Pub Date : 2022-09-13DOI: 10.1017/S0885715622000380
Analio Dugarte-Dugarte, R. Toro, J. van de Streek, J. Henao, G. C. Diaz de Delgado, J. M. Delgado
The previously unreported crystal structure of (S)-Dapoxetine hydrochloride (DAPHCl), the only active pharmaceutical ingredient specially developed for the treatment of premature ejaculation in men, has been determined from laboratory X-ray powder diffraction data with DASH and refined by the Rietveld method with TOPAS-Academic. The structure was evaluated and optimized by dispersion-corrected DFT calculations. This compound crystallizes in an orthorhombic cell, space group P212121, with unit-cell parameters a= 6.3208(3) Å, b = 10.6681(5) Å, c = 28.1754(10) Å, V = 1899.89(14) Å3, Z = 4. The refinement converged to Rp = 0.0442, Rwp = 0.0577, and GoF = 2.440. The crystal structure is a complex 3D arrangement of DAPHCl moieties held together by hydrogen bonds, π⋯π, and C–H⋯π interactions. The chloride ions form layers parallel to the ab plane and are connected by dapoxetinium moieties through N–H⋯Cl and C–H⋯Cl hydrogen bonds. These layers stack along the c-axis, which are connected by C–H⋯π interactions. Hirshfeld surface analysis and fingerprint plot calculations have been performed.
{"title":"Crystal structure from laboratory X-ray powder diffraction data, DFT-D calculations, and Hirshfeld surface analysis of (S)-dapoxetine hydrochloride","authors":"Analio Dugarte-Dugarte, R. Toro, J. van de Streek, J. Henao, G. C. Diaz de Delgado, J. M. Delgado","doi":"10.1017/S0885715622000380","DOIUrl":"https://doi.org/10.1017/S0885715622000380","url":null,"abstract":"The previously unreported crystal structure of (S)-Dapoxetine hydrochloride (DAPHCl), the only active pharmaceutical ingredient specially developed for the treatment of premature ejaculation in men, has been determined from laboratory X-ray powder diffraction data with DASH and refined by the Rietveld method with TOPAS-Academic. The structure was evaluated and optimized by dispersion-corrected DFT calculations. This compound crystallizes in an orthorhombic cell, space group P212121, with unit-cell parameters a= 6.3208(3) Å, b = 10.6681(5) Å, c = 28.1754(10) Å, V = 1899.89(14) Å3, Z = 4. The refinement converged to Rp = 0.0442, Rwp = 0.0577, and GoF = 2.440. The crystal structure is a complex 3D arrangement of DAPHCl moieties held together by hydrogen bonds, π⋯π, and C–H⋯π interactions. The chloride ions form layers parallel to the ab plane and are connected by dapoxetinium moieties through N–H⋯Cl and C–H⋯Cl hydrogen bonds. These layers stack along the c-axis, which are connected by C–H⋯π interactions. Hirshfeld surface analysis and fingerprint plot calculations have been performed.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2022-09-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41756134","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 : 2022-09-09DOI: 10.1017/S0885715622000331
J. Kaduk, A. Gindhart, S. Gates-Rector, T. Blanton
The crystal structure of altrenogest has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Altrenogest crystallizes in space group P212121 (#19) with a = 7.286 916(16), b = 10.580 333(19), c = 22.266 08(7) Å, V = 1716.671(6) Å3, and Z = 4 at 295 K. Thermal expansion between 113 and 295 K is anisotropic. An O–H⋯O hydrogen bond links the molecules into chains along the c-axis. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).
