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Inorganics
Special Issues
Innovative Inorganic Synthesis
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Innovative Inorganic Synthesis

A special issue of Inorganics (ISSN 2304-6740).

Deadline for manuscript submissions: closed (15 November 2013) | Viewed by 86528

Printed Edition Available!
A printed edition of this Special Issue is available here.

Special Issue Editor

Prof. Dr. Duncan H. Gregory

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Guest Editor
School of Chemistry, University of Glasgow, University Avenue, Glasgow G12 8QQ, UK
Interests: nitrides; chalcogenides; carbides; hydrides; synthesis; structure; solid-state chemistry; materials chemistry
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear colleagues,

The synthesis of inorganic compounds embraces an immense range of techniques and approaches. New organometallic molecules, for example, might demand multi-step organic reactions in the successful production of ligands followed by precision handling and manipulation to form the desired complexes under anaerobic conditions. By contrast, preparation of solid state compounds can demand extreme conditions of temperature and pressure to overcome the formidable thermodynamic and kinetic barriers to their formation. It is the target of many inorganic chemists, both by experiment and computation, to prepare or predict new compounds and materials, to discover the most appropriate conditions under which such substances can be made and to design the experiments that will realise them. New inorganic compounds remain attractive, for example, for their inherent complexity and beauty, for their chemical behaviour, their chemical or biological activity or for their physical properties.

The need and desire for new compounds often demands increasingly sophisticated and imaginative synthesis strategies. Equally, the modern societal pressures of cost, safety and environmental protection require new attitudes to the synthesis of high value chemical products. Time and energy efficiency, use of earth-abundant resources and many other green chemistry principles become key parameters in the design of new synthetic processes. I would like to dedicate this inaugural issue of “Inorganics” therefore, to the concept of “innovative synthesis” – from the intricacy of constructing extended molecular solids on the basis of weak supramolecular forces through the appealing simplicity of “one-pot” methods to make cluster and hybrid materials and soft chemical means to produce solid state materials to the adaptation of inefficient lab techniques towards streamlined flow processes for the preparation of fine chemicals. This special issue invites contributions in all of the above areas and beyond; the primary requisite being the application of creative approaches to achieve synthetic goals.

Prof. Duncan H. Gregory
Guest Editor.

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Published Papers (10 papers)

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Editorial

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172 KiB  
Editorial
Innovative Inorganic Synthesis
by Duncan H. Gregory
Inorganics 2014, 2(4), 552-555; https://doi.org/10.3390/inorganics2040552 - 17 Oct 2014
Cited by 1 | Viewed by 4934
Abstract
I am delighted to introduce this Special Issue of Inorganics; the first themed issue of the journal and one dedicated to Innovative Inorganic Synthesis. [...] Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis)

