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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 August 2024) | Viewed by 16676

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Dr. Huahong Zou

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School of Chemistry and Pharmaceutical Science, Guangxi Normal University, Guilin, China
Interests: high-nuclear Ln(III) cluster; molecular magnetism; assembly mechanism; assembly process; crystal structure
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Dear Colleagues,

The sustainable development of metal complexes is an interesting and significant topic, attracting increasing attention due to the complexes’ aesthetically pleasing structures and unique electronic and stereochemical properties. Their sustainable development has been successfully applied in the fields of solid-state lighting, biological diagnosis treatment, molecular magnetism, catalysis, adsorption, and intelligent sensing, and is gradually moving towards emerging fields. In addition, metal complexes contain both inorganic and organic substances. Therefore, the unique physical and chemical properties of both inorganic and organic compounds are of great significance for the development of a new generation of multifunctional materials, and various multifunctional metal complexes have emerged. However, chemists prefer to select specific organic ligands and metal ions to synthesize metal complexes with certain specificity, in particular, the design and synthesis of finite high-nuclear metal complexes with specific structural connections, beautiful topologies, and rich properties. In recent years, high-nuclear metal complexes have attracted intense interest, which can be attributed to their wide application value in emerging fields such as luminescent materials, chemical sensors, biosensors, catalysis, and smart materials. With the development of science and technology, focus on metal complexes has become more and more specific and scientific, which provides valuable opportunities for their cross-application in different fields.

Dr. Huahong Zou
Guest Editor

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Keywords

high-nuclear complexes
magnetism
catalysis
fluorescence
adsorption

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Published Papers (12 papers)

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Research

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13 pages, 1816 KiB

Open AccessArticle

Palladium(II) and Platinum(II) Complexes Bearing ONS-Type Pincer Ligands: Synthesis, Characterization and Catalytic Investigations

by Alfonso Castiñeiras and Isabel García-Santos

Molecules 2024, 29(14), 3425; https://doi.org/10.3390/molecules29143425 - 22 Jul 2024

Viewed by 815

Abstract

This work describes the synthesis of eight new Pd(II) and Pt(II) complexes with the general formula [M(TSC)Cl], where TSC represents the 4N-monosubstituted thiosemicarbazone derived from 2-acetylpyridine N-oxide with the substituents CH₃ (H4MLO), C₂H₅ (H4ELO), phenyl (H4PLO) and (CH₃)₂ (H4DMLO). These complexes have been characterized by elemental analysis, molar conductivity, IR spectroscopy, ¹H, ¹³C, ¹⁹⁵Pt and ESI-MS. The complexes exhibit a square planar geometry around the metallic center coordinated by a thiosemicarbazone molecule acting as a donor ONS-type pincer ligand and by a chloride, as confirmed by the molecular structures of the complexes, [Pd(4ELO)Cl] (3) and [Pd(4PLO)Cl] (5), determined by single-crystal X-ray diffraction. The ¹⁹⁵Pt NMR spectra of the complexes of formulae [Pt(4PLO)Cl] (6) and [Pt(4DMLO)Cl] (8) in DMSO show a single signal at −2420.4 ppm, confirming the absence of solvolysis products. Complexes 3 and 5 have been tested as catalysts in the Suzuki–Miyaura cross-coupling reactions of aryl bromides with phenylboronic acid, with yields of between 50 and 90% Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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11 pages, 1955 KiB

Open AccessArticle

Chiral Star-Shaped [Co^III₃Ln^III] Clusters with Enantiopure Schiff Bases: Synthesis, Structure, and Magnetism

by Liudi Ji, Juntao Wang, Zeyu Li, Xiaoming Zhu and Peng Hu

Molecules 2024, 29(14), 3304; https://doi.org/10.3390/molecules29143304 - 12 Jul 2024

Viewed by 869

Abstract

Two enantiomeric pairs of new 3d–4f heterometallic clusters have been synthesized from two enantiomer Schiff base derivatives: (R/S)-2-[(2-hydroxy-1-phenylethylimino)methyl] phenol (R-/S-H₂L). The formulae of the series clusters are Co₃Ln(R-L)₆ (Ln = Dy (1R), Gd (2R)), Co₃Ln (S-L)₆ (Ln = Dy (1S), Gd (2S)), whose crystal structures and magnetic properties have been characterized. Structural analysis indicated that the above clusters crystallize in the chiral P2₁3 group space. The central lanthanide ion has a coordination geometry of D₃ surrounded by three [Co^III(L)₂]^– anions using six aliphatic oxygen atoms of L²⁻ featuring a star-shaped [Co^III₃Ln^III] configuration. Magnetic measurements showed the presence of slow magnetic relaxation with an effective energy barrier of 22.33 K in the Dy^III derivatives under a zero-dc field. Furthermore, the circular dichroism (CD) spectra of 1R and 1S confirmed their enantiomeric nature. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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20 pages, 7706 KiB

Open AccessArticle

Magnetic Ion-Imprinted Materials for Selective Adsorption of Cr(VI): Adsorption Behavior and Mechanism Study

by Shunfei Li, Siqing Ye, Weiye Zhang, Hongxing He, Yi Zhang, Mingyang Xiong, Yuhan Chen, Mingqiu Wang and Zhifeng Nie

Molecules 2024, 29(9), 1952; https://doi.org/10.3390/molecules29091952 - 24 Apr 2024

Cited by 1 | Viewed by 956

Abstract

With the increase of hexavalent Cr(VI) wastewater discharged from industrial production, it seriously pollutes water bodies and poses a risk to human health. Adsorption is used as an effective means to treat Cr(VI), but its effectiveness is affected by pH, and the adsorption performance decreases when acidity is strong. Furthermore, research on the mechanism of Cr(VI) adsorption using DFT calculations needs to be developed. This study focuses on the development of magnetically responsive core–shell nano-ion imprinted materials (Fe₃O₄@GO@IIP) through magnetic separation and surface imprinting techniques. Characterization techniques including FT-IR, XRD, and EDS confirmed the core–shell nanostructure of Fe₃O₄@GO@IIP. Batch adsorption experiments and model simulations demonstrated the exceptional adsorption capacity of Fe₃O₄@GO@IIP for Cr(VI) in strongly acidic solutions (pH = 1), reaching a maximum of 89.18 mg/g. The adsorption mechanism was elucidated through XPS and DFT calculations, revealing that Fe₃O₄@GO@IIP operates through electrostatic interactions and chemical adsorption, with charge transfer dynamics quantified during the process. This research provides new insights for addressing Cr(VI) treatment in highly acidic environments. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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20 pages, 4077 KiB

Open AccessArticle

Investigating Ligand Sphere Perturbations on Mn^III–Alkylperoxo Complexes

by Samuel A. Brunclik, Elizabeth N. Grotemeyer, Zahra Aghaei, Mohammad Rasel Mian and Timothy A. Jackson

Molecules 2024, 29(8), 1849; https://doi.org/10.3390/molecules29081849 - 18 Apr 2024

Viewed by 1357

Abstract

Manganese catalysts that activate hydrogen peroxide carry out several different hydrocarbon oxidation reactions with high stereoselectivity. The commonly proposed mechanism for these reactions involves a key manganese(III)-hydroperoxo intermediate, which decays via O–O bond heterolysis to generate a Mn(V)–oxo species that institutes substrate oxidation. Due to the scarcity of characterized Mn^III–hydroperoxo complexes, Mn^III–alkylperoxo complexes are employed to understand factors that affect the mechanism of the O–O cleavage. Herein, we report a series of novel complexes, including two room-temperature-stable Mn^III–alkylperoxo species, supported by a new amide-containing pentadentate ligand (^6Medpaq^5NO2). We use a combination of spectroscopic methods and density functional theory computations to probe the effects of the electronic changes in the ligand sphere trans to the hydroxo and alkylperoxo units to thermal stability and reactivity. The structural characterizations for both Mn^II(OTf)(^6Medpaq^5NO2) and [Mn^III(OH)(^6Medpaq^5NO2)](OTf) were obtained via single-crystal X-ray crystallography. A perturbation to the ligand sphere allowed for a marked increase in reactivity towards an organic substrate, a modest change in the distribution of the O–O cleavage products from homolytic and heterolytic pathways, and little change in thermal stability. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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15 pages, 2719 KiB

Open AccessArticle

DFT Studies of Dimethylaminophenyl-Substituted Phthalocyanine and Its Silver Complexes

by Martin Breza

Molecules 2024, 29(6), 1344; https://doi.org/10.3390/molecules29061344 - 18 Mar 2024