{"title":"Powder X-ray diffraction of altrenogest, C21H26O2","authors":"J. Kaduk, A. Gindhart, S. Gates-Rector, T. Blanton","doi":"10.1017/S0885715622000331","DOIUrl":"https://doi.org/10.1017/S0885715622000331","url":null,"abstract":"The crystal structure of altrenogest has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Altrenogest crystallizes in space group P212121 (#19) with a = 7.286 916(16), b = 10.580 333(19), c = 22.266 08(7) Å, V = 1716.671(6) Å3, and Z = 4 at 295 K. Thermal expansion between 113 and 295 K is anisotropic. An O–H⋯O hydrogen bond links the molecules into chains along the c-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":"2022-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45045706","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 : 2022-09-09DOI: 10.1017/S0885715622000343
J. Kaduk, A. Gindhart, S. Gates-Rector, T. Blanton
The crystal structure of aminopentamide hydrogen sulfate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Aminopentamide hydrogen sulfate crystallizes in space group P21/c (#14) with a = 17.62255(14), b = 6.35534(4), c = 17.82499(10) Å, β = 96.4005(6)°, V = 1983.906(14) Å3, and Z = 4. The structure consists of layers parallel to the bc-plane with hydrogen sulfate anions at the core and aminopentamide cations on the outside. There is a strong charge-assisted O49–H53⋯O52 hydrogen bond between the hydrogen sulfate anions. This hydrogen bond links the anions in a chain parallel to the b-axis. The cation forms a discrete N–H⋯O hydrogen bond to the anion. The amide group also forms two weaker discrete hydrogen bonds to the anion. The three N–H⋯O hydrogen bonds link the cations and anions into columns parallel to the b-axis. This commercial material from USP contained an unidentified impurity, the powder pattern of which could be indexed on a monoclinic unit cell. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).
{"title":"Crystal structure of aminopentamide hydrogen sulfate, (C19H25N2O)(HSO4)","authors":"J. Kaduk, A. Gindhart, S. Gates-Rector, T. Blanton","doi":"10.1017/S0885715622000343","DOIUrl":"https://doi.org/10.1017/S0885715622000343","url":null,"abstract":"The crystal structure of aminopentamide hydrogen sulfate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Aminopentamide hydrogen sulfate crystallizes in space group P21/c (#14) with a = 17.62255(14), b = 6.35534(4), c = 17.82499(10) Å, β = 96.4005(6)°, V = 1983.906(14) Å3, and Z = 4. The structure consists of layers parallel to the bc-plane with hydrogen sulfate anions at the core and aminopentamide cations on the outside. There is a strong charge-assisted O49–H53⋯O52 hydrogen bond between the hydrogen sulfate anions. This hydrogen bond links the anions in a chain parallel to the b-axis. The cation forms a discrete N–H⋯O hydrogen bond to the anion. The amide group also forms two weaker discrete hydrogen bonds to the anion. The three N–H⋯O hydrogen bonds link the cations and anions into columns parallel to the b-axis. This commercial material from USP contained an unidentified impurity, the powder pattern of which could be indexed on a monoclinic unit cell. 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":"2022-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42555122","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 : 2022-09-01DOI: 10.1017/s088571562200032x
Gang Wang
{"title":"Calendar of short courses and workshops","authors":"Gang Wang","doi":"10.1017/s088571562200032x","DOIUrl":"https://doi.org/10.1017/s088571562200032x","url":null,"abstract":"","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2022-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"57032417","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 : 2022-09-01DOI: 10.1017/S0885715622000355
On the Cover: In the manuscript ” Crystal Morphology Prediction and Experimental Veri fi cation of Venlafaxine Hydrochloride ” by C. Liang, et al , it was shown that modeling can be successfully used to predict the in fl uence of solvent effects on crystal habit of venlafaxine hydrochloride. Modeling of habit of the precipitates was based on the modi fi ed attachment energy model using molecular dynamics simulation and was supported by showing the differences in the X-ray powder diffraction patterns of the three precipitates compared with the calculated pattern. Further, physical properties of the precipitates from the three solvents were shown to be related with the morphologies of the crystals.
{"title":"PDJ volume 37 issue 3 Cover and Front matter","authors":"","doi":"10.1017/S0885715622000355","DOIUrl":"https://doi.org/10.1017/S0885715622000355","url":null,"abstract":"On the Cover: In the manuscript ” Crystal Morphology Prediction and Experimental Veri fi cation of Venlafaxine Hydrochloride ” by C. Liang, et al , it was shown that modeling can be successfully used to predict the in fl uence of solvent effects on crystal habit of venlafaxine hydrochloride. Modeling of habit of the precipitates was based on the modi fi ed attachment energy model using molecular dynamics simulation and was supported by showing the differences in the X-ray powder diffraction patterns of the three precipitates compared with the calculated pattern. Further, physical properties of the precipitates from the three solvents were shown to be related with the morphologies of the crystals.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2022-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43667756","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 : 2022-09-01DOI: 10.1017/S0885715622000276
S. Bourne
The first Pan-African Conference on Crystallography, PCCr1, was held in Dschang, Cameroon in 2016. This highly successful meeting attracted 192 participants from 32 countries, including 20 African countries. PCCr2 followed in 2019, with over 200 participants from 35 countries. This was a joint meeting with AfLS and was hosted in Accra, Ghana. PPCCr3 was scheduled to take place in Nairobi, Kenya in 2021. Unfortunately, due to the pandemic, this meeting had to be postponed. The Steering Committee of the African Crystallographic Association, along with the Local Organizing Committee of PCCr3, decided to hold an online meeting in order to continue the momentum and sense of community generated during the first two PCCr meetings. ePCCr was, therefore, organized.
{"title":"ePCCr: an online conference organized jointly with the African Light Source and the African Physical Society","authors":"S. Bourne","doi":"10.1017/S0885715622000276","DOIUrl":"https://doi.org/10.1017/S0885715622000276","url":null,"abstract":"The first Pan-African Conference on Crystallography, PCCr1, was held in Dschang, Cameroon in 2016. This highly successful meeting attracted 192 participants from 32 countries, including 20 African countries. PCCr2 followed in 2019, with over 200 participants from 35 countries. This was a joint meeting with AfLS and was hosted in Accra, Ghana. PPCCr3 was scheduled to take place in Nairobi, Kenya in 2021. Unfortunately, due to the pandemic, this meeting had to be postponed. The Steering Committee of the African Crystallographic Association, along with the Local Organizing Committee of PCCr3, decided to hold an online meeting in order to continue the momentum and sense of community generated during the first two PCCr meetings. ePCCr was, therefore, organized.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2022-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41879536","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 : 2022-09-01DOI: 10.1017/s0885715622000306
C. Hubbard
{"title":"Recent readership and impact metrics for the Journal Powder Diffraction (PDJ)","authors":"C. Hubbard","doi":"10.1017/s0885715622000306","DOIUrl":"https://doi.org/10.1017/s0885715622000306","url":null,"abstract":"","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2022-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49483744","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 : 2022-08-31DOI: 10.1017/S0885715622000288
J. Kaduk
The crystal structure of anhydrous alfuzosin hydrochloride has been solved and refined using laboratory X-ray powder diffraction data and optimized using density functional theory techniques. Anhydrous alfuzosin hydrochloride crystallizes in space group P-1 with a = 9.3214(16), b = 9.3997(29), c = 12.6172(64) Å, α = 107.993(11), β = 100.386(9), γ = 90.229(6)°, V = 1032.1(10) Å3, and Z = 2 at ambient conditions. Thermal expansion is anisotropic, being 8× larger in the c-direction than in the other two. The crystal structure is characterized by a stack of planar fused rings along the b-axis, and layers of the more-corrugated portion of the molecule parallel to the ab-plane. There are two strong N–H⋯Cl hydrogen bonds, as well as seven C-H⋯Cl hydrogen bonds. The powder patterns have been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).
{"title":"Crystal structure of alfuzosin hydrochloride, C19H28N5O4Cl","authors":"J. Kaduk","doi":"10.1017/S0885715622000288","DOIUrl":"https://doi.org/10.1017/S0885715622000288","url":null,"abstract":"The crystal structure of anhydrous alfuzosin hydrochloride has been solved and refined using laboratory X-ray powder diffraction data and optimized using density functional theory techniques. Anhydrous alfuzosin hydrochloride crystallizes in space group P-1 with a = 9.3214(16), b = 9.3997(29), c = 12.6172(64) Å, α = 107.993(11), β = 100.386(9), γ = 90.229(6)°, V = 1032.1(10) Å3, and Z = 2 at ambient conditions. Thermal expansion is anisotropic, being 8× larger in the c-direction than in the other two. The crystal structure is characterized by a stack of planar fused rings along the b-axis, and layers of the more-corrugated portion of the molecule parallel to the ab-plane. There are two strong N–H⋯Cl hydrogen bonds, as well as seven C-H⋯Cl hydrogen bonds. The powder patterns have 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":"2022-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49635517","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 : 2022-08-30DOI: 10.1017/S088571562200029X
Dier Shi, Jiyong Liu, Xiurong Hu
X-ray powder diffraction data, unit-cell parameters, and space group for the topiroxostat form II, C13H8N6, are reported [a = 7.344(9) Å, b = 12.946(7) Å, c = 12.133(5) Å, β = 96.99(3)°, V = 1145.2(4) Å3, Z = 4, and space group P21/c]. The topiroxostat monohydrate, C13H8N6·H2O, crystallized in a triclinic system and unit-cell parameters are also reported [a = 7.422(9) Å, b = 8.552(1) Å, c = 11.193(5) Å, α = 74.85(1)°, β = 81.17(1)°, γ = 66.29(1)°, V = 627.0(6) Å3, Z = 2, and space group P-1]. In each case, all measured lines were indexed and are consistent with the corresponding space group. The single-crystal data of two solid-state forms of topiroxostat are also reported, respectively [a = 7.346(2) Å, b = 12.955(2) Å, c = 12.130(7) Å, β = 96.91(6)°, V = 1146.1(3) Å3, Z = 4, and space group P21/c] and [a = 7.418(6) Å, b = 8.532(8) Å, c = 11.183(9) Å, α = 74.807(1) °, β = 81.13(1)°, γ = 66.32(1) °, V = 624.7(6) Å3, Z = 2, and space group P-1]. The experimental powder diffraction pattern has been well matched with the simulated pattern derived from the single-crystal data.
本文报道了topiroxostat form II, C13H8N6的x射线粉末衍射数据、单胞参数和空间群[a = 7.344(9) Å， b = 12.946(7) Å， c = 12.133(5) Å， β = 96.99(3)°，V = 1145.2(4) Å3, Z = 4，空间群P21/c]。托吡司他一水合物C13H8N6·H2O在三斜体系中结晶，单位胞参数也被报道[a = 7.422(9) Å， b = 8.552(1) Å， c = 11.193(5) Å， α = 74.85(1)°，β = 81.17(1)°，γ = 66.29(1)°，V = 627.0(6) Å3, Z = 2，空间群P-1]。在每种情况下，所有测量线都被索引，并且与相应的空间组一致。本文还报道了两种固态形态topiroxostat的单晶数据，分别为[a = 7.346(2) Å， b = 12.955(2) Å， c = 12.130(7) Å， β = 96.91(6)°，V = 1146.1(3) Å3, Z = 4，空间群P21/c]和[a = 7.418(6) Å， b = 8.532(8) Å， c = 11.183(9) Å， α = 74.807(1)°，β = 81.13(1)°，γ = 66.32(1)°，V = 624.7(6) Å3, Z = 2，空间群P-1]。实验所得的粉末衍射图与模拟所得的单晶衍射图吻合较好。
{"title":"Crystal structure and X-ray powder diffraction data for two solid-state forms of topiroxostat","authors":"Dier Shi, Jiyong Liu, