Pub Date : 2023-05-26DOI: 10.1017/S0885715623000179
J. Lyza, T. Fawcett, Sarah N. Page, K. L. Cook
Quantitative phase analysis (QPA) of slags is complex due to the natural richness of phases and variability in sample composition. The number of phases frequently exceeds 10, with certain slag types (EAF, BOF, blends, stainless) having extreme peak overlap, making identification difficult. Another convolution arises from the variable crystallite sizes of phases found in slag, as well as the mixture of crystalline and amorphous components specific to each slag type. Additionally, polymorphs are common because of the complexity of the steelmaking and slag cooling processes, such as the cation-doped calcium aluminum silicate (Ca3Al2O6, C3A, Z = 24) supercell in LMF slag. References for these doped variants may not exist or in many cases are not known in advance, therefore it is incumbent on the analyzer to be aware of such discrepancies and choose the best available reference. All issues can compound to form a highly intricate QPA and have prevented previous methods of QPA from accurately measuring phase components in slag. QPA was performed via the internal standard method using 8 wt% ZnO as the internal standard and JADE Pro's Whole Pattern Fitting analysis. For each phase, five variables (lattice parameters, preferred orientation, scale factor, temperature factor, and crystallite size) must be accounted for during quantitation, with a specific emphasis on not refining crystallite sizes for iron oxides and trace phases as they are inclined to over-broaden and interact with the background to improve the goodness of fit (R/E value). Preliminary investigations show somewhat reliable results with the use of custom file sets created within PDF-4+ specifically targeted toward slag minerals to further regulate and normalize the analysis process. The objective of this research is to provide a standard protocol for collecting data, as well as to update methodologies and databases for QPA, to the slag community for implementation in a conventional laboratory setting. Currently, Whole Pattern Fitting “Modified” Rietveld block refinement coupled with the addition of a ZnO internal standard gives the most accurate QPA results, though further research is needed to improve upon the complex issues found in this study of the QPA of slags.
{"title":"Challenges of quantitative phase analysis of iron and steel slags: a look at sample complexity","authors":"J. Lyza, T. Fawcett, Sarah N. Page, K. L. Cook","doi":"10.1017/S0885715623000179","DOIUrl":"https://doi.org/10.1017/S0885715623000179","url":null,"abstract":"Quantitative phase analysis (QPA) of slags is complex due to the natural richness of phases and variability in sample composition. The number of phases frequently exceeds 10, with certain slag types (EAF, BOF, blends, stainless) having extreme peak overlap, making identification difficult. Another convolution arises from the variable crystallite sizes of phases found in slag, as well as the mixture of crystalline and amorphous components specific to each slag type. Additionally, polymorphs are common because of the complexity of the steelmaking and slag cooling processes, such as the cation-doped calcium aluminum silicate (Ca3Al2O6, C3A, Z = 24) supercell in LMF slag. References for these doped variants may not exist or in many cases are not known in advance, therefore it is incumbent on the analyzer to be aware of such discrepancies and choose the best available reference. All issues can compound to form a highly intricate QPA and have prevented previous methods of QPA from accurately measuring phase components in slag. QPA was performed via the internal standard method using 8 wt% ZnO as the internal standard and JADE Pro's Whole Pattern Fitting analysis. For each phase, five variables (lattice parameters, preferred orientation, scale factor, temperature factor, and crystallite size) must be accounted for during quantitation, with a specific emphasis on not refining crystallite sizes for iron oxides and trace phases as they are inclined to over-broaden and interact with the background to improve the goodness of fit (R/E value). Preliminary investigations show somewhat reliable results with the use of custom file sets created within PDF-4+ specifically targeted toward slag minerals to further regulate and normalize the analysis process. The objective of this research is to provide a standard protocol for collecting data, as well as to update methodologies and databases for QPA, to the slag community for implementation in a conventional laboratory setting. Currently, Whole Pattern Fitting “Modified” Rietveld block refinement coupled with the addition of a ZnO internal standard gives the most accurate QPA results, though further research is needed to improve upon the complex issues found in this study of the QPA of slags.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"38 1","pages":"119 - 138"},"PeriodicalIF":0.5,"publicationDate":"2023-05-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45489455","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-18DOI: 10.1017/s0885715623000167
F. Ferreira, A. Pereira, I. B. Reis, B. Sasaki, W. Fávaro, N. Durán
Although being an old concern, phosphate analysis is still a tremendous challenge. While many different experimental techniques are found in the literature, very few use powder X-ray diffraction (PXRD) patterns for quantitative phase analysis of different phosphate types. Our measurements performed in four commercial samples of diammonium hydrogen phosphate ((NH4)2HPO4) (DAP) show the existence of phosphate contamination mixtures, such as ammonium dihydrogen phosphate (NH4H2PO4) (ADP). The larger the amount of ADP, the larger the microstrain induced in the DAP phase, which impacts both the aggregation of the nanoparticles in solution and the final anticancer activity of the nanostructure. This study shows that PXRD is an excellent technique for quantitative phase analysis to determine the presence and amount of phosphate contamination in diammonium hydrogen phosphate samples.
{"title":"Quantitative phase analysis of commercial ammonium phosphates by PXRD for application in biological systems","authors":"F. Ferreira, A. Pereira, I. B. Reis, B. Sasaki, W. Fávaro, N. Durán","doi":"10.1017/s0885715623000167","DOIUrl":"https://doi.org/10.1017/s0885715623000167","url":null,"abstract":"Although being an old concern, phosphate analysis is still a tremendous challenge. While many different experimental techniques are found in the literature, very few use powder X-ray diffraction (PXRD) patterns for quantitative phase analysis of different phosphate types. Our measurements performed in four commercial samples of diammonium hydrogen phosphate ((NH4)2HPO4) (DAP) show the existence of phosphate contamination mixtures, such as ammonium dihydrogen phosphate (NH4H2PO4) (ADP). The larger the amount of ADP, the larger the microstrain induced in the DAP phase, which impacts both the aggregation of the nanoparticles in solution and the final anticancer activity of the nanostructure. This study shows that PXRD is an excellent technique for quantitative phase analysis to determine the presence and amount of phosphate contamination in diammonium hydrogen phosphate samples.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":" ","pages":""},"PeriodicalIF":0.5,"publicationDate":"2023-05-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47393980","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-16DOI: 10.1017/s0885715623000155
L. Liang, Weijun Li, Meiwen Lu, Sheng-Kun Li, Degui Li, Bin Gu
A new ternary intermetallic compound Al3GaCu9 was synthesized experimentally. A high-quality powder diffraction pattern of the compound was collected by an X-ray diffractometer, and its crystal structure was determined using the Rietveld refinement method. Results show that the compound has a cubic cell with the Al4Cu9 structure type (space group $Pbar{4}3m$ and Pearson symbol cP52). The lattice parameter a = 8.7132(3) Å, unit-cell volume V = 661.52 Å3, calculated density Dcalc = 7.26 g/cm3, and Z = 4. The residual factors converge to Rp = 2.96%, Rwp = 4.06%, and Rexp = 2.57%. The experimentally obtained reference intensity ratio value is 7.04.