Research

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2197 KiB  
Article
Long Alkyl Chain Organophosphorus Coupling Agents for in Situ Surface Functionalization by Reactive Milling
by Annika Betke and Guido Kickelbick
Inorganics 2014, 2(3), 410-423; https://doi.org/10.3390/inorganics2030410 - 4 Aug 2014
Cited by 18 | Viewed by 7032
Abstract
Innovative synthetic approaches should be simple and environmentally friendly. Here, we present the surface modification of inorganic submicrometer particles with long alkyl chain organophosphorus coupling agents without the need of a solvent, which makes the technique environmentally friendly. In addition, it is of [...] Read more.
Innovative synthetic approaches should be simple and environmentally friendly. Here, we present the surface modification of inorganic submicrometer particles with long alkyl chain organophosphorus coupling agents without the need of a solvent, which makes the technique environmentally friendly. In addition, it is of great benefit to realize two goals in one step: size reduction and, simultaneously, surface functionalization. A top-down approach for the synthesis of metal oxide particles with in situ surface functionalization is used to modify titania with long alkyl chain organophosphorus coupling agents. A high energy planetary ball mill was used to perform reactive milling using titania as inorganic pigment and long alkyl chain organophosphorus coupling agents like dodecyl and octadecyl phosphonic acid. The final products were characterized by IR, NMR and X-ray fluorescence spectroscopy, thermal and elemental analysis as well as by X-ray powder diffraction and scanning electron microscopy. The process entailed a tribochemical phase transformation from the starting material anatase to a high-pressure modification of titania and the thermodynamically more stable rutile depending on the process parameters. Furthermore, the particles show sizes between 100 nm and 300 nm and a degree of surface coverage up to 0.8 mmol phosphonate per gram. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis)
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3489 KiB  
Article
Supercritical Fluid Synthesis of LiCoPO4 Nanoparticles and Their Application to Lithium Ion Battery
by Murukanahally Kempaiah Devaraju, Quang Duc Truong, Hiroshi Hyodo, Takaaki Tomai and Itaru Honma
Inorganics 2014, 2(2), 233-247; https://doi.org/10.3390/inorganics2020233 - 28 May 2014
Cited by 11 | Viewed by 8155
Abstract
In this work, LiCoPO4 nanoparticles were synthesized by supercritical fluid method using cobalt nitrate hexahydrate (Co(NO3)2 6H2O) and cobalt acetate tetrahydrate (C4H6CoO4 4H2O) as starting materials. The effect of starting [...] Read more.
In this work, LiCoPO4 nanoparticles were synthesized by supercritical fluid method using cobalt nitrate hexahydrate (Co(NO3)2 6H2O) and cobalt acetate tetrahydrate (C4H6CoO4 4H2O) as starting materials. The effect of starting materials on particle morphology, size, and the crystalline phase were investigated. The as-synthesized samples were systematically characterized by XRD, TEM, STEM, EDS, BET, and TG and charge-discharge measurements. In addition, Rietveld refinement analysis was performed. The electrochemical measurements of LiCoPO4 nanoparticles have shown differences in capacities depending on the starting materials used in the synthesis and the results have been discussed in this paper. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis)
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1033 KiB  
Article
Bottom-Up, Wet Chemical Technique for the Continuous Synthesis of Inorganic Nanoparticles
by Annika Betke and Guido Kickelbick
Inorganics 2014, 2(1), 1-15; https://doi.org/10.3390/inorganics2010001 - 27 Jan 2014
Cited by 37 | Viewed by 10488
Abstract
Continuous wet chemical approaches for the production of inorganic nanoparticles are important for large scale production of nanoparticles. Here we describe a bottom-up, wet chemical method applying a microjet reactor. This technique allows the separation between nucleation and growth in a continuous reactor [...] Read more.
Continuous wet chemical approaches for the production of inorganic nanoparticles are important for large scale production of nanoparticles. Here we describe a bottom-up, wet chemical method applying a microjet reactor. This technique allows the separation between nucleation and growth in a continuous reactor environment. Zinc oxide (ZnO), magnetite (Fe3O4), as well as brushite (CaHPO4·2H2O), particles with a small particle size distribution can be obtained continuously by using the rapid mixing of two precursor solutions and the fast removal of the nuclei from the reaction environment. The final particles were characterized by FT-IR, TGA, DLS, XRD and SEM techniques. Systematic studies on the influence of the different process parameters, such as flow rate and process temperature, show that the particle size can be influenced. Zinc oxide was obtained with particle sizes between 44 nm and 102 nm. The obtained magnetite particles have particle sizes in the range of 46 nm to 132 nm. Brushite behaves differently; the obtained particles were shaped like small plates with edge lengths between 100 nm and 500 nm. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis)
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1018 KiB  
Article
Synthesis of Diazonium Tetrachloroaurate(III) Precursors for Surface Grafting
by Sabine N. Neal, Samuel A. Orefuwa, Atiya T. Overton, Richard J. Staples and Ahmed A. Mohamed
Inorganics 2013, 1(1), 70-84; https://doi.org/10.3390/inorganics1010070 - 17 Dec 2013
Cited by 14 | Viewed by 8716
Abstract
The synthesis of diazonium tetrachloroaurate(III) complexes [R-4-C6H4N≡N]AuCl4 involves protonation of anilines CN-4-C6H4NH2, C8F17-4-C6H4NH2, and C6H13-4-C6H4 [...] Read more.
The synthesis of diazonium tetrachloroaurate(III) complexes [R-4-C6H4N≡N]AuCl4 involves protonation of anilines CN-4-C6H4NH2, C8F17-4-C6H4NH2, and C6H13-4-C6H4NH2 with tetrachloroauric acid H[AuCl4] 3H2O in acetonitrile followed by one-electron oxidation using [NO]PF6. FT-IR shows the diazonium stretching frequency at 2277 cm−1 (CN), 2305 cm−1 (C8F17), and 2253 cm−1 (C6H13). Thermogravimetric Analysis (TGA) shows the high stabilities of the electron-withdrawing substituents C8F17 and CN compared with the electron-donating substituent C6H13. Residual Gas Analysis (RGA) shows the release of molecular nitrogen as the main gas residue among other small molecular weight chlorinated hydrocarbons and chlorobenzene. Temperature-Dependent X-Ray Powder Diffraction (TD-XRD) shows the thermal decomposition in C6H13 diffraction patterns at low temperature of 80 °C which supports the TGA and RGA (TGA-MS) conclusions. X-ray structure shows N≡N bond distance of approximately 1.10 Å and N≡N-C bond angle of 178°. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis)
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2258 KiB  
Article
Synthesis and Characterisation of Lanthanide N-Trimethylsilyl and -Mesityl Functionalised Bis(iminophosphorano)methanides and -Methanediides
by George Marshall, Ashley J. Wooles, David P. Mills, William Lewis, Alexander J. Blake and Stephen T. Liddle
Inorganics 2013, 1(1), 46-69; https://doi.org/10.3390/inorganics1010046 - 12 Dec 2013
Cited by 19 | Viewed by 6972
Abstract
We report the extension of the series of {BIPMTMSH}− (BIPMR = C{PPh2NR}2, TMS = trimethylsilyl) derived rare earth methanides by the preparation of [Ln(BIPMTMSH)(I)2(THF)] (Ln = Nd, Gd, Tb), 1a–c, [...] Read more.
We report the extension of the series of {BIPMTMSH}− (BIPMR = C{PPh2NR}2, TMS = trimethylsilyl) derived rare earth methanides by the preparation of [Ln(BIPMTMSH)(I)2(THF)] (Ln = Nd, Gd, Tb), 1a–c, in 34–50% crystalline yields via the reaction of [Ln(I)3(THF)3.5] with [Cs(BIPMTMSH)]. Similarly, we have extended the range of {BIPMMesH}− (Mes = 2,4,6-trimethylphenyl) derived rare earth methanides with the preparation of [Gd(BIPMMesH)(I)2(THF)2], 3, (49%) and [Yb(BIPMMesH)(I)2(THF)], 4, (26%), via the reaction of [Ln(I)3(THF)3.5] with [{K(BIPMMesH)}2]. Attempts to prepare dysprosium and erbium analogues of 3 or 4 were not successful, with the ion pair species [Ln(BIPMMesH)2][BIPMMesH] (Ln = Dy, Er), 5a–b, isolated in 31–39% yield. The TMEDA (N',N',N",N"-tetramethylethylenediamine) adducts [Ln(BIPMMesH)(I)2(TMEDA)] (Ln = La, Gd), 6a–b, were prepared in quantitative yield via the dissolution of [La(BIPMMesH)(I)2(THF)] or 3 in a TMEDA/THF solution. The reactions of [Ln(BIPMMesH)(I)2(THF)] [Ln = La, Ce, Pr, and Gd (3)] or 6a–b with a selection of bases did not afford [La(BIPMMes)(I)(S)n] (S = solvent) as predicted, but instead led to the isolation of the heteroleptic complexes [Ln(BIPMMes)(BIPMMesH)] (Ln = La, Ce, Pr and Gd), 7a–d, in low yields due to ligand scrambling. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis)
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1420 KiB  
Article
Facile and Selective Synthetic Approach for Ruthenium Complexes Utilizing a Molecular Sieve Effect in the Supporting Ligand
by Dai Oyama, Ayumi Fukuda, Takashi Yamanaka and Tsugiko Takase
Inorganics 2013, 1(1), 32-45; https://doi.org/10.3390/inorganics1010032 - 9 Dec 2013
Cited by 6 | Viewed by 6969
Abstract
It is extremely important for synthetic chemists to control the structure of new compounds. We have constructed ruthenium-based mononuclear complexes with the tridentate 2,6-di(1,8-naphthyridin-2-yl)pyridine (dnp) ligand to investigate a new synthetic approach using a specific coordination space. The synthesis of a family of [...] Read more.
It is extremely important for synthetic chemists to control the structure of new compounds. We have constructed ruthenium-based mononuclear complexes with the tridentate 2,6-di(1,8-naphthyridin-2-yl)pyridine (dnp) ligand to investigate a new synthetic approach using a specific coordination space. The synthesis of a family of new ruthenium complexes containing both the dnp and triphenylphosphine (PPh3) ligands, [Ru(dnp)(PPh3)(X)(L)]n+ (X = PPh3, NO2−, Cl−, Br−; L = OH2, CH3CN, C6H5CN, SCN−), has been described. All complexes have been spectroscopically characterized in solution, and the nitrile complexes have also been characterized in the solid state through single-crystal X-ray diffraction analysis. Dnp in the present complex system behaves like a “molecular sieve” in ligand replacement reactions. Both experimental data and density functional theory (DFT) calculations suggest that dnp plays a crucial role in the selectivity observed in this study. The results provide useful information toward elucidating this facile and selective synthetic approach to new transition metal complexes. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis)
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Review

