of these bonds (e.g., strength). We have demonstrated that bond critical points (BCP) of intra-unit H-bonds are absent in cyclodextrins, similar to α-d-Glcp and ethylene glycol. In contrast, the CECA analysis showed the existence of an exchange (bond-like) interaction between the interacting O…H atoms. Consequently, the exchange interaction refers to a chemical bond, namely the H-bond between two atoms, unlike BCP, which is not suitable for its detection. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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23 pages, 6719 KiB

Open AccessArticle

Old Acquaintances and Novel Complex Structures for the Ni(II) and Cu(II) Complexes of bis-Chelate Oxime–Amide Ligands

by Carla Bazzicalupi, Craig Grimmer and Igor Vasyl Nikolayenko

Molecules 2024, 29(2), 522; https://doi.org/10.3390/molecules29020522 - 20 Jan 2024

Cited by 2 | Viewed by 1583

Abstract

In the process of systematically studying the methylhydroxyiminoethaneamide bis-chelate ligands with polymethylene spacers of different lengths, L1–L3, and their transition metal complexes, a number of new Ni(II) and Cu(II) species have been isolated, and their molecular and crystal structures were determined using single-crystal X-ray diffraction. In all of these compounds, the divalent metal is coordinated by the ligand donor atoms in a square-planar arrangement. In addition, a serendipitously discovered new type of neutral Ni(II) complex, where the propane spacer of ligand L2 underwent oxidation to the propene spacer, and one of the amide groups was oxidised to the ketoimine, is also reported. The resulting ligand L2′ affords the formation of neutral planar Ni(II) complexes, which are assembled in the solid state on top of each other, and yield two polymorphic structures. In both structures, the resulting infinite, exclusively parallel metal ion columns in ligand insulation may serve as precursor materials for sub-nano-conducting connectors. Overall, this paper reports the synthesis and characterisation of seven new anionic, cationic, and neutral Ni(II) and Cu(II) complexes, their crystal structures, as well as experimental and computed UV–Vis absorption spectra for two structurally similar Ni(II) complexes, yellow and red. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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Review

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34 pages, 10137 KiB

Open AccessReview

Progress in Luminescent Materials Based on Europium(III) Complexes of β-Diketones and Organic Carboxylic Acids

by Qianting Chen, Jie Zhang, Quanfeng Ye, Shanqi Qin, Lingyi Li, Mingyu Teng and Wai-Yeung Wong

Molecules 2025, 30(6), 1342; https://doi.org/10.3390/molecules30061342 - 17 Mar 2025

Viewed by 482

Abstract

Europium(III) β-diketone and organic carboxylic acid complexes are designable, easy to prepare, and easy to modify and have excellent fluorescence properties (narrow emission spectral band, high colour purity, long fluorescence lifetime, high quantum yield, and a spectral emission range covering both the visible and near-infrared regions). These complexes play important roles in popular fields such as laser and fibre-optic communications, medical diagnostics, immunoassays, fluorescent lasers, sensors, anticounterfeiting, and organic light-emitting diodes (OLEDs). In the field of light-emitting materials, europium complexes are especially widely used in OLED lamps, especially because of their high-efficiency emission of red (among the three primary colours); accordingly, these complexes can be mixed with blue and green phosphors to obtain high-efficiency white phosphors that can be excited by near-ultraviolet light. This paper reviews the red-light-emitting europium complexes with β-diketone and organic carboxylic acid as ligands that have been studied over the last five years, describes the current problems, and discusses their future application prospects. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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37 pages, 2813 KiB

Open AccessReview

Manganese Oxide Nanoparticles for MRI-Based Multimodal Imaging and Theranostics

by Carlos F. G. C. Geraldes

Molecules 2024, 29(23), 5591; https://doi.org/10.3390/molecules29235591 - 26 Nov 2024

Cited by 2 | Viewed by 1193

Abstract

Manganese-based MRI contrast agents have recently attracted much attention as an alternative to Gd-based compounds. Various nanostructures have been proposed for potential applications in in vivo diagnostics and theranostics. This review is focused on the discussion of different types of Mn oxide-based nanoparticles (Mn_xO_y NPs) obtained at the +2, +3 and +4 oxidation states for MRI, multimodal imaging or theranostic applications. These NPs show favorable magnetic properties, good biocompatibility, and an improved toxicity profile relative to Gd(III)-based nanosystems, showing that the Mn paramagnetic ions offer advantages for the next generation of nanoscale MRI and theranostic contrast agents. Their potential for enhancing relaxivity and MRI contrast effects is illustrated through discussion of selected examples published in the past decade. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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34 pages, 18408 KiB

Open AccessReview

Bis(Dicarbollide) Complexes of Transition Metals: How Substituents in Dicarbollide Ligands Affect the Geometry and Properties of the Complexes

by Igor B. Sivaev

Molecules 2024, 29(15), 3510; https://doi.org/10.3390/molecules29153510 - 26 Jul 2024

Cited by 2 | Viewed by 1358

Abstract

The interaction between different types of substituents in dicarbollide ligands and their influence on the stabilization of various rotational conformers (rotamers) of transition metal bis(dicarbollide) complexes [3,3′-M(1,2-C₂B₉H₁₁)₂]⁻ are considered. It has been shown that the formation of intramolecular CH···X hydrogen bonds between dicarbollide ligands is determined by the size of the proton acceptor atom X rather than its electronegativity. Due to the stabilization of rotamers with different dipole moments, intramolecular hydrogen bonds between ligands in transition metal bis(dicarbollide) complexes can have a significant impact on the biological properties of their derivatives. In the presence of external complexing metals, weak intramolecular CH···X hydrogen bonds can be broken to form stronger X—>M donor-acceptor bonds. This process is accompanied by the mutual rotation of dicarbollide ligands and can be used in sensors and molecular switches based on transition metal bis(dicarbollide) complexes. Full article

(This article belongs to the Special Issue Exclusive Contributions by the Editorial Board Members (EBMs) of the Inorganic Chemistry Section of Molecules 2024)

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