Powder Diffraction最新文献

英文中文

Simple preparation of specimens for X-ray powder diffraction analysis of radioactive materials: an illustrative example on irradiated granite 放射性材料 X 射线粉末衍射分析试样的简单制备：辐照花岗岩示例

IF 0.5 4区材料科学 Q4 MATERIALS SCIENCE, CHARACTERIZATION & TESTING

Powder Diffraction

Pub Date : 2024-02-29 DOI: 10.1017/s088571562400006x

Claudia Aparicio, Vít Rosnecký, Patricie Halodová

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 (<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.

高放射性环境中的材料会发生结构变化。X 射线衍射 (XRD) 通常用于研究这类材料的微观结构变化。因此，需要一个安全的试样制备程序。本文介绍了一种制备放射性粉末试样的简单方法，以便在非核化实验室衍射仪中进行分析。该过程在屏蔽手套箱内进行，放射性样品的研磨和试样制备都在手套箱内进行。只需最小量的样品（20 毫克），将其滴铸在聚醚醚酮（PEEK）箔上，然后用胶水密封在一次性塑料支架内，以便安全处理样品。图中展示了一个使用中子辐照花岗岩的示例，在该示例中计算了主要相的单胞参数和晶体密度。所开发的方法是在实验室规模研究低活性中子辐照材料的一种简便而经济的方法。

引用次数: 0

Proposed crystal structure of carbadox, C11H10N4O4 卡巴多克斯（C11H10N4O4）的拟议晶体结构

IF 0.5 4区材料科学 Q4 MATERIALS SCIENCE, CHARACTERIZATION & TESTING

Powder Diffraction

Pub Date : 2024-02-29 DOI: 10.1017/s0885715624000083

James A. Kaduk, Anja Dosen, Thomas N. Blanton

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 P21 (#4) with a = 13.8155(3), b = 21.4662(1), c = 16.3297(3) Å, β = 110.0931(7)°, V = 4548.10(3) Å3, and Z = 16. The crystal structure is characterized by approximately parallel stacking of the eight independent carbadox molecules parallel to the bc-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 R2,2(14). 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®).

利用同步辐射 X 射线粉末衍射数据生成并完善了卡巴多克的晶体结构模型，并利用密度泛函理论技术对其进行了优化。Carbadox 在空间群 P21（#4）中结晶，a = 13.8155(3)，b = 21.4662(1)，c = 16.3297(3)埃，β = 110.0931(7)°，V = 4548.10(3)埃3，Z = 16。晶体结构的特点是八个独立的卡巴多克斯分子平行于 bc 平面近似平行堆积。八个卡巴多克斯分子有两种不同的分子构型：五个处于低能构型，三个处于约 10% 的高能构型。这种排列可能是通过氢键实现最低能量的晶体堆积。氢键将平面内和平面间的分子连接起来。每个氨基都与另一个分子的 1,4-二氧代喹喔啉环系统的一个氧原子形成 N-H⋯O 氢键。这样就形成了四对氢键分子，它们构成了图集为 R2,2(14)的环。试样制备的不同会对颗粒的优先取向产生很大影响。该粉末图样已提交给 ICDD，以便纳入粉末衍射文件™ (PDF®)。

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引用次数: 0

Crystal structure of ractopamine hydrochloride, C18H24NO3Cl 盐酸莱克多巴胺（C18H24NO3Cl）的晶体结构

IF 0.5 4区材料科学 Q4 MATERIALS SCIENCE, CHARACTERIZATION & TESTING

Powder Diffraction

Pub Date : 2024-02-29 DOI: 10.1017/s0885715624000095

Colin W. Scherry, Nicholas C. Boaz, James A. Kaduk, Anja Dosen, Thomas N. Blanton

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 Pbca (#61) with a = 38.5871(49), b = 10.7691(3), c = 8.4003(2) Å, V = 3490.75(41) Å3, and Z = 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 bc-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®).

