This article is an open access article distributed under the terms and conditions of the Creative... more This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY
New very fast and efficient detectors, installed both on laboratory instruments and synchrotron f... more New very fast and efficient detectors, installed both on laboratory instruments and synchrotron facilities, allow the monitoring of solid-state reactions from subsecond to minute scales with the production of large amounts of data. Traditional “one-by-one” pattern refinement needs complementary approaches, useful to handle hundreds to thousands of X-ray patterns. Principal-component analysis (PCA) has been applied to these fields in the last few years to speed up analysis with the specific goals of assessing data quality, identifying patterns where a reaction occurs, and extracting the kinetics. PCA is applied to the adsorption/desorption of Xe and CO2 within a Y zeolite. CO2 sequestration is a key issue in relation to climate change, while Xe is a critical raw material, and its purification is an important topic for the industry. At first, results were compared to traditional sequential Rietveld refinement. CO2-Y data were also compared with in situ single crystal data to investiga...
Low-ordered carbon/layered double hydroxide (LDH) nanocomposites were prepared by rehydration of ... more Low-ordered carbon/layered double hydroxide (LDH) nanocomposites were prepared by rehydration of the oxides produced by calcination of an organic LDH. While the memory effect is a widely recognized effect on oxides produced by inorganic LDH, it is unprecedented from the calcination/rehydration of organic ones. Different temperatures (400, 600, and 1100 °C) were tested on the basis of thermogravimetric data. Water, instead of a carbonate solution, was used for the rehydration, with CO2 available from water itself and/or air to induce a slower process with an easier and better intercalation of the carbonaceous species. The samples were characterized by X-ray powder diffraction (XRPD), infrared in reflection mode (IR), and Raman spectroscopies and scanning electron microscopy (SEM). XRPD indicated the presence of carbonate LDH, and of residuals of unreacted oxides. IR confirmed that the prevailing anion is carbonate, coming from the water used for the rehydration and/or air. Raman data...
Composite lightweight materials for X-ray shielding applications were studied and developed with ... more Composite lightweight materials for X-ray shielding applications were studied and developed with the goal of replacing traditional screens made of lead and steel, with innovative materials with similar shielding properties, but lighter, more easily formed and workable, with lower impact on the environment and reduced toxicity for human health. New epoxy based composites additivated with barium sulfate and bismuth oxide were designed through simulations performed with softwares based on Geant4. Then, they were prepared and characterized using different techniques starting from digital radiography in order to test the radiopacity of the composites, in comparison with traditional materials. The lower environmental impact and toxicity of these innovative screens were quantified by Life Cycle Assessment (LCA) calculation based on the ecoinvent database, within the openLCA framework. Optimized mixtures are (i) 20% epoxy/60% bismuth oxide/20% barite, which guarantees the best performance i...
The title compound bis(2-phenylpyridine-C,N’)-bis(acetonitrile)iridium(III)hexafluorophosphate, a... more The title compound bis(2-phenylpyridine-C,N’)-bis(acetonitrile)iridium(III)hexafluorophosphate, a six-coordinate iridium(III) complex, crystallizes in the P-1 space group. Iridium is in a distorted octahedral (n = 6) coordination with the N,C’ atoms of two phenylpyridine and the N atoms of two acetonitrile ligands. The peculiarity of this structure is that three independent moieties of the title compound and three PF6− anions, to counterbalance the charge, are observed in the asymmetric unit and this is a rather uncommon fact among the Cambridge Crystallographic Database (CSD) entries. The three couples are almost identical conformers with very similar torsional angles. The packing, symmetry, and space group were accurately analyzed and described also by means of Hirshfeld surface analysis, which is able to underline subtle differences among the three anion/cation couples in the asymmetric unit. The driving force of the packing is the clustering of the aromatic rings and the maximiz...
Layered double hydroxides (LDHs) are nanomaterials with interesting properties finding applicatio... more Layered double hydroxides (LDHs) are nanomaterials with interesting properties finding applications in many fields, such as catalysis, environmental chemistry, and pharmaceuticals. They are anionic clays with positively charged layers and anions within the layers to reach neutrality. Their properties are defined by both composition and morphology. The composition can be tuned by exchanging the interlayer anion. The far more stable, common, and highly prevalent among natural LDHs is the carbonate anion thanks to its double negative charge. To adapt the properties of LDHs for technological applications, the challenge is to exchange the carbonate with the functionalizing monovalent anions in an effective and cheap way. In this study, the exchange of carbonate with nitrate ions is studied by in situ X-ray powder diffraction (XRPD). The exchange is carried out by a liquid-assisted grinding approach, inserting the mechanically ground dry sample in a capillary and then wetting it with a dr...
