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Crystals, Volume 7, Issue 7 (July 2017)

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Cover Story (view full-size image) In this review, we briefly summarize the history of mesocrystal research. We introduce the current [...] Read more.
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Open AccessArticle Synthesis, Crystal Structures, and Photoluminescent Properties of Two Supramolecular Architectures Based on Difunctional Ligands Containing Imidazolyl and Carboxyl Groups
Crystals 2017, 7(7), 228; https://doi.org/10.3390/cryst7070228
Received: 13 June 2017 / Revised: 21 July 2017 / Accepted: 21 July 2017 / Published: 23 July 2017
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Abstract
Two new supramolecular architectures, namely, [Cd(L1)2(H2O)]n (1) and [Ni(L2)2(H2O)]n (2), were synthesized by the reaction of corresponding metal salts of CdCl2·2.5H2O
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Two new supramolecular architectures, namely, [Cd(L1)2(H2O)]n (1) and [Ni(L2)2(H2O)]n (2), were synthesized by the reaction of corresponding metal salts of CdCl2·2.5H2O and NiCl2·6H2O with 2-(1H-imidazol-4-yl)benzoic acid (HL1) and 3-(1H-imidazol-4-yl)benzoic acid (HL2) respectively, and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and powder X-ray diffraction (PXRD). Both HL1 and HL2 ligands are deprotonated to be L1- and L2- anions that coordinate with Cd(II) and Ni(II) atoms to form two-dimensional (2D) layer structure. Topologically, complex 1 is a 2D network with (4, 4) sql topology, while 2 is a typical 63-hcb topology net. Complex 1 exhibits intense light blue emission in the solid state at room temperature. Full article
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Open AccessCommunication Electrohydrodynamics-Induced Abnormal Electro-Optic Characteristics in a Polymer-Dispersed Liquid Crystal Film
Crystals 2017, 7(7), 227; https://doi.org/10.3390/cryst7070227
Received: 14 June 2017 / Revised: 17 July 2017 / Accepted: 18 July 2017 / Published: 21 July 2017
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Abstract
This study demonstrates for the first time abnormal electro-optic (EO) characteristics induced by electrohydrodynamics (EHD) in a polymer-dispersed liquid crystal (PDLC) film in the presence of a low-frequency (1 kHz) AC voltage. Large LC droplets (20−40 µm) buried in the film can be
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This study demonstrates for the first time abnormal electro-optic (EO) characteristics induced by electrohydrodynamics (EHD) in a polymer-dispersed liquid crystal (PDLC) film in the presence of a low-frequency (1 kHz) AC voltage. Large LC droplets (20−40 µm) buried in the film can be obtained after the illumination of one UV light with a weak intensity (~0.96 mW/cm2) for 12 h. This film exhibits abnormal EO features, including the transmittance’s decay at a high voltage regime at normal incidence and the conversion between polarization independence and polarization dependence for the transmittance-voltage curve at normal and oblique incidences, respectively, of which properties are different from those shown in traditional PDLC films with small droplets. The abnormal EO characteristics of the large-droplet PDLC at the high voltage regime are attributed to a strong scattering effect associated with the formation of the foggy LC droplets in the cell. This effect is induced by a vortex-like LC director field with a rotational axis normal to the cell substrates in each dome-like droplet of the cell at the high voltage regime. The vortex-like director field is induced by a vortex-like turbulence of charged impurity generated by the EHD effect under the action of the AC electric field along the cell normal and the confinement of the dome-like boundary of the droplet on the charged impurities in each droplet. The scattering is decided by the degrees of mismatch between the refractive indices of the LC droplet and polymer, and the local fluctuation of the vortex-like director field in the droplet, resulting in the abnormal EO behaviors of the large-droplet PDLC. This investigation provides novel insight into the EHD effect in three dimensional (3D) microdroplets with anisotropic fluid. Such a large-droplet PDLC has potential in photonic applications, such as electrically controlled polarization-based optical components or optical converters between polarization independence and polarization dependence. Full article
