Powder Diffraction最新文献

{"title":"Determination of two structures of the solvent 3-hydroxypropionitrile crystallized at low temperatures","authors":"Pamela S. Whitfield, Zouina Karkar, Yaser Abu-Lebdeh","doi":"10.1017/s0885715624000010","DOIUrl":"https://doi.org/10.1017/s0885715624000010","url":null,"abstract":"<p>The title compound, 3-hydroxypropionitrile, was crystallized repeatedly <span>in situ</span> inside a quartz capillary using a liquid nitrogen cryostream. The X-ray powder diffraction patterns obtained indicated the presence of two distinct crystalline phases. The cleanest datasets for each of the phases were used to solve the crystal structures via simulated annealing, followed by refinement and optimization via dispersion-corrected density functional theory (DFT) calculations, with a final Rietveld refinement against the experimental data. The two structures appear to correspond to those proposed in a 1960s literature vibrational spectroscopy paper, one being the more stable with a <span>gauche</span> molecular conformation and the second metastable phase more complex with mixed conformations. Dispersion-corrected DFT computation using lattice parameters for both phases obtained from a single 84 K dataset with co-existing phases shows the stable and metastable phases to differ in energy by less than 0.5 kJ mol<span>−1</span>. A comparison of experimental far infrared spectra published in the 1960s with those calculated from the proposed crystal structures provides some independent supporting evidence for the proposed structures.</p>","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2024-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140008880","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}

{"title":"Crystal structure of indacaterol hydrogen maleate (C24H29N2O3)(HC4H2O4)","authors":"James A. Kaduk, Megan M. Rost, Anja Dosen, Thomas N. Blanton","doi":"10.1017/s0885715624000071","DOIUrl":"https://doi.org/10.1017/s0885715624000071","url":null,"abstract":"The crystal structure of indacaterol hydrogen maleate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Indacaterol hydrogen maleate crystallizes in space group <jats:italic>P</jats:italic>-1 (#24) with <jats:italic>a</jats:italic> = 8.86616(9), <jats:italic>b</jats:italic> = 9.75866(21), <jats:italic>c</jats:italic> = 16.67848(36) Å, <jats:italic>α</jats:italic> = 102.6301(10), β = 94.1736(6), <jats:italic>γ</jats:italic> = 113.2644(2)°, <jats:italic>V</jats:italic> = 1273.095(7) Å<jats:sup>3</jats:sup>, and <jats:italic>Z</jats:italic> = 2 at 295 K. The crystal structure consists of layers of cations and anions parallel to the <jats:italic>ab</jats:italic>-plane. Traditional N–H⋯O and O–H⋯O hydrogen bonds link the cations and anions into chains along the <jats:italic>a</jats:italic>-axis. There is a strong intramolecular charge-assisted O–H⋯O hydrogen bond in the non-planar hydrogen maleate anion. There are also two C–H⋯O hydrogen bonds between the anion and cation. The cation makes a strong N–H⋯O hydrogen bond to the anion, but also acts as a hydrogen bond donor to an aromatic C in another cation. The amino group makes bifurcated N–H⋯O hydrogen bonds, one intramolecular and the other intermolecular. The hydroxyl group acts as a donor to another cation. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2024-02-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140008817","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}