利用同步辐射 X 射线粉末衍射数据解决和完善了盐酸莱克多巴胺的晶体结构，并利用密度泛函理论技术对其晶体结构进行了优化。莱克多巴胺盐酸盐在空间群 Pbca (#61) 中结晶，a = 38.5871(49)，b = 10.7691(3)，c = 8.4003(2) Å，V = 3490.75(41) Å3，Z = 8。对 S,S 和 S,R 两种非对映异构体的模型进行了改进，得到了相同的残差，但 S,R 形式的能量要低得多。晶体结构由平行于 bc 平面的分子层组成。在每种结构中，质子化 N 原子上的一个 H 原子都是强离散 N-H⋯Cl 氢键的供体。羟基在 O-H⋯Cl 和 O-H⋯O 氢键中充当供体。经典氢键、C-H⋯Cl 氢键和 C-H⋯O 氢键在不同形式之间都存在差异，这有助于解释在样品中观察到的巨大微应变。粉末图样已提交给 ICDD®，以便纳入粉末衍射文件™ (PDF®)。

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引用次数: 0

Crystal structure of anthraquinone-2-carboxylic acid, C15H8O4 蒽醌-2-羧酸（C15H8O4）的晶体结构

IF 0.5 4区材料科学 Q4 MATERIALS SCIENCE, CHARACTERIZATION & TESTING

Powder Diffraction

Pub Date : 2024-02-19 DOI: 10.1017/s0885715624000046

Tawnee M. Ens, James A. Kaduk, Anja Dosen, Thomas N. Blanton

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 P-1 (#2) with a = 3.7942(2), b = 13.266(5), c = 22.835(15) Å, α = 73.355(30), β = 89.486(6), γ = 86.061(1)°, V = 1098.50(7) Å3, and Z = 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 bc-plane. The molecules stack along the short a-axis. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™ (PDF®).

利用同步辐射 X 射线粉末衍射数据解决和完善了蒽醌-2-羧酸的晶体结构，并利用密度泛函理论技术对其进行了优化。蒽醌-2-羧酸在空间群 P-1 (#2) 中结晶，a = 3.7942(2)，b = 13.266(5)，c = 22.835(15) Å，α = 73.355(30)，β = 89.486(6)，γ = 86.061(1)°，V = 1098.50(7) Å3，Z = 4。该晶体结构包含两个独立的蒽醌-2-羧酸分子。虽然存在预期的氢键二聚体，但二聚体并不是中心对称的。二聚体中每个平面低能构象都包含一个分子。晶体结构由一对对平行于 bc 平面的中心对称分子组成。分子沿短 a 轴堆叠。该粉末图样已提交给 ICDD®，以便纳入粉末衍射文件™ (PDF®)。

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引用次数: 0

Experimental electron density distribution of KZnB3O6 constructed by maximum-entropy method 用最大熵法构建 KZnB3O6 的实验电子密度分布

IF 0.5 4区材料科学 Q4 MATERIALS SCIENCE, CHARACTERIZATION & TESTING

Powder Diffraction

Pub Date : 2024-02-08 DOI: 10.1017/s0885715623000428

Qi Li, Yi Huang, Yanfang Lou, Munan Hao, Shifeng Jin

The dynamic charge density of KZnB3O6, which contains edge-sharing BO4 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 B2O2 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 B2O2 ring. The experimental EDD of KZnB3O6 obtained aligns with the results obtained from ab-initio calculations. Our work underscores the importance of obtaining high-quality experimental data to accurately determine EDDs.

利用实验室和同步辐射 X 射线衍射技术对 KZnB3O6 的动态电荷密度进行了表征，KZnB3O6 包含边缘共享的 BO4 单元。室温单晶衍射数据和低温同步辐射粉末衍射数据都揭示了一个有趣的现象：边缘共享的 B2O2 环在 O 原子间表现出显著的电荷密度积累。对在 81 K 温度下采集的高质量单晶衍射数据（具有高分辨率和高信噪比）的进一步分析表明，B2O2 环内没有直接的 O-O 键。KZnB3O6 的实验 EDD 与原子模拟计算的结果一致。我们的工作强调了获得高质量实验数据对准确测定 EDD 的重要性。

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引用次数: 0

Adsorption of Ar into zeolite Al-MFI (NH4) 沸石 Al-MFI (NH4) 对 Ar 的吸附情况

IF 0.5 4区材料科学 Q4 MATERIALS SCIENCE, CHARACTERIZATION & TESTING

Powder Diffraction

Pub Date : 2024-02-08 DOI: 10.1017/s0885715623000453

Colin W. Scherry, James A. Kaduk, Winnie Wong-Ng, Huong Giang T. Nguyen

The crystal structure of anhydrous Al-MFI (NH4) containing adsorbed Ar has been determined and refined using synchrotron X-ray powder diffraction data taken at 90 K, and optimized using density functional theory techniques. Six highly occupied Ar sites almost completely fill the pore volume of the zeolite. Changing the gas flow from Ar to He at 90 K decreases the Ar occupancies of all six sites, but two decrease more than the others. Warming the sample from 90 to 295 K in Ar flow results in further decreases in site occupancies, but five of the original six sites persist.

我们利用同步辐射 X 射线粉末衍射数据测定并完善了含有吸附 Ar 的无水 Al-MFI (NH4) 的晶体结构，并利用密度泛函理论技术对其进行了优化。六个高度占据的 Ar 位点几乎完全填满了沸石的孔隙。在开氏 90 度时，将气流从氩气改为氦气，会降低所有六个位点的氩气占有率，但其中两个位点的降低幅度更大。将样品在氩气流中的温度从 90 K 升至 295 K 会导致位点占有率进一步降低，但原来六个位点中的五个仍然存在。

引用次数: 0

X-ray powder diffraction data for three new compounds obtained as a result of CO2 capture 由于CO2捕获而获得的三种新化合物的x射线粉末衍射数据

IF 0.5 4区材料科学 Q4 MATERIALS SCIENCE, CHARACTERIZATION & TESTING

Powder Diffraction

Pub Date : 2023-11-23 DOI: 10.1017/s0885715623000404

Klaudia Nowakowska, Wiesław Łasocha

The field of research related to CO2 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-propCO2 (C4H10N2O2) [a = 9.3033(7), b = 9.2485(7), c = 7.4735(7) Å, β = 111.214(7)°, V = 599.46 Å3, Z = 4, space group Ia]; 13-propCO2 (C4H10N2O2) [a = 5.0065(10), b = 12.2093(23), c = 4.9006(10) Å, β = 96.457(18)°, V = 297.65 Å3, Z = 2, space group P21]; and 13-dytekCO2 (C6H14N2O2) [a = 28.374(3), c = 5.1726(9) Å, V = 3606.53 Å3, Z = 18, space group

$Rbar{3}$

] are reported in this paper.

与二氧化碳捕获相关的研究领域对于可持续的绿色化学来说是非常重要和有吸引力的。在我们的研究中对这一主题的关注导致了以二胺为基础的新化合物的获得。由于二胺的水溶液暴露在空气中二氧化碳的缓慢作用下进行合成，得到了三种新的单氨基甲酸酯。所得化合物的x射线粉末衍射数据:12-propCO2 (C4H10N2O2) [a = 9.3033(7)， b = 9.2485(7)， c = 7.4735(7) Å， β = 111.214(7)°，V = 599.46 Å3, Z = 4，空间群Ia];13- proco2 (C4H10N2O2) [a = 5.0065(10)， b = 12.2093(23)， c = 4.9006(10) Å， β = 96.457(18)°，V = 297.65 Å3, Z = 2，空间群P21];和13-dytekCO2 (C6H14N2O2) [a = 28.374(3)， c = 5.1726(9) Å， V = 3606.53 Å3, Z = 18，空间群$Rbar{3}$]。

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引用次数: 0

Crystal structure and X-ray powder diffraction data for Lumateperone tosylate 甲磺酸Lumateperone的晶体结构和x射线粉末衍射数据

4区材料科学 Q4 MATERIALS SCIENCE, CHARACTERIZATION & TESTING

Powder Diffraction

Pub Date : 2023-10-27 DOI: 10.1017/s0885715623000337

Jiyong Liu, Dier Shi, Shuna Liu, Xiurong Hu

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).

本文报道了甲磺酸Lumateperone tosylate的x射线粉末衍射数据、单位胞参数和空间群[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，空间群C 2]。在每种情况下，所有测量线都被索引，并与相应的空间组一致。本文还报道了甲磺酸Lumateperone tosylate的单晶数据，分别为[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，空间群c 2]。实验粉末衍射图与单晶数据模拟得到的衍射图匹配良好，取向在[002]方向(取向系数= 0.75)。

引用次数: 0

Synthesis, powder diffraction pattern, crystal structure determination of the pharmaceutical co-crystal of levetiracetam and 3,5-dinitrosalicylic acid 左乙拉西坦与3,5-二硝基水杨酸药用共晶的合成、粉末衍射模式及晶体结构测定

4区材料科学 Q4 MATERIALS SCIENCE, CHARACTERIZATION & TESTING

Powder Diffraction

Pub Date : 2023-10-16 DOI: 10.1017/s0885715623000374

Lingling Shi, Zhengguo Chen, Hany Kafafy, Zhaoxia Zhang, Guocheng Zhu, Juming Yao, Guoqing Zhang

( S )-α-Ethyl-2-oxo-1-pyrrolidineacetamide (trade name levetiracetam), a derivative of piracetam, is used clinically as an add-on treatment for partial-onset seizures. In this study, we report the solid-state structure of a new drug co-crystal produced from levetiracetam and 3,5-dinitrosalicylic acid through cooling crystallization. This compound was further characterized by infrared spectroscopy, powder X-ray diffraction, and single-crystal X-ray diffraction. The new co-crystals show a 1:1 stoichiometry and crystallize in the monoclinic system, space group P 2 1 , with cell parameters: a = 9.7709(3) Å, b = 6.2202(2) Å, c = 14.7280(4) Å, α = 90°, β = 96.0340(10)°, γ = 90°, V = 890.16(5) Å 3 , and Z = 2. It is identified that hydrogen bonds are the main interactions between levetiracetam and 3,5-dinitrosalicylic acid, and the contribution of each hydrogen bond in maintaining the stability of the crystal structure was also quantified using Hirshfeld surface analysis.

(S)-α-乙基-2-氧-1-吡咯烷乙酰胺(商品名左乙拉西坦)是吡拉西坦的衍生物，临床上用作部分发作性癫痫的附加治疗。本文报道了以左乙拉西坦和3,5-二硝基水杨酸为原料，通过冷却结晶法制备的新型药物共晶的固态结构。通过红外光谱、粉末x射线衍射和单晶x射线衍射对该化合物进行了进一步的表征。新共晶呈1:1的化学配比，在单斜晶系p21空间群中结晶，晶胞参数为:a = 9.7709(3) Å， b = 6.2202(2) Å， c = 14.7280(4) Å， α = 90°，β = 96.0340(10)°，γ = 90°，V = 890.16(5) Å 3, Z = 2。发现氢键是左乙乙胺与3,5-二硝基水杨酸之间的主要相互作用，并利用Hirshfeld表面分析定量了每个氢键对维持晶体结构稳定性的贡献。

引用次数: 0

Long-term benefit after allergen immunotherapy to HDM in elderly patients with allergic rhinitis. 过敏原免疫治疗老年变应性鼻炎患者HDM的远期疗效。

4区材料科学 Q4 MATERIALS SCIENCE, CHARACTERIZATION & TESTING

Powder Diffraction

Pub Date : 2023-10-01 Epub Date: 2023-07-19 DOI: 10.5114/ada.2023.129942

Andrzej Bożek, Agnieszka Bogacz-Piaseczyńska, Martyna Miodońska, Dominika Sadowska

Introduction: Allergen immunotherapy (AIT) is an effective therapy for allergic rhinitis and may have long-term benefits. However, these benefits have not been strictly defined for older people.

Aim: The evaluation of the effectiveness of AIT in patients over 60 with allergic rhinitis and house dust mites (HDM) allergy over a period of 7 years was performed.

Material and methods: Patients after three years of HDM-AIT were observed to assess the sustained clinical effect of treatment. The average adjusted symptom score (AAdSS) and sIgG4 were monitored for 7 years after sublingual (SLIT) and injection AIT (SCIT).

Results: After 3 years of HDM-AIT, a significant clinical effect was observed in the group after SLIT and SCIT based on AAdSS compared to the baseline and the placebo group (p < 0.05). After 7 years of follow-up, there was a sustained trend of decrease in clinical symptoms in desensitized patients relative to placebo. Serum sIgG4 was constantly present in all desensitized patients.

Conclusions: AIT may be beneficial for treating seniors with allergic rhinitis and allergies to house dust mites.

简介:过敏原免疫疗法(AIT)是一种有效的治疗变应性鼻炎，可能有长期的好处。然而，这些福利并没有严格规定给老年人。目的:评价AIT对60岁以上变应性鼻炎和屋尘螨(HDM)过敏患者7年的治疗效果。材料与方法:观察HDM-AIT治疗3年后的患者，评估治疗的持续临床效果。在舌下(SLIT)和注射AIT (SCIT)后监测7年的平均调整症状评分(AAdSS)和sIgG4。结果:HDM-AIT治疗3年后，基于AAdSS的SLIT组和SCIT组与基线组和安慰剂组比较，临床疗效显著(p < 0.05)。经过7年的随访，与安慰剂相比，脱敏患者的临床症状有持续下降的趋势。所有脱敏患者血清sIgG4均持续存在。结论:AIT对老年人变应性鼻炎和屋尘螨过敏有一定的治疗作用。

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