{"title":"Experimental synthesis and crystal structure refinement of a new ternary intermetallic compound Al3GaCu9","authors":"L. Liang, Weijun Li, Meiwen Lu, Sheng-Kun Li, Degui Li, Bin Gu","doi":"10.1017/s0885715623000155","DOIUrl":"https://doi.org/10.1017/s0885715623000155","url":null,"abstract":"A new ternary intermetallic compound Al3GaCu9 was synthesized experimentally. A high-quality powder diffraction pattern of the compound was collected by an X-ray diffractometer, and its crystal structure was determined using the Rietveld refinement method. Results show that the compound has a cubic cell with the Al4Cu9 structure type (space group \u0000 \u0000 \u0000 $Pbar{4}3m$\u0000 \u0000 and Pearson symbol cP52). The lattice parameter a = 8.7132(3) Å, unit-cell volume V = 661.52 Å3, calculated density Dcalc = 7.26 g/cm3, and Z = 4. The residual factors converge to Rp = 2.96%, Rwp = 4.06%, and Rexp = 2.57%. The experimentally obtained reference intensity ratio value is 7.04.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":" ","pages":""},"PeriodicalIF":0.5,"publicationDate":"2023-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42643706","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-16DOI: 10.1017/S0885715623000143
M. Rodriguez, John Krukar, N. Valdez, James Z. Harris, Kathryn A. Perkins, C. Diantonio, Pin Yang
Pb–Zr–Ti–O (PZT) perovskites span a large solid-solution range and have found widespread use due to their piezoelectric and ferroelectric properties that also span a large range. Crystal structure analysis via Rietveld refinement facilitates materials analysis via the extraction of the structural parameters. These parameters, often obtained as a function of an additional dimension (e.g., pressure), can help to diagnose materials response within a use environment. Often referred to as “in-situ” studies, these experiments provide an abundance of data. Viewing structural changes due to applied pressure conditions can give much-needed insight into materials performance. However, challenges exist for viewing/presenting results when the details are inherently three-dimensional (3D) in nature. For PZT perovskites, the use of polyhedra (e.g., Zr/Ti–O6 octahedra) to view bonding/connectivity is beneficial; however, the visualization of the octahedra behavior with pressure dependence is less easily demonstrated due to the complexity of the added pressure dimension. We present a more intuitive visualization by projecting structural data into virtual reality (VR). We employ previously published structural data for Pb0.99(Zr0.95Ti0.05)0.98Nb0.02O3 as an exemplar for VR visualization of the PZT R3c crystal structure between ambient and 0.62 GPa pressure. This is accomplished via our in-house CAD2VR™ software platform and the new CrystalVR plugin. The use of the VR environment enables a more intuitive viewing experience, while enabling on-the-fly evaluation of crystal data, to form a detailed and comprehensive understanding of in-situ datasets. Discussion of methodology and tools for viewing are given, along with how recording results in video form can enable the viewing experience.
{"title":"Evaluating the pressure dependence of PZT structures using a virtual reality environment","authors":"M. Rodriguez, John Krukar, N. Valdez, James Z. Harris, Kathryn A. Perkins, C. Diantonio, Pin Yang","doi":"10.1017/S0885715623000143","DOIUrl":"https://doi.org/10.1017/S0885715623000143","url":null,"abstract":"Pb–Zr–Ti–O (PZT) perovskites span a large solid-solution range and have found widespread use due to their piezoelectric and ferroelectric properties that also span a large range. Crystal structure analysis via Rietveld refinement facilitates materials analysis via the extraction of the structural parameters. These parameters, often obtained as a function of an additional dimension (e.g., pressure), can help to diagnose materials response within a use environment. Often referred to as “in-situ” studies, these experiments provide an abundance of data. Viewing structural changes due to applied pressure conditions can give much-needed insight into materials performance. However, challenges exist for viewing/presenting results when the details are inherently three-dimensional (3D) in nature. For PZT perovskites, the use of polyhedra (e.g., Zr/Ti–O6 octahedra) to view bonding/connectivity is beneficial; however, the visualization of the octahedra behavior with pressure dependence is less easily demonstrated due to the complexity of the added pressure dimension. We present a more intuitive visualization by projecting structural data into virtual reality (VR). We employ previously published structural data for Pb0.99(Zr0.95Ti0.05)0.98Nb0.02O3 as an exemplar for VR visualization of the PZT R3c crystal structure between ambient and 0.62 GPa pressure. This is accomplished via our in-house CAD2VR™ software platform and the new CrystalVR plugin. The use of the VR environment enables a more intuitive viewing experience, while enabling on-the-fly evaluation of crystal data, to form a detailed and comprehensive understanding of in-situ datasets. Discussion of methodology and tools for viewing are given, along with how recording results in video form can enable the viewing experience.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"38 1","pages":"90 - 99"},"PeriodicalIF":0.5,"publicationDate":"2023-05-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44726273","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-04-28DOI: 10.1017/S0885715623000106
M. Zampieri, Guseppe Barreca, N. Masciocchi
X-ray powder diffraction data, including unit cell parameters and space group assignment, for the ESP15228 species of C19H34O5 formula, are here reported [a = 6.0434(6), b = 12.2543(6), c = 14.0285(8) Å, α = 86.584(3), β = 85.707(10), γ = 78.801(5)°, V = 1015.2(1) Å3, Z = 2, ρcalc = 1.152 g cm−3, and space group P-1]. All measured lines were indexed and no detectable impurities were observed.
本文报道了C19H34O5式ESP15228物种的X射线粉末衍射数据，包括晶胞参数和空间组分配[a=6.0434（6），b=12.2543（6）、c=14.0285（8）Å，α=86.584（3），β=85.707（10），γ=78.801（5）°，V=105.2（1）Å3，Z=2，ρcalc=1.152 g cm−3和空间组P-1]。所有测得的线都被索引，并且没有观察到可检测的杂质。
{"title":"X-ray powder diffraction data for ESP15228, C19H34O5, a bempedoic acid metabolite","authors":"M. Zampieri, Guseppe Barreca, N. Masciocchi","doi":"10.1017/S0885715623000106","DOIUrl":"https://doi.org/10.1017/S0885715623000106","url":null,"abstract":"X-ray powder diffraction data, including unit cell parameters and space group assignment, for the ESP15228 species of C19H34O5 formula, are here reported [a = 6.0434(6), b = 12.2543(6), c = 14.0285(8) Å, α = 86.584(3), β = 85.707(10), γ = 78.801(5)°, V = 1015.2(1) Å3, Z = 2, ρcalc = 1.152 g cm−3, and space group P-1]. All measured lines were indexed and no detectable impurities were observed.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"38 1","pages":"158 - 160"},"PeriodicalIF":0.5,"publicationDate":"2023-04-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48657237","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-04-03DOI: 10.1017/S088571562300012X
M. Witte
X-ray fluorescence (XRF) is frequently used to measure layer thickness in the micrometer range. But also X-ray diffraction (XRD) can be used in a comparable way and offers the benefit to differentiate coating layers by their crystal structure. Thus, the thickness of different oxide layers of the same element can be determined, e.g., FeO, Fe3O4, and Fe2O3 on Fe-substrate. An approach for such measurement is discussed. Furthermore, with a suitable sample stage, a spatially resolved coating thickness map can be measured in a nondestructive way. Applications and validations of the presented XRD method for the measurement of the thickness of zinc coatings on steel are given and compared with results from XRF, glow-discharge optical emission spectroscopy, and optical micrographs. In addition, the methodology was tested and validated using XRF reference standards and iron nitride and iron oxide layers.
{"title":"Measurement of coating thickness with X-ray diffraction","authors":"M. Witte","doi":"10.1017/S088571562300012X","DOIUrl":"https://doi.org/10.1017/S088571562300012X","url":null,"abstract":"X-ray fluorescence (XRF) is frequently used to measure layer thickness in the micrometer range. But also X-ray diffraction (XRD) can be used in a comparable way and offers the benefit to differentiate coating layers by their crystal structure. Thus, the thickness of different oxide layers of the same element can be determined, e.g., FeO, Fe3O4, and Fe2O3 on Fe-substrate. An approach for such measurement is discussed. Furthermore, with a suitable sample stage, a spatially resolved coating thickness map can be measured in a nondestructive way. Applications and validations of the presented XRD method for the measurement of the thickness of zinc coatings on steel are given and compared with results from XRF, glow-discharge optical emission spectroscopy, and optical micrographs. In addition, the methodology was tested and validated using XRF reference standards and iron nitride and iron oxide layers.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"38 1","pages":"112 - 118"},"PeriodicalIF":0.5,"publicationDate":"2023-04-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46537647","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-04-03DOI: 10.1017/S0885715623000118
J. Kaduk, A. Došen, T. Blanton
The crystal structure of encorafenib, C22H27ClFN7O4S, has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Encorafenib crystallizes in space group P21 (#4) with a = 16.17355(25), b = 9.52334(11), c = 17.12368(19) Å, β = 89.9928(22)°, V = 2637.50(4) Å3, and Z = 4. The crystal structure consists of alternating layers of stacked halogenated phenyl rings and the other parts of the molecules perpendicular to the a-axis. One molecule participates in two strong N–H⋯N hydrogen bonds (one intra- and the other intermolecular), which are not present for the other molecule. The intermolecular hydrogen bonds link molecule 2 into a spiral chain along the b-axis. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).
{"title":"Crystal structure of encorafenib, C22H27ClFN7O4S","authors":"J. Kaduk, A. Došen, T. Blanton","doi":"10.1017/S0885715623000118","DOIUrl":"https://doi.org/10.1017/S0885715623000118","url":null,"abstract":"The crystal structure of encorafenib, C22H27ClFN7O4S, has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Encorafenib crystallizes in space group P21 (#4) with a = 16.17355(25), b = 9.52334(11), c = 17.12368(19) Å, β = 89.9928(22)°, V = 2637.50(4) Å3, and Z = 4. The crystal structure consists of alternating layers of stacked halogenated phenyl rings and the other parts of the molecules perpendicular to the a-axis. One molecule participates in two strong N–H⋯N hydrogen bonds (one intra- and the other intermolecular), which are not present for the other molecule. The intermolecular hydrogen bonds link molecule 2 into a spiral chain along the b-axis. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"38 1","pages":"145 - 151"},"PeriodicalIF":0.5,"publicationDate":"2023-04-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44736849","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-22DOI: 10.1017/S088571562300009X
P. Whitfield
Dimethyl carbonate (DMC) is an important industrial solvent but is additionally a common component of liquid lithium-ion battery electrolytes. Pure DMC has a melting point of 277 K, so encountering solidification under outdoor climatic conditions is very likely in many locations around the globe. Even eutectic, ethylene carbonate:dimethyl carbonate commercial LiPF6 salt electrolyte formulations can start to solidify at temperatures around 260 K with obvious consequences for their performance. No structures for crystalline DMC are currently available which could be a hindrance for in situ battery studies at reduced temperatures. A time-of-flight neutron powder diffraction study of the phase behavior and crystal structures of deuterated DMC was undertaken to help fill this knowledge gap. Three different orthorhombic crystalline phases were found with a previously unreported low-temperature phase transition around 50–55 K. The progression of Pbca → Pbcm → Ibam space groups follow a sequence of group–subgroup relationships with the final Ibam structure being disordered around the central carbon atom.
{"title":"Low-temperature crystal structures of the solvent dimethyl carbonate","authors":"P. Whitfield","doi":"10.1017/S088571562300009X","DOIUrl":"https://doi.org/10.1017/S088571562300009X","url":null,"abstract":"Dimethyl carbonate (DMC) is an important industrial solvent but is additionally a common component of liquid lithium-ion battery electrolytes. Pure DMC has a melting point of 277 K, so encountering solidification under outdoor climatic conditions is very likely in many locations around the globe. Even eutectic, ethylene carbonate:dimethyl carbonate commercial LiPF6 salt electrolyte formulations can start to solidify at temperatures around 260 K with obvious consequences for their performance. No structures for crystalline DMC are currently available which could be a hindrance for in situ battery studies at reduced temperatures. A time-of-flight neutron powder diffraction study of the phase behavior and crystal structures of deuterated DMC was undertaken to help fill this knowledge gap. Three different orthorhombic crystalline phases were found with a previously unreported low-temperature phase transition around 50–55 K. The progression of Pbca → Pbcm → Ibam space groups follow a sequence of group–subgroup relationships with the final Ibam structure being disordered around the central carbon atom.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"38 1","pages":"100 - 111"},"PeriodicalIF":0.5,"publicationDate":"2023-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46366293","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-01DOI: 10.1017/S0885715623000064
A. Ferreras, Mitchell D. Miller
The U.S. National Committee for Crystallography (USNC/Cr) of the National Academies of Sciences, Engineering, and Medicine provided an online workshop series for researchers on the use, development, and maintenance of crystallographic and structural databases in the Spring of 2022. Encompassing macromolecular, small molecule, and powder diffraction information, the series included 11 modules each meeting for 1 or 2 days. Graduate students, postdoctoral fellows, faculty members and researchers in any of the crystallographic, diffraction, and imaging sciences affiliated with the International Union of Crystallography (IUCr) were encouraged to register and participate in the training sessions that interest them.
{"title":"Exploring structural database use in crystallography: a workshop series of the U.S. National Committee for Crystallography","authors":"A. Ferreras, Mitchell D. Miller","doi":"10.1017/S0885715623000064","DOIUrl":"https://doi.org/10.1017/S0885715623000064","url":null,"abstract":"The U.S. National Committee for Crystallography (USNC/Cr) of the National Academies of Sciences, Engineering, and Medicine provided an online workshop series for researchers on the use, development, and maintenance of crystallographic and structural databases in the Spring of 2022. Encompassing macromolecular, small molecule, and powder diffraction information, the series included 11 modules each meeting for 1 or 2 days. Graduate students, postdoctoral fellows, faculty members and researchers in any of the crystallographic, diffraction, and imaging sciences affiliated with the International Union of Crystallography (IUCr) were encouraged to register and participate in the training sessions that interest them.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"38 1","pages":"74 - 78"},"PeriodicalIF":0.5,"publicationDate":"2023-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41776250","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-01DOI: 10.1017/S0885715622000562
J. Kaduk, S. Gates-Rector, T. Blanton
The crystal structure of butenafine hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Butenafine hydrochloride crystallizes in space group P21 (#4) with a = 13.94807(5), b = 9.10722(2), c = 16.46676(6) Å, β = 93.9663(5)°, V = 2086.733(8) Å3, and Z = 4. Butenafine hydrochloride occurs as a racemic co-crystal of R and S enantiomers of the cation. The crystal structure is characterized by parallel stacks of aromatic rings along the b-axis. Each cation forms a strong discrete N–H⋯Cl hydrogen bond. The chloride anions also act as acceptors in several C–H⋯Cl hydrogen bonds from methylene, methyl, and aromatic groups. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).
{"title":"Crystal structure of butenafine hydrochloride, C23H28NCl","authors":"J. Kaduk, S. Gates-Rector, T. Blanton","doi":"10.1017/S0885715622000562","DOIUrl":"https://doi.org/10.1017/S0885715622000562","url":null,"abstract":"The crystal structure of butenafine hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Butenafine hydrochloride crystallizes in space group P21 (#4) with a = 13.94807(5), b = 9.10722(2), c = 16.46676(6) Å, β = 93.9663(5)°, V = 2086.733(8) Å3, and Z = 4. Butenafine hydrochloride occurs as a racemic co-crystal of R and S enantiomers of the cation. The crystal structure is characterized by parallel stacks of aromatic rings along the b-axis. Each cation forms a strong discrete N–H⋯Cl hydrogen bond. The chloride anions also act as acceptors in several C–H⋯Cl hydrogen bonds from methylene, methyl, and aromatic groups. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":"38 1","pages":"30 - 36"},"PeriodicalIF":0.5,"publicationDate":"2023-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45324187","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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