Acta Crystallographica Section A Foundations and Advances
The increasing efficiency of detectors and brightness of X-rays in both laboratory and large-scal... more The increasing efficiency of detectors and brightness of X-rays in both laboratory and large-scale facilities allow the collection of full single-crystal X-ray data sets within minutes. The analysis of these `crystallographic big data' requires new tools and approaches. To answer these needs, the use of principal component analysis (PCA) is proposed to improve the efficiency and speed of the analysis. Potentialities and limitations of PCA were investigated using single-crystal X-ray diffraction (XRD) data collected in situ on Y zeolite, in which CO2, acting as an active species, is thermally adsorbed while cooling from 300 to 200 K. For the first time, thanks to the high sensitivity of single-crystal XRD, it was possible to determine the sites where CO2 is adsorbed, the increase in their occupancy while the temperature is decreased, and the correlated motion of active species, i.e. CO2, H2O and Na+. PCA allowed identification and elimination of problematic data sets, and better ...
A graphene-containing LDH was prepared by re-hydration of the oxides produced by the calcination ... more A graphene-containing LDH was prepared by re-hydration of the oxides produced by the calcination of an organic LDH. While the memory effect is a widely recognized effect on oxides produced by inorganic LDHs, it is unprecedented from the calcination/re-hydration of organic ones. Different temperatures (400, 600 and 1100 °C) were tested, on the basis of thermogravimetric data. Water instead of a carbonate solution was used for the re-hydration, with CO2 available from water itself and/or air to induce a slower process with an easier and better intercalation of the carbonaceous species within the layers. The samples were characterized by X-ray Powder Diffraction (XRPD), IR and Raman spectroscopy and scanning electron microscopy (SEM). XRPD indicate the presence of carbonate LDH mixed with a layered phase with a larger d-spacing. IR confirmed that the prevailing anion is carbonate, coming from the water used for the re-hydration and/or air. Raman data indicated the presence of low-o...
Zeitschrift für Kristallographie - Crystalline Materials, 2017
The crystal structure of sodium naphthalene 2-sulfonate (Na2-NS) is reported. This compound raise... more The crystal structure of sodium naphthalene 2-sulfonate (Na2-NS) is reported. This compound raised the attention as a pollutant, being widely used in industry, and its intercalation in inorganic matrices, such as layered double hydroxides (LDH), could be a suitable removal strategy. The crystal structure of the title compound, despite its simplicity, is not known in the literature, so we looked for a strategy to grow crystals suitable for a single crystal study. Although many attempts were made to recrystallize it, Na2-NS grows in bunches of very thin laminae, with a high degree of mosaicity and intergrowth, explaining the absence of a reported crystal structure. The crystal structure shows layers of Na
PCA, coupled to molecular descriptors, proved to be an effective tool to rationalize the mechanoc... more PCA, coupled to molecular descriptors, proved to be an effective tool to rationalize the mechanochemical intercalation yields of layered materials.
This article is an open access article distributed under the terms and conditions of the Creative... more This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY
New very fast and efficient detectors, installed both on laboratory instruments and synchrotron f... more New very fast and efficient detectors, installed both on laboratory instruments and synchrotron facilities, allow the monitoring of solid-state reactions from subsecond to minute scales with the production of large amounts of data. Traditional “one-by-one” pattern refinement needs complementary approaches, useful to handle hundreds to thousands of X-ray patterns. Principal-component analysis (PCA) has been applied to these fields in the last few years to speed up analysis with the specific goals of assessing data quality, identifying patterns where a reaction occurs, and extracting the kinetics. PCA is applied to the adsorption/desorption of Xe and CO2 within a Y zeolite. CO2 sequestration is a key issue in relation to climate change, while Xe is a critical raw material, and its purification is an important topic for the industry. At first, results were compared to traditional sequential Rietveld refinement. CO2-Y data were also compared with in situ single crystal data to investiga...
Low-ordered carbon/layered double hydroxide (LDH) nanocomposites were prepared by rehydration of ... more Low-ordered carbon/layered double hydroxide (LDH) nanocomposites were prepared by rehydration of the oxides produced by calcination of an organic LDH. While the memory effect is a widely recognized effect on oxides produced by inorganic LDH, it is unprecedented from the calcination/rehydration of organic ones. Different temperatures (400, 600, and 1100 °C) were tested on the basis of thermogravimetric data. Water, instead of a carbonate solution, was used for the rehydration, with CO2 available from water itself and/or air to induce a slower process with an easier and better intercalation of the carbonaceous species. The samples were characterized by X-ray powder diffraction (XRPD), infrared in reflection mode (IR), and Raman spectroscopies and scanning electron microscopy (SEM). XRPD indicated the presence of carbonate LDH, and of residuals of unreacted oxides. IR confirmed that the prevailing anion is carbonate, coming from the water used for the rehydration and/or air. Raman data...
Composite lightweight materials for X-ray shielding applications were studied and developed with ... more Composite lightweight materials for X-ray shielding applications were studied and developed with the goal of replacing traditional screens made of lead and steel, with innovative materials with similar shielding properties, but lighter, more easily formed and workable, with lower impact on the environment and reduced toxicity for human health. New epoxy based composites additivated with barium sulfate and bismuth oxide were designed through simulations performed with softwares based on Geant4. Then, they were prepared and characterized using different techniques starting from digital radiography in order to test the radiopacity of the composites, in comparison with traditional materials. The lower environmental impact and toxicity of these innovative screens were quantified by Life Cycle Assessment (LCA) calculation based on the ecoinvent database, within the openLCA framework. Optimized mixtures are (i) 20% epoxy/60% bismuth oxide/20% barite, which guarantees the best performance i...