Viewed by 907

Abstract

The dimethylaminophenyl-substituted silver phthalocyanine [dmaphPcAg] can be used as a UV-vis photoinitiator for in situ preparation of a silver/polymer nanocomposite. To verify early steps of the supposed mechanism of radical polymerization, we performed quantum chemical calculations of ^m[dmaphPcAg]^q complexes with charges q = +1 to −2 in the two lowest spin states m, of a free ligand and its dehydrogenated/deprotonated products ^m[dmaphPcH_n]^q, n = 2 to 0, q = 0, −1 or −2, in the lowest spin states m. The calculated electronic structures and electron transitions of all the optimized structures in CHCl₃ solutions are compared with experimental EPR and UV-vis spectra, respectively. The unstable ³[dmaphPcAg]⁺ species deduced only from previous EPR spin trap experiments was identified. In addition to ²[dmaphPcAg]⁰, our results suggest the coexistence of both reaction intermediates ¹[dmaphPcAg]⁻ and ³[dmaphPcAg]⁻ in reaction solutions. Silver nanoparticle formation is a weak point of the supposed reaction mechanism from the energetic, stereochemistry, and electronic structure points of view. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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21 pages, 3284 KiB

Open AccessArticle

New Copper Complexes with N,O-Donor Ligands Based on Pyrazole Moieties Supported by 3-Substituted Acetylacetone Scaffolds

by Jo’ Del Gobbo, Carlo Santini, Alessandro Dolmella, Zhenzhen Li, Miriam Caviglia and Maura Pellei

Molecules 2024, 29(3), 621; https://doi.org/10.3390/molecules29030621 - 28 Jan 2024

Cited by 2 | Viewed by 1541

Abstract

The new 3-monosubstituted acetylacetone ligands, 3-(phenyl(1H-pyrazol-1-yl)methyl)pentane-2,4-dione (HL^acPz) and 3-((3,5-dimethyl-1H-pyrazol-1-yl)(phenyl)methyl)pentane-2,4-dione (HL^acPzMe), were synthesized and used as supporting ligands for new copper(II) and copper(I) phosphane complexes of the general formulae [Cu(HL^acX)₂(L^acX)₂] and [Cu(PPh₃)₂(HL^acX)]PF₆ (X = Pz (pyrazole) or PzMe (3,5-dimethylpyrazole)), respectively. In the syntheses of the Cu(I) complexes, the triphenylphosphine coligand (PPh₃) was used to stabilize copper in the +1 oxidation state, avoiding oxidation to Cu(II). All compounds were characterized by CHN analysis, ¹H-NMR, ¹³C-NMR, FT-IR spectroscopy, and electrospray ionization mass spectrometry (ESI-MS). The ligands HL^acPz (1) and HL^acPzMe (2) and the copper complex [Cu(PPh₃)₂(HL^acPz)]PF₆ (3) were also characterized by X-ray crystallography. The reactivity of these new compounds was investigated and the new compounds 4-phenyl-4-(1H-pyrazol-1-yl)butan-2-one (7) and 4-(3,5-dimethyl-1H-pyrazol-1-yl)-4-phenylbutan-2-one (8) were obtained in basic conditions via the retro-Claisen reaction of related 3-monosubstituted acetylacetone, providing efficient access to synthetically useful ketone compounds. Compound 8 was also characterized by X-ray crystallography. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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14 pages, 2746 KiB

Open AccessArticle

Luminescent Behavior of Zn(II) and Mn(II) Halide Derivatives of 4-Phenyldinaphtho[2,1-d:1′,2′-f][1,3,2]dioxaphosphepine 4-Oxide and Single-Crystal X-ray Structure Determination of the Ligand

by Valentina Ferraro, Jesús Castro and Marco Bortoluzzi

Molecules 2024, 29(1), 239; https://doi.org/10.3390/molecules29010239 - 1 Jan 2024

Cited by 1 | Viewed by 1333

Abstract

The two enantiomers of chiral phosphonate 4-phenyldinaphtho[2,1-d:1′,2′-f][1,3,2]dioxaphosphepine 4-oxide, O=PPh(BINOL), were synthesized from the proper 1,1′-bi-2-naphtol (BINOL) enantiomer and characterized. The structure of the (S)-enantiomer was elucidated by means of single-crystal X-ray diffraction. The reaction with anhydrous ZnBr₂ afforded complexes having the general formula [ZnBr₂{O=PPh(BINOL)}₂] that showed intense fluorescence centered in the near-UV region rationalized on the basis of TD-DFT calculations. The corresponding Mn(II) complexes with the general formula [MnX₂{O=PPh(BINOL)}₂] (X = Cl, Br) exhibited dual emission upon excitation with UV light, with the relative intensity of the bands dependent upon the choice of the halide. The highest energy transition is comparable with that of the Zn(II) complex, while the lowest energy emission falls in the red region of the spectrum and is characterized by lifetimes in the hundreds of microseconds range. Although the emission at lower energy can also be achieved by direct excitation of the metal center, the luminescence decay curves suggest that the band in the red range is possibly derived from BINOL-centered excited states populated by intersystem crossing. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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14 pages, 1635 KiB