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Open AccessArticle The Role of Halogen Bonding in Controlling Assembly and Organization of Cu(II)-Acac Based Coordination Complexes
Crystals 2017, 7(7), 226; https://doi.org/10.3390/cryst7070226
Received: 23 June 2017 / Revised: 15 July 2017 / Accepted: 17 July 2017 / Published: 20 July 2017
Cited by 6 | PDF Full-text (11531 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
In order to explore the use of non-covalent interactions in the deliberate assembly of metal-supramolecular architectures, a series of β-diketone based ligands capable of simultaneously acting as halogen-bond donors and chelating ligands were synthesized. The three ligands, L1, L2, and L3
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In order to explore the use of non-covalent interactions in the deliberate assembly of metal-supramolecular architectures, a series of β-diketone based ligands capable of simultaneously acting as halogen-bond donors and chelating ligands were synthesized. The three ligands, L1, L2, and L3, carry ethynyl-activated chlorine, bromine, and iodine atoms, respectively and copper(II) complexes of all three ligands were crystallized from different solvents, acetonitrile, ethyl acetate, and nitromethane in order to study specific ligand-solvent interaction. The free ligands L2 and L3, with more polarizable halogen atoms, display C-X⋯O halogen bonds in the solid state, whereas the chloro-analogue (L1) does not engage in halogen bonding. Both acetonitrile and ethyl acetate act as halogen-bond acceptors in Cu(II)-complexes of L2 and L3 whereas nitromethane is present as a ‘space-filling’ guest without participating in any significant intermolecular interactions in Cu(II)-complexes of L2. L3, which is decorated with an iodoethynyl moiety and consistently engages in halogen-bonds with suitable acceptors. This systematic structural analysis allows us to rank the relative importance of a variety of electron-pair donors in these metal complexes. Full article
(This article belongs to the Special Issue Analysis of Halogen and Other σ-Hole Bonds in Crystals)
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Open AccessArticle The Interplay between Various σ- and π-Hole Interactions of Trigonal Boron and Trigonal Pyramidal Arsenic Triiodides
Crystals 2017, 7(7), 225; https://doi.org/10.3390/cryst7070225
Received: 26 June 2017 / Revised: 17 July 2017 / Accepted: 17 July 2017 / Published: 19 July 2017
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Abstract
Boron and arsenic triiodides (BI3 and AsI3, respectively) are similar molecules that differ mainly in their geometries. BI3 is a planar trigonal molecule with D3h symmetry, while AsI3 exhibits a trigonal pyramidal shape with C3v symmetry.
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Boron and arsenic triiodides (BI3 and AsI3, respectively) are similar molecules that differ mainly in their geometries. BI3 is a planar trigonal molecule with D3h symmetry, while AsI3 exhibits a trigonal pyramidal shape with C3v symmetry. Consequently, the As atom of the AsI3 molecule has three σ-holes, whereas the B atom of the BI3 molecule has two symmetrical π-holes. Additionally, there are σ-holes on the iodine atoms in the molecules studied. In the first step, we have studied σ-hole and π-hole interactions in the known monocrystals of BI3 and AsI3. Quantum mechanical calculations have revealed that the crystal packing of BI3 is dominated by π-hole interactions. In the case of AsI3, the overall contribution of dihalogen bonding is comparable to that of pnictogen bonding. Additionally, we have prepared the [Na(THF)6]+[I(AsI3)6](AsI3)2 complex, which can be described as the inverse coordination compound where the iodine anion is the center of the aggregate surrounded by six AsI3 molecules in the close octahedral environment and adjacent two molecules in remote distances. This complex is, besides expected dihalogen and pnictogen bonds, also stabilized by systematically attractive dispersion interactions. Full article
(This article belongs to the Special Issue Analysis of Halogen and Other σ-Hole Bonds in Crystals)
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Open AccessArticle Inorganic Anions Regulate the Phase Transition in Two Organic Cation Salts Containing [(4-Nitroanilinium)(18-crown-6)]+ Supramolecules
Crystals 2017, 7(7), 224; https://doi.org/10.3390/cryst7070224
Received: 28 May 2017 / Revised: 30 June 2017 / Accepted: 6 July 2017 / Published: 15 July 2017
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Abstract
Inorganic Anions Regulate the Phase Transition in Two Organic Cation Salts Containing [(4-Nitroanilinium)(18-crown-6)]+ Supramolecules Full article
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Open AccessReview Structural Aspects of Porphyrins for Functional Materials Applications
Crystals 2017, 7(7), 223; https://doi.org/10.3390/cryst7070223
Received: 19 April 2017 / Revised: 22 June 2017 / Accepted: 12 July 2017 / Published: 15 July 2017
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Abstract
Porphyrinic compounds comprise a diverse group of materials which have in common the presence of one or more cyclic tetrapyrroles known as porphyrins in their molecular structures. The resulting aromaticity gives rise to the semiconducting properties that make these compounds of interest for
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Porphyrinic compounds comprise a diverse group of materials which have in common the presence of one or more cyclic tetrapyrroles known as porphyrins in their molecular structures. The resulting aromaticity gives rise to the semiconducting properties that make these compounds of interest for a broad range of applications, including artificial photosynthesis, catalysis, molecular electronics, sensors, non-linear optics, and solar cells. In this brief review, the crystallographic attributes of porphyrins are emphasized. Examples are given showing how the structural orientations of the porphyrin macrocycle, and the inter-porphyrin covalent bonding present in multiporphyrins influence the semiconducting properties. Beginning with porphine, the simplest porphyrin, we discuss how the more complex structures that have been reported are described by adding peripheral substituents and internal metalation to the macrocycles. We illustrate how the conjugation of the π-bonding, and the presence of electron donor/acceptor pairs, which are the basis for the semiconducting properties, are affected by the crystallographic topology. Full article
(This article belongs to the Special Issue Crystallography of Functional Materials)
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Open AccessArticle σ-Holes on Transition Metal Nanoclusters and Their Influence on the Local Lewis Acidity
Crystals 2017, 7(7), 222; https://doi.org/10.3390/cryst7070222
Received: 10 June 2017 / Revised: 10 July 2017 / Accepted: 11 July 2017 / Published: 14 July 2017
Cited by 4 | PDF Full-text (6211 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
Understanding the molecular interaction behavior of transition metal nanoclusters lies at the heart of their efficient use in, e.g., heterogeneous catalysis, medical therapy and solar energy harvesting. For this purpose, we have evaluated the applicability of the surface electrostatic potential [VS
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Understanding the molecular interaction behavior of transition metal nanoclusters lies at the heart of their efficient use in, e.g., heterogeneous catalysis, medical therapy and solar energy harvesting. For this purpose, we have evaluated the applicability of the surface electrostatic potential [VS(r)] and the local surface electron attachment energy [ES(r)] properties for characterizing the local Lewis acidity of a series of low-energy TM13 transition metal nanoclusters (TM = Au, Cu, Ru, Rh, Pd, Ir, Pt, Co), including also Pt7Cu6. The clusters have been studied using hybrid Kohn–Sham density functional theory (DFT) calculations. The VS(r) and ES(r), evaluated at 0.001 a.u. isodensity contours, are used to analyze the interactions with H2O. We find that the maxima of VS(r), σ-holes, are either localized or diffuse. This is rationalized in terms of the nanocluster geometry and occupation of the clusters’s, p and d valence orbitals. Our findings motivate a new scheme for characterizing σ-holes as σs (diffuse), σp (localized) or σd (localized) depending on their electronic origin. The positions of the maxima in VS(r) (and minima in ES(r)) are found to coincide with O-down adsorption sites of H2O, whereas minima in VS(r) leads to H-down adsorption. Linear relationships between VS,max (and ES,min) and H2O interaction energies are further discussed. Full article