The title compound bis(2-phenylpyridine-C,N’)-bis(acetonitrile)iridium(III)hexafluorophosphate, a... more The title compound bis(2-phenylpyridine-C,N’)-bis(acetonitrile)iridium(III)hexafluorophosphate, a six-coordinate iridium(III) complex, crystallizes in the P-1 space group. Iridium is in a distorted octahedral (n = 6) coordination with the N,C’ atoms of two phenylpyridine and the N atoms of two acetonitrile ligands. The peculiarity of this structure is that three independent moieties of the title compound and three PF6− anions, to counterbalance the charge, are observed in the asymmetric unit and this is a rather uncommon fact among the Cambridge Crystallographic Database (CSD) entries. The three couples are almost identical conformers with very similar torsional angles. The packing, symmetry, and space group were accurately analyzed and described also by means of Hirshfeld surface analysis, which is able to underline subtle differences among the three anion/cation couples in the asymmetric unit. The driving force of the packing is the clustering of the aromatic rings and the maximiz...
Layered double hydroxides (LDHs) are nanomaterials with interesting properties finding applicatio... more Layered double hydroxides (LDHs) are nanomaterials with interesting properties finding applications in many fields, such as catalysis, environmental chemistry, and pharmaceuticals. They are anionic clays with positively charged layers and anions within the layers to reach neutrality. Their properties are defined by both composition and morphology. The composition can be tuned by exchanging the interlayer anion. The far more stable, common, and highly prevalent among natural LDHs is the carbonate anion thanks to its double negative charge. To adapt the properties of LDHs for technological applications, the challenge is to exchange the carbonate with the functionalizing monovalent anions in an effective and cheap way. In this study, the exchange of carbonate with nitrate ions is studied by in situ X-ray powder diffraction (XRPD). The exchange is carried out by a liquid-assisted grinding approach, inserting the mechanically ground dry sample in a capillary and then wetting it with a dr...
Acta Crystallographica Section A Foundations and Advances
The increasing efficiency of detectors and brightness of X-rays in both laboratory and large-scal... more The increasing efficiency of detectors and brightness of X-rays in both laboratory and large-scale facilities allow the collection of full single-crystal X-ray data sets within minutes. The analysis of these `crystallographic big data' requires new tools and approaches. To answer these needs, the use of principal component analysis (PCA) is proposed to improve the efficiency and speed of the analysis. Potentialities and limitations of PCA were investigated using single-crystal X-ray diffraction (XRD) data collected in situ on Y zeolite, in which CO2, acting as an active species, is thermally adsorbed while cooling from 300 to 200 K. For the first time, thanks to the high sensitivity of single-crystal XRD, it was possible to determine the sites where CO2 is adsorbed, the increase in their occupancy while the temperature is decreased, and the correlated motion of active species, i.e. CO2, H2O and Na+. PCA allowed identification and elimination of problematic data sets, and better ...
A graphene-containing LDH was prepared by re-hydration of the oxides produced by the calcination ... more A graphene-containing LDH was prepared by re-hydration of the oxides produced by the calcination of an organic LDH. While the memory effect is a widely recognized effect on oxides produced by inorganic LDHs, it is unprecedented from the calcination/re-hydration of organic ones. Different temperatures (400, 600 and 1100 °C) were tested, on the basis of thermogravimetric data. Water instead of a carbonate solution was used for the re-hydration, with CO2 available from water itself and/or air to induce a slower process with an easier and better intercalation of the carbonaceous species within the layers. The samples were characterized by X-ray Powder Diffraction (XRPD), IR and Raman spectroscopy and scanning electron microscopy (SEM). XRPD indicate the presence of carbonate LDH mixed with a layered phase with a larger d-spacing. IR confirmed that the prevailing anion is carbonate, coming from the water used for the re-hydration and/or air. Raman data indicated the presence of low-o...
Zeitschrift für Kristallographie - Crystalline Materials, 2017
The crystal structure of sodium naphthalene 2-sulfonate (Na2-NS) is reported. This compound raise... more The crystal structure of sodium naphthalene 2-sulfonate (Na2-NS) is reported. This compound raised the attention as a pollutant, being widely used in industry, and its intercalation in inorganic matrices, such as layered double hydroxides (LDH), could be a suitable removal strategy. The crystal structure of the title compound, despite its simplicity, is not known in the literature, so we looked for a strategy to grow crystals suitable for a single crystal study. Although many attempts were made to recrystallize it, Na2-NS grows in bunches of very thin laminae, with a high degree of mosaicity and intergrowth, explaining the absence of a reported crystal structure. The crystal structure shows layers of Na
PCA, coupled to molecular descriptors, proved to be an effective tool to rationalize the mechanoc... more PCA, coupled to molecular descriptors, proved to be an effective tool to rationalize the mechanochemical intercalation yields of layered materials.
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