{"title":"Crystal structure and synchrotron X-ray powder reference pattern for the porous pillared cyanonickelate, Ni(3-amino-4,4′-bipyridine)[Ni(CN)4]","authors":"W. Wong-Ng, J. Culp, J.A. Kaduk, Y.S. Chen, S. Lapidus","doi":"10.1017/s0885715624000058","DOIUrl":"https://doi.org/10.1017/s0885715624000058","url":null,"abstract":"The structure of Ni(3-amino-4,4′-bipyridine)[Ni(CN)<jats:sub>4</jats:sub>] (or known as Ni-BpyNH<jats:sub>2</jats:sub>) in powder form was determined using synchrotron X-ray diffraction and refined using the Rietveld refinement technique (<jats:italic>R</jats:italic> = 8.8%). The orthorhombic (C<jats:italic>mca</jats:italic>) cell parameters were determined to be <jats:italic>a</jats:italic> = 14.7218(3) Å, <jats:italic>b</jats:italic> = 22.6615(3) Å, <jats:italic>c</jats:italic> = 12.3833(3) Å, <jats:italic>V</jats:italic> = 4131.29(9) Å<jats:sup>3</jats:sup>, and <jats:italic>Z</jats:italic> = 8. Ni-BpyNH<jats:sub>2</jats:sub> forms a 3-D network, with a 2-D Ni(CN)<jats:sub>4</jats:sub> net connecting to each other via the BpyNH<jats:sub>2</jats:sub> ligands. There are two independent Ni sites on the net. The 2-D nets are connected to each other via the bonding of the pyridine “N” atom to Ni2. The Ni2 site is of six-fold coordination to N with relatively long Ni2–N distances (average of 2.118 Å) as compared to the four-fold coordinated Ni1–C distances (average of 1.850 Å). The Ni(CN)<jats:sub>4</jats:sub> net is arranged in a wave-like fashion. The functional group, –NH<jats:sub>2</jats:sub>, is disordered and was found to be in the <jats:italic>m</jats:italic>-position relative to the N atom of the pyridine ring. Instead of having a unique position, N has ¼ site occupancy in each of the four <jats:italic>m</jats:italic>-positions. The powder reference diffraction pattern for Ni-BpyNH<jats:sub>2</jats:sub> was prepared and submitted to the Powder Diffraction File (PDF) at the International Centre of Diffraction Data (ICDD).","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2024-02-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140008477","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}

{"title":"Simple preparation of specimens for X-ray powder diffraction analysis of radioactive materials: an illustrative example on irradiated granite","authors":"Claudia Aparicio, Vít Rosnecký, Patricie Halodová","doi":"10.1017/s088571562400006x","DOIUrl":"https://doi.org/10.1017/s088571562400006x","url":null,"abstract":"Materials in a high radioactive environment undergo structural changes. X-ray diffraction (XRD) is commonly used to study the micro-structural changes of such materials. Therefore, a safe procedure is required for the preparation of specimens. In this paper, a simple methodology for the preparation of radioactive powder specimens to be analyzed in a non-nuclearized laboratory diffractometer is presented. The process is carried out inside a shielded glove box, where the milling of the radioactive sample and specimen preparation occurs. Minimum amount of sample is required (&lt;20 mg), which is drop-casted on a polyether ether ketone (PEEK) foil and glue-sealed inside a disposable plastic holder for a safe handling of the specimen. One example using neutron-irradiated granite is shown, where unit-cell parameters and crystal density of the main phases were calculated. The developed methodology represents an easy and affordable way to study neutron irradiated materials with low activity at laboratory scale.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2024-02-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140001958","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}

{"title":"Proposed crystal structure of carbadox, C11H10N4O4","authors":"James A. Kaduk, Anja Dosen, Thomas N. Blanton","doi":"10.1017/s0885715624000083","DOIUrl":"https://doi.org/10.1017/s0885715624000083","url":null,"abstract":"A model for the crystal structure of carbadox has been generated and refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Carbadox crystallizes in space group <jats:italic>P2</jats:italic><jats:sub>1</jats:sub> (#4) with <jats:italic>a</jats:italic> = 13.8155(3), <jats:italic>b</jats:italic> = 21.4662(1), <jats:italic>c</jats:italic> = 16.3297(3) Å, <jats:italic>β</jats:italic> = 110.0931(7)°, <jats:italic>V</jats:italic> = 4548.10(3) Å<jats:sup>3</jats:sup>, and <jats:italic>Z</jats:italic> = 16. The crystal structure is characterized by approximately parallel stacking of the eight independent carbadox molecules parallel to the <jats:italic>bc</jats:italic>-plane. There are two different molecular configurations of the eight carbadox molecules; five are in the lower-energy configuration and three are in a ~10% higher-energy configuration. This arrangement likely achieves the lowest-energy crystalline packing via hydrogen bonding. Hydrogen bonds link the molecules both within and between the planes. Each of the amino groups forms a N–H⋯O hydrogen bond to an oxygen atom of the 1,4-dioxidoquinoxaline ring system of another molecule. The result is four pairs of hydrogen-bonded molecules, which form rings with graph set <jats:italic>R2,2(14)</jats:italic>. Variation in specimen preparation can affect the preferred orientation of particles considerably. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2024-02-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140008526","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}