(This article belongs to the Special Issue Analysis of Halogen and Other σ-Hole Bonds in Crystals)
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Open AccessArticle Analysis of Diffracted Intensities from Finite Protein Crystals with Incomplete Unit Cells
Crystals 2017, 7(7), 220; https://doi.org/10.3390/cryst7070220
Received: 31 May 2017 / Revised: 7 July 2017 / Accepted: 8 July 2017 / Published: 14 July 2017
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Abstract
Developments in experimental techniques in micro electron diffraction and serial X-ray crystallography provide the opportunity to collect diffraction data from protein nanocrystals. Incomplete unit cells on the surfaces of protein crystals can affect the distribution of diffracted intensities for crystals with very high
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Developments in experimental techniques in micro electron diffraction and serial X-ray crystallography provide the opportunity to collect diffraction data from protein nanocrystals. Incomplete unit cells on the surfaces of protein crystals can affect the distribution of diffracted intensities for crystals with very high surface-to-volume ratios. The extraction of structure factors from diffraction data for such finite protein crystals sizes is considered here. A theoretical model for the continuous diffracted intensity distribution for data merged from finite crystals with two symmetry-related sub-units of the conventional unit cell is presented. This is used to extend a whole-pattern fitting technique to account for incomplete unit cells in the extraction of structure factor amplitudes. The accuracy of structure factor amplitudes found from this whole-pattern fitting technique and from an integration approach are evaluated. Full article
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Open AccessReview Understanding Mn-Based Intercalation Cathodes from Thermodynamics and Kinetics
Crystals 2017, 7(7), 221; https://doi.org/10.3390/cryst7070221
Received: 24 June 2017 / Revised: 7 July 2017 / Accepted: 11 July 2017 / Published: 13 July 2017
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Abstract
A series of Mn-based intercalation compounds have been applied as the cathode materials of Li-ion batteries, such as LiMn2O4, LiNi1xyCoxMnyO2, etc. With open structures, intercalation compounds exhibit
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A series of Mn-based intercalation compounds have been applied as the cathode materials of Li-ion batteries, such as LiMn2O4, LiNi1xyCoxMnyO2, etc. With open structures, intercalation compounds exhibit a wide variety of thermodynamic and kinetic properties depending on their crystal structures, host chemistries, etc. Understanding these materials from thermodynamic and kinetic points of view can facilitate the exploration of cathodes with better electrochemical performances. This article reviews the current available thermodynamic and kinetic knowledge on Mn-based intercalation compounds, including the thermal stability, structural intrinsic features, involved redox couples, phase transformations as well as the electrical and ionic conductivity. Full article
(This article belongs to the Special Issue Solution-Processed Inorganic Functional Crystals)
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Open AccessReview A Review on Metal Nanoparticles Nucleation and Growth on/in Graphene
Crystals 2017, 7(7), 219; https://doi.org/10.3390/cryst7070219
Received: 8 June 2017 / Revised: 4 July 2017 / Accepted: 11 July 2017 / Published: 13 July 2017
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Abstract
In this review, the fundamental aspects (with particular focus to the microscopic thermodynamics and kinetics mechanisms) concerning the fabrication of graphene-metal nanoparticles composites are discussed. In particular, the attention is devoted to those fabrication methods involving vapor-phase depositions of metals on/in graphene-based materials.