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3545 KiB  
Review
Direct Energy Supply to the Reaction Mixture during Microwave-Assisted Hydrothermal and Combustion Synthesis of Inorganic Materials
by Roberto Rosa, Chiara Ponzoni and Cristina Leonelli
Inorganics 2014, 2(2), 191-210; https://doi.org/10.3390/inorganics2020191 - 5 May 2014
Cited by 27 | Viewed by 9108
Abstract
The use of microwaves to perform inorganic synthesis allows the direct transfer of electromagnetic energy inside the reaction mixture, independently of the temperature manifested therein. The conversion of microwave (MW) radiation into heat is useful in overcoming the activation energy barriers associated with [...] Read more.
The use of microwaves to perform inorganic synthesis allows the direct transfer of electromagnetic energy inside the reaction mixture, independently of the temperature manifested therein. The conversion of microwave (MW) radiation into heat is useful in overcoming the activation energy barriers associated with chemical transformations, but the use of microwaves can be further extended to higher temperatures, thus creating unusual high-energy environments. In devising synthetic methodologies to engineered nanomaterials, hydrothermal synthesis and solution combustion synthesis can be used as reference systems to illustrate effects related to microwave irradiation. In the first case, energy is transferred to the entire reaction volume, causing a homogeneous temperature rise within a closed vessel in a few minutes, hence assuring uniform crystal growth at the nanometer scale. In the second case, strong exothermic combustion syntheses can benefit from the application of microwaves to convey energy to the reaction not only during the ignition step, but also while it is occurring and even after its completion. In both approaches, however, the direct interaction of microwaves with the reaction mixture can lead to practically gradient-less heating profiles, on the basis of which the main observed characteristics and properties of the aforementioned reactions and products can be explained. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis)
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580 KiB  
Review
Syntheses of Macromolecular Ruthenium Compounds: A New Approach for the Search of Anticancer Drugs
by Andreia Valente and M. Helena Garcia
Inorganics 2014, 2(1), 96-114; https://doi.org/10.3390/inorganics2010096 - 21 Mar 2014
Cited by 22 | Viewed by 7986
Abstract
The continuous rising of the cancer patient death rate undoubtedly shows the pressure to find more potent and efficient drugs than those in clinical use. These agents only treat a narrow range of cancer conditions with limited success and are associated with serious [...] Read more.
The continuous rising of the cancer patient death rate undoubtedly shows the pressure to find more potent and efficient drugs than those in clinical use. These agents only treat a narrow range of cancer conditions with limited success and are associated with serious side effects caused by the lack of selectivity. In this frame, innovative syntheses approaches can decisively contribute to the success of “smart compounds” that might be only selective and/or active towards the cancer cells, sparing the healthy ones. In this scope, ruthenium chemistry is a rising field for the search of proficient metallodrugs by the use of macromolecular ruthenium complexes (dendrimers and dendronized polymers, coordination-cage and protein conjugates, nanoparticles and polymer-“ruthenium-cyclopentadienyl” conjugates) that can take advantage of the singularities of tumor cells (vs. healthy cells). Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis)
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1825 KiB  
Review
Chemistry of Ammonothermal Synthesis
by Theresia M. M. Richter and Rainer Niewa
Inorganics 2014, 2(1), 29-78; https://doi.org/10.3390/inorganics2010029 - 28 Feb 2014
Cited by 112 | Viewed by 12551
Abstract
Ammonothermal synthesis is a method for synthesis and crystal growth suitable for a large range of chemically different materials, such as nitrides (e.g., GaN, AlN), amides (e.g., LiNH2, Zn(NH2)2), imides (e.g., Th(NH)2), ammoniates (e.g., Ga(NH [...] Read more.
Ammonothermal synthesis is a method for synthesis and crystal growth suitable for a large range of chemically different materials, such as nitrides (e.g., GaN, AlN), amides (e.g., LiNH2, Zn(NH2)2), imides (e.g., Th(NH)2), ammoniates (e.g., Ga(NH3)3F3, [Al(NH3)6]I3 · NH3) and non-nitrogen compounds like hydroxides, hydrogen sulfides and polychalcogenides (e.g., NaOH, LiHS, CaS, Cs2Te5). In particular, large scale production of high quality crystals is possible, due to comparatively simple scalability of the experimental set-up. The ammonothermal method is defined as employing a heterogeneous reaction in ammonia as one homogenous fluid close to or in supercritical state. Three types of milieus may be applied during ammonothermal synthesis: ammonobasic, ammononeutral or ammonoacidic, evoked by the used starting materials and mineralizers, strongly influencing the obtained products. There is little known about the dissolution and materials transport processes or the deposition mechanisms during ammonothermal crystal growth. However, the initial results indicate the possible nature of different intermediate species present in the respective milieus. Full article
(This article belongs to the Special Issue Innovative Inorganic Synthesis)
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