{"title":"Crystal structure of ractopamine hydrochloride, C18H24NO3Cl","authors":"Colin W. Scherry, Nicholas C. Boaz, James A. Kaduk, Anja Dosen, Thomas N. Blanton","doi":"10.1017/s0885715624000095","DOIUrl":"https://doi.org/10.1017/s0885715624000095","url":null,"abstract":"The crystal structure of ractopamine hydrochloride has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Ractopamine hydrochloride crystallizes in space group <jats:italic>Pbca</jats:italic> (#61) with <jats:italic>a</jats:italic> = 38.5871(49), <jats:italic>b</jats:italic> = 10.7691(3), <jats:italic>c</jats:italic> = 8.4003(2) Å, <jats:italic>V</jats:italic> = 3490.75(41) Å<jats:sup>3</jats:sup>, and <jats:italic>Z</jats:italic> = 8. The ractopamine cation contains two chiral centers, and the sample consists of a mixture of the S,S/R,R/S,R and R,S forms. Models for the two diastereomers S,S and S,R were refined, and yielded equivalent residuals, but the S,R form is significantly lower in energy. The crystal structure consists of layers of molecules parallel to the <jats:italic>bc</jats:italic>-plane. In each structure one of the H atoms on the protonated N atom acts as a donor in a strong discrete N–H⋯Cl hydrogen bond. Hydroxyl groups act as donors in O–H⋯Cl and O–H⋯O hydrogen bonds. Both the classical and C–H⋯Cl and C–H⋯O hydrogen bonds differ between the forms, helping to explain the large microstrain observed for the sample. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2024-02-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140008729","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}

{"title":"Crystal structure of anthraquinone-2-carboxylic acid, C15H8O4","authors":"Tawnee M. Ens, James A. Kaduk, Anja Dosen, Thomas N. Blanton","doi":"10.1017/s0885715624000046","DOIUrl":"https://doi.org/10.1017/s0885715624000046","url":null,"abstract":"The crystal structure of anthraquinone-2-carboxylic acid has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Anthraquinone-2-carboxylic acid crystallizes in space group <jats:italic>P</jats:italic>-1 (#2) with <jats:italic>a</jats:italic> = 3.7942(2), <jats:italic>b</jats:italic> = 13.266(5), <jats:italic>c</jats:italic> = 22.835(15) Å, <jats:italic>α</jats:italic> = 73.355(30), <jats:italic>β</jats:italic> = 89.486(6), <jats:italic>γ</jats:italic> = 86.061(1)°, <jats:italic>V</jats:italic> = 1098.50(7) Å<jats:sup>3</jats:sup>, and <jats:italic>Z</jats:italic> = 4. The crystal structure contains two independent molecules of anthraquinone-2-carboxylic acid. Although the expected hydrogen-bonded dimers are present, the dimers are not centrosymmetric. The dimer contains one molecule of each planar low-energy conformation. The crystal structure consists of a herringbone array of centrosymmetric pairs of molecules parallel to the <jats:italic>bc</jats:italic>-plane. The molecules stack along the short <jats:italic>a</jats:italic>-axis. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2024-02-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139909589","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}

{"title":"Experimental electron density distribution of KZnB3O6 constructed by maximum-entropy method","authors":"Qi Li, Yi Huang, Yanfang Lou, Munan Hao, Shifeng Jin","doi":"10.1017/s0885715623000428","DOIUrl":"https://doi.org/10.1017/s0885715623000428","url":null,"abstract":"<p>The dynamic charge density of KZnB<span>3</span>O<span>6</span>, which contains edge-sharing BO<span>4</span> units, has been characterized using laboratory and synchrotron X-ray diffraction techniques. The experimental electron density distribution (EDD) was constructed using the maximum-entropy method (MEM) from single crystal diffraction data obtained at 81 and 298 K. Additionally, MEM-based pattern fitting (MPF) method was employed to refine the synchrotron powder diffraction data obtained at 100 K. Both the room-temperature single crystal diffraction data and the cryogenic synchrotron powder diffraction data reveal an intriguing phenomenon: the edge-shared B<span>2</span>O<span>2</span> ring exhibits a significant charge density accumulation between the O atoms. Further analysis of high-quality single crystal diffraction data collected at 81 K, with both high resolution and large signal-to-noise ratio, reveals no direct O–O bonding within the B<span>2</span>O<span>2</span> ring. The experimental EDD of KZnB<span>3</span>O<span>6</span> obtained aligns with the results obtained from <span>ab-initio</span> calculations. Our work underscores the importance of obtaining high-quality experimental data to accurately determine EDDs.</p>","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2024-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139762794","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}

{"title":"X-ray powder diffraction data for three new compounds obtained as a result of CO2 capture","authors":"Klaudia Nowakowska, Wiesław Łasocha","doi":"10.1017/s0885715623000404","DOIUrl":"https://doi.org/10.1017/s0885715623000404","url":null,"abstract":"The field of research related to CO<jats:sub>2</jats:sub> capture is significant and really attractive for sustainable green chemistry. Focusing attention on this topic in our research led to obtaining new compounds based on diamines. As a result of the syntheses carried out using aqueous solutions of diamines exposed to the slow action of carbon dioxide from the air, three new monocarbamates were obtained. X-ray powder diffraction data for the obtained compounds: 12-propCO<jats:sub>2</jats:sub> (C<jats:sub>4</jats:sub>H<jats:sub>10</jats:sub>N<jats:sub>2</jats:sub>O<jats:sub>2</jats:sub>) [<jats:italic>a =</jats:italic> 9.3033(7), <jats:italic>b =</jats:italic> 9.2485(7), <jats:italic>c =</jats:italic> 7.4735(7) <jats:italic>Å</jats:italic>, <jats:italic>β =</jats:italic> 111.214(7)<jats:italic>°</jats:italic>, <jats:italic>V =</jats:italic> 599.46 <jats:italic>Å<jats:sup>3</jats:sup></jats:italic>, <jats:italic>Z = 4</jats:italic>, space group <jats:italic>Ia</jats:italic>]; 13-propCO<jats:sub>2</jats:sub> (C<jats:sub>4</jats:sub>H<jats:sub>10</jats:sub>N<jats:sub>2</jats:sub>O<jats:sub>2</jats:sub>) [<jats:italic>a =</jats:italic> 5.0065(10), <jats:italic>b =</jats:italic> 12.2093(23), <jats:italic>c =</jats:italic> 4.9006(10) <jats:italic>Å</jats:italic>, <jats:italic>β =</jats:italic> 96.457(18)<jats:italic>°</jats:italic>, <jats:italic>V =</jats:italic> 297.65 <jats:italic>Å<jats:sup>3</jats:sup></jats:italic>, <jats:italic>Z = 2,</jats:italic> space group <jats:italic>P</jats:italic>2<jats:sub>1</jats:sub>]; and 13-dytekCO<jats:sub>2</jats:sub> (C<jats:sub>6</jats:sub>H<jats:sub>14</jats:sub>N<jats:sub>2</jats:sub>O<jats:sub>2</jats:sub>) [<jats:italic>a =</jats:italic> 28.374(3), <jats:italic>c =</jats:italic> 5.1726(9) <jats:italic>Å</jats:italic>, <jats:italic>V =</jats:italic> 3606.53 <jats:italic>Å<jats:sup>3</jats:sup></jats:italic>, <jats:italic>Z = 18,</jats:italic> space group <jats:inline-formula> <jats:alternatives> <jats:inline-graphic xmlns:xlink=\"http://www.w3.org/1999/xlink\" mime-subtype=\"png\" xlink:href=\"S0885715623000404_inline1.png\" /> <jats:tex-math>$Rbar{3}$</jats:tex-math> </jats:alternatives> </jats:inline-formula>] are reported in this paper.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2023-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138495279","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}

{"title":"Crystal structure and X-ray powder diffraction data for Lumateperone tosylate","authors":"Jiyong Liu, Dier Shi, Shuna Liu, Xiurong Hu","doi":"10.1017/s0885715623000337","DOIUrl":"https://doi.org/10.1017/s0885715623000337","url":null,"abstract":"X-ray powder diffraction data, unit-cell parameters, and space group for the Lumateperone tosylate, C 24 H 29 FN 3 O⋅C 7 H 7 O 3 S, are reported [ a = 15.5848(10) Å, b = 6.0700(4) Å, c = 31.3201(14) Å, β = 96.544(5)°, V = 2943.58 Å 3 , Z = 4, and space group C 2]. In each case, all measured lines were indexed and were consistent with the corresponding space group. The single-crystal data of Lumateperone tosylate is also reported, respectively [ a = 15.626(3) Å, b = 6.0806(10) Å, c = 31.415(5) Å, β = 96.609(7)°, V = 2965.1(8) Å 3 , Z = 4, and space group C 2]. The experimental powder diffraction pattern has been well matched with the simulated pattern derived from the single-crystal data with preferred orientation in the [002] direction (orientation coefficient = 0.75).","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136262759","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}