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In this review, the fundamental aspects (with particular focus to the microscopic thermodynamics and kinetics mechanisms) concerning the fabrication of graphene-metal nanoparticles composites are discussed. In particular, the attention is devoted to those fabrication methods involving vapor-phase depositions of metals on/in graphene-based materials. Graphene-metal nanoparticles composites are, nowadays, widely investigated both from a basic scientific and from several technological point of views. In fact, these graphene-based systems present wide-range tunable and functional electrical, optical, and mechanical properties which can be exploited for the design and production of innovative and high-efficiency devices. This research field is, so, a wide and multidisciplinary section in the nanotechnology field of study. So, this review aims to discuss, in a synthetic and systematic framework, the basic microscopic mechanisms and processes involved in metal nanoparticles formation on graphene sheets by physical vapor deposition methods and on their evolution by post-deposition processes. This is made by putting at the basis of the discussions some specific examples to draw insights on the common general physical and chemical properties and parameters involved in the synergistic interaction processes between graphene and metals. Full article
(This article belongs to the Special Issue Integration of 2D Materials for Electronics Applications)
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Open AccessArticle Crystal Structure of 17α-Dihydroequilin, C18H22O2, from Synchrotron Powder Diffraction Data and Density Functional Theory
Crystals 2017, 7(7), 218; https://doi.org/10.3390/cryst7070218
Received: 9 April 2017 / Revised: 4 June 2017 / Accepted: 22 June 2017 / Published: 13 July 2017
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Abstract
The crystal structure of 17α-dihydroequilin has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. 17α-dihydroequilin crystallizes in space group P212121 (#19) with a = 6.76849(1) Å, b = 8.96849(1) Å,
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The crystal structure of 17α-dihydroequilin has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. 17α-dihydroequilin crystallizes in space group P212121 (#19) with a = 6.76849(1) Å, b = 8.96849(1) Å, c = 23.39031(5) Å, V = 1419.915(3) Å3, and Z = 4. Both hydroxyl groups form hydrogen bonds to each other, resulting in zig-zag chains along the b-axis. The powder diffraction pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ as the entry 00-066-1608. Full article
(This article belongs to the Special Issue Structural Analysis of Crystalline Materials from Powders)
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Open AccessArticle Synthesis, Crystal Structures, and Properties of a New Supramolecular Polymer Based on Mixed Imidazole and Carboxylate Ligands
Crystals 2017, 7(7), 210; https://doi.org/10.3390/cryst7070210
Received: 5 June 2017 / Revised: 1 July 2017 / Accepted: 2 July 2017 / Published: 13 July 2017
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Abstract
One new coordination polymer, namely, [Cd3(H2L)3(Pza)2(H2O)2]n (1) was synthesized by the reaction of Cd(NO3)2·4H2O with 1,4-di(1H-imidazol-4-yl)benzene (H2L) and
[...] Read more.
One new coordination polymer, namely, [Cd3(H2L)3(Pza)2(H2O)2]n (1) was synthesized by the reaction of Cd(NO3)2·4H2O with 1,4-di(1H-imidazol-4-yl)benzene (H2L) and 3,5-pyrazoledicarboxylic acid (H3pza) and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis, and powder X-ray diffraction (PXRD). The H3pza ligand was completely deprotonated to pza3−, which bridged the Cd2+ to form one-dimensional (1D) chain. The adjacent 1D chains were further linked into the two-dimensional (2D) layer by the linear H2L ligands. The weak interaction, including hydrogen bonds and π−π stacking interactions, extends the 2D layers into three-dimensional (3D) supramolecular polymer. Complex 1 shows intense light blue emission in the solid state at room temperature. Full article
(This article belongs to the Section Crystal Engineering)
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Open AccessArticle Syntheses, Crystal Structures and Thermal Behaviors of Two Supramolecular Salamo-Type Cobalt(II) and Zinc(II) Complexes
Crystals 2017, 7(7), 217; https://doi.org/10.3390/cryst7070217
Received: 4 June 2017 / Revised: 3 July 2017 / Accepted: 5 July 2017 / Published: 12 July 2017
Cited by 14 | PDF Full-text (2429 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
This paper reports the syntheses of two new complexes, [Co(L1)(H2O)2] (1) and [{Zn(L2)(μ-OAc)Zn(n-PrOH)}2] (2), from asymmetric halogen-substituted Salamo-type ligands H2L1 and H3L
[...] Read more.