Open AccessArticle

Synthesis and Characterization of Iridium(III) Complexes with Substituted Phenylimidazo(4,5-f)1,10-phenanthroline Ancillary Ligands and Their Application in LEC Devices

by Bárbara Vásquez, Max Bayas, Paulina Dreyse, Juan Luis Palma, Alan R. Cabrera, Elena Rossin, Mirco Natali, Cesar Saldias and Iván González-Pavez

Molecules 2024, 29(1), 53; https://doi.org/10.3390/molecules29010053 - 21 Dec 2023

Viewed by 2114

Abstract

In this work, we report on the synthesis and characterization of six new iridium(III) complexes of the type [Ir(C^N)₂(N^N)]⁺ using 2-phenylpyridine (C1–3) and its fluorinated derivative (C4–6) as cyclometalating ligands (C^N) and R-phenylimidazo(4,5-f)1,10-phenanthroline (R = H, CH₃, F) as the ancillary ligand (N^N). These luminescent complexes have been fully characterized through optical and electrochemical studies. In solution, the C4–6 series exhibits quantum yields (Ф) twice as high as the C1–3 series, exceeding 60% in dichloromethane and where ³MLCT/³LLCT and ³LC emissions participate in the phenomenon. These complexes were employed in the active layer of light-emitting electrochemical cells (LECs). Device performance of maximum luminance values of up to 21.7 Lx at 14.7 V were observed for the C2 complex and long lifetimes for the C1–3 series. These values are counterintuitive to the quantum yields observed in solution. Thus, we established that the rigidity of the system and the structure of the solid matrix dramatically affect the electronic properties of the complex. This research contributes to understanding the effects of the modifications in the ancillary and cyclometalating ligands, the photophysics of the complexes, and their performance in LEC devices. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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10 pages, 1630 KiB

Open AccessCommunication

Russian Doll-like 3d–4f Cluster Wheels with Slow Relaxation of Magnetization

by Lan Liu, Panpan Yang, Zhihui Qiu, Kai Wang, Dongcheng Liu, Yuning Liang, Huancheng Hu, Huahong Zou, Fupei Liang and Zilu Chen

Molecules 2023, 28(15), 5906; https://doi.org/10.3390/molecules28155906 - 6 Aug 2023

Cited by 1 | Viewed by 1461

Abstract

The solvothermal reactions of LnCl₃·6H₂O and MCl₂·6H₂O (M = Co, Ni) with 2,2′-diphenol (H₂L¹) and 5,7-dichloro-8-hydroxyquinoline (HL²) gave three 3d–4f heterometallic wheel-like nano-clusters [Ln₇M₆(L¹)₆(L²)₆(µ₃-OH)₆(OCH₃)₆Cl(CH₃CN)₆]Cl₂·xH₂O (Ln = Dy, M = Co, x = 3 for 1; Ln = Dy, M = Ni, x = 0 for 2; Ln = Tb, M = Ni, x = 0 for 3) with similar cluster structure. The innermost Ln(III) ion is encapsulated in a planar Ln₆ ring which is further embedded in a chair-conformation M₆ ring, constructing a Russian doll-like 3d–4f cluster wheel Ln(III)⸦Ln₆⸦M₆. 2 and 3 show obvious slow magnetic relaxation behavior with negligible opening of the magnetic hysteresis loop. Such a Russian doll-like 3d–4f cluster wheel with the lanthanide disc isolated by transition metallo-ring is rarely reported. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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12 pages, 2170 KiB

Open AccessArticle

Synthesis and Characterization of Iron Bispyridine Bisdicyanamide, Fe[C₅H₅N]₂[N(CN)₂]₂

by Laura Henrich, Peter C. Müller, Jan Hempelmann, Markus Mann, Jan van Leusen, Simon Steinberg and Richard Dronskowski

Molecules 2023, 28(13), 4886; https://doi.org/10.3390/molecules28134886 - 21 Jun 2023

