Pub Date : 2024-03-01DOI: 10.1017/s0885715624000010
Pamela S. Whitfield, Zouina Karkar, Yaser Abu-Lebdeh
The title compound, 3-hydroxypropionitrile, was crystallized repeatedly in situ 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 gauche 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−1. 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.
利用液氮低温流在石英毛细管内反复原位结晶了标题化合物--3-羟基丙腈。所获得的 X 射线粉末衍射图样表明存在两种不同的结晶相。通过模拟退火法求解晶体结构，然后通过色散校正密度泛函理论（DFT）计算进行细化和优化，最后根据实验数据进行里特维尔德细化。这两种结构似乎与 20 世纪 60 年代一篇振动光谱学文献中提出的结构相对应，其中一种结构的分子构象更为稳定，而第二种结构的蜕变相则更为复杂，具有混合构象。使用从 84 K 数据集中获得的两种相的晶格参数进行色散校正的 DFT 计算表明，稳定相和蜕变相的能量相差不到 0.5 kJ mol-1。将 20 世纪 60 年代发表的实验远红外光谱与根据所提出的晶体结构计算得出的光谱进行比较，为所提出的结构提供了一些独立的支持证据。
{"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}
Pub Date : 2024-02-29DOI: 10.1017/s0885715624000071
James A. Kaduk, Megan M. Rost, Anja Dosen, Thomas N. Blanton
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 P-1 (#24) with a = 8.86616(9), b = 9.75866(21), c = 16.67848(36) Å, α = 102.6301(10), β = 94.1736(6), γ = 113.2644(2)°, V = 1273.095(7) Å3, and Z = 2 at 295 K. The crystal structure consists of layers of cations and anions parallel to the ab-plane. Traditional N–H⋯O and O–H⋯O hydrogen bonds link the cations and anions into chains along the a-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®).
{"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}
Pub Date : 2024-02-29DOI: 10.1017/s0885715624000058
W. Wong-Ng, J. Culp, J.A. Kaduk, Y.S. Chen, S. Lapidus
The structure of Ni(3-amino-4,4′-bipyridine)[Ni(CN)4] (or known as Ni-BpyNH2) in powder form was determined using synchrotron X-ray diffraction and refined using the Rietveld refinement technique (R = 8.8%). The orthorhombic (Cmca) cell parameters were determined to be a = 14.7218(3) Å, b = 22.6615(3) Å, c = 12.3833(3) Å, V = 4131.29(9) Å3, and Z = 8. Ni-BpyNH2 forms a 3-D network, with a 2-D Ni(CN)4 net connecting to each other via the BpyNH2 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)4 net is arranged in a wave-like fashion. The functional group, –NH2, is disordered and was found to be in the m-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 m-positions. The powder reference diffraction pattern for Ni-BpyNH2 was prepared and submitted to the Powder Diffraction File (PDF) at the International Centre of Diffraction Data (ICDD).
利用同步辐射 X 射线衍射法测定了粉末状 Ni（3-氨基-4,4′-联吡啶）[Ni(CN)4]（或称为 Ni-BpyNH2）的结构，并利用里特维尔德精炼技术（R = 8.8%）对其进行了精炼。Ni-BpyNH2 形成了一个三维网络，二维 Ni(CN)4 网通过 BpyNH2 配体相互连接。网络上有两个独立的 Ni 位点。二维网络通过吡啶 "N "原子与 Ni2 的结合相互连接。Ni2 位点与 N 具有六倍配位，与四倍配位的 Ni1-C 间距（平均 1.850 Å）相比，Ni2-N 间距相对较长（平均 2.118 Å）。Ni(CN)4 网呈波浪状排列。官能团 -NH2 是无序的，相对于吡啶环的 N 原子处于 m 位置。在四个 m 位中，N 原子不是处于唯一的位置，而是各占 1/4 个位点。Ni-BpyNH2 的粉末参考衍射图样已经制作完成，并提交给了国际衍射数据中心（ICDD）的粉末衍射文件（PDF）。
{"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}
Pub Date : 2024-02-29DOI: 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.
{"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 (<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}
Pub Date : 2024-02-29DOI: 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®).
{"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}
Pub Date : 2024-02-29DOI: 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®).
{"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}
Pub Date : 2024-02-19DOI: 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®)。
{"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}
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