This paper reports the syntheses of two new complexes, [Co(L1)(H2O)2] (1) and [{Zn(L2)(μ-OAc)Zn(n-PrOH)}2] (2), from asymmetric halogen-substituted Salamo-type ligands H2L1 and H3L2, respectively. Investigation of the crystal structure of complex 1 reveals that the complex includes one Co(II) ion, one (L1)2− unit and two coordinated water molecules. Complex 1 shows slightly distorted octahedral coordination geometry, forming an infinite 2D supramolecular structure by intermolecular hydrogen bond and π–π stacking interactions. Complex 2 contains four Zn(II)ions, two completely deprotonated (L2)3− moieties, two coordinated μ-OAc ions and n-propanol molecules. The Zn(II) ions in complex 2 display slightly distorted trigonal bipyramidal or square pyramidal geometries. Full article
(This article belongs to the Section Interactions in Crystal Structures)
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Open AccessArticle σ-Hole Interactions: Perspectives and Misconceptions
Crystals 2017, 7(7), 212; https://doi.org/10.3390/cryst7070212
Received: 4 June 2017 / Revised: 21 June 2017 / Accepted: 22 June 2017 / Published: 12 July 2017
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Abstract
After a brief discussion of the σ-hole concept and the significance of molecular electrostatic potentials in noncovalent interactions, we draw attention to some common misconceptions that are encountered in that context: (1) Since the electrostatic potential reflects the contributions of both the nuclei
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After a brief discussion of the σ-hole concept and the significance of molecular electrostatic potentials in noncovalent interactions, we draw attention to some common misconceptions that are encountered in that context: (1) Since the electrostatic potential reflects the contributions of both the nuclei and the electrons, it cannot be assumed that negative potentials correspond to “electron-rich” regions and positive potentials to “electron-poor” ones; (2) The electrostatic potential in a given region is determined not only by the electrons and nuclei in that region, but also by those in other portions of the molecule, especially neighboring ones; (3) A σ-hole is a region of lower electronic density on the extension of a covalent bond, not an electrostatic potential; (4) Noncovalent interactions are between positive and negative regions, which are not necessarily associated with specific atoms, so that “close contacts” between atoms do not always indicate the actual interactions. Full article
(This article belongs to the Special Issue Analysis of Halogen and Other σ-Hole Bonds in Crystals)
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Open AccessReview Advanced Scanning Probe Microscopy of Graphene and Other 2D Materials
Crystals 2017, 7(7), 216; https://doi.org/10.3390/cryst7070216
Received: 17 May 2017 / Revised: 3 July 2017 / Accepted: 7 July 2017 / Published: 11 July 2017
Cited by 1 | PDF Full-text (1669 KB) | HTML Full-text | XML Full-text
Abstract
Two-dimensional (2D) materials, such as graphene and metal dichalcogenides, are an emerging class of materials, which hold the promise to enable next-generation electronics. Features such as average flake size, shape, concentration, and density of defects are among the most significant properties affecting these
[...] Read more.
Two-dimensional (2D) materials, such as graphene and metal dichalcogenides, are an emerging class of materials, which hold the promise to enable next-generation electronics. Features such as average flake size, shape, concentration, and density of defects are among the most significant properties affecting these materials’ functions. Because of the nanoscopic nature of these features, a tool performing morphological and functional characterization on this scale is required. Scanning Probe Microscopy (SPM) techniques offer the possibility to correlate morphology and structure with other significant properties, such as opto-electronic and mechanical properties, in a multilevel characterization at atomic- and nanoscale. This review gives an overview of the different SPM techniques used for the characterization of 2D materials. A basic introduction of the working principles of these methods is provided along with some of the most significant examples reported in the literature. Particular attention is given to those techniques where the scanning probe is not used as a simple imaging tool, but rather as a force sensor with very high sensitivity and resolution. Full article
(This article belongs to the Special Issue Integration of 2D Materials for Electronics Applications)
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