Cited by 1 | Viewed by 1439

Abstract

Fe[C₅H₅N]₂[N(CN)₂]₂ (1) was synthesized from a reaction of stoichiometric amounts of NaN(CN)₂ and FeCl₂·4H₂O in a methanol/pyridine solution. Single-crystal and powder diffraction show that 1 crystallizes in the monoclinic space group I2/m (no. 12), different from Mn[C₅H₅N]₂[N(CN)₂]₂ (P2₁/c, no. 14) due to tilted pyridine rings, with a = 7.453(7) Å, b = 13.167(13) Å, c = 8.522(6) Å, β = 114.98(6)° and Z = 2. ATR-IR, AAS, and CHN measurements confirm the presence of dicyanamide and pyridine. Thermogravimetric analysis shows that π-stacking interactions of the pyridine rings play an important role in structural stabilization. Based on DFT-optimized structures, a chemical bonding analysis was performed using a local-orbital framework by projection from a plane-wave basis. The resulting bond orders and atomic charges are in good agreement with the expectations based on the structure analysis. SQUID magnetic susceptibility measurements show a high-spin state Fe^II compound with predominantly antiferromagnetic exchange interactions at lower temperatures. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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14 pages, 6281 KiB

Open AccessReview

Metal Complexes of Redox Non-Innocent Ligand N,N′-Bis(3,5-di-tertbutyl-2-hydroxy-phenyl)-1,2-phenylenediamine

by Ari Lehtonen

Molecules 2024, 29(5), 1088; https://doi.org/10.3390/molecules29051088 - 29 Feb 2024

Cited by 1 | Viewed by 1430

Abstract

Redox non-innocent ligands react with metal precursors to form complexes where the oxidation states of the ligand and thus the metal atom cannot be easily defined. A well-known example of such ligands is bis(o-aminophenol) N,N′-bis(3,5-di-tertbutyl-2-hydroxy-phenyl)-1,2-phenylenediamine, previously developed by the Wieghardt group, which has a potentially tetradentate coordination mode and four distinct protonation states, whereas its electrochemical behavior allows for five distinct oxidation states. This rich redox chemistry, as well as the ability to coordinate to various transition metals, has been utilized in the syntheses of metal complexes with M₂L, ML and ML₂ stoichiometries, sometimes supported with other ligands. Different oxidation states of the ligand can adopt different coordination modes. For example, in the fully oxidized form, two N donors are sp²-hybridized, which makes the ligand planar, whereas in the fully reduced form, the sp³-hybridized N donors allow the formation of more flexible chelate structures. In general, the metal can be reduced during complexation, but redox processes of the isolated complexes typically occur on the ligand. Combination of this non-innocent ligand with redox-active transition metals may lead to complexes with interesting magnetic, electrochemical, photonic and catalytic properties. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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40 pages, 14175 KiB

Open AccessReview

Advances for Triangular and Sandwich-Shaped All-Metal Aromatics

by Miaomiao Wang and Yanlan Wang

Molecules 2024, 29(4), 763; https://doi.org/10.3390/molecules29040763 - 7 Feb 2024

Cited by 1 | Viewed by 1496

Abstract

Much experimental work has been contributed to all-metal σ, π and δ-aromaticity among transition metals, semimetallics and other metals in the past two decades. Before our focused investigations on the properties of triangular and sandwich-shaped all-metal aromatics, A. I. Boldyrev presented general discussions on the concepts of all-metal σ-aromaticity and σ-antiaromaticity for metallo-clusters. Schleyer illustrated that Nucleus-Independent Chemical Shifts (NICS) were among the most authoritative criteria for aromaticity. Ugalde discussed the earlier developments of all-metal aromatic compounds with all possible shapes. Besides the theoretical predictions, many stable all-metal aromatic trinuclear clusters have been isolated as the metallic analogues of either the σ-aromatic molecule’s [H₃]⁺ ion or the π-aromatic molecule’s [C₃H₃]⁺ ion. Different from Hoffman’s opinion on all-metal aromaticity, triangular all-metal aromatics were found to hold great potential in applications in coordination chemistry, catalysis, and material science. Triangular all-metal aromatics, which were theoretically proved to conform to the Hückel (4n + 2) rule and possess the smallest aromatic ring, could also play roles as stable ligands during the formation of all-metal sandwiches. The triangular and sandwich-shaped all-metal aromatics have not yet been specifically summarized despite their diversity of existence, puissant developments and various interesting applications. These findings are different from the public opinion that all-metal aromatics would be limited to further applications due to their overstated difficulties in synthesis and uncertain stabilities. Our review will specifically focus on the summarization of theoretical predictions, feasible syntheses and isolations, and multiple applications of triangular and sandwich shaped all-metal aromatics. The appropriateness and necessities of this review will emphasize and disseminate their importance and applications forcefully and in a timely manner. Full article

(This article belongs to the Special Issue Recent Advances in Coordination Chemistry of Metal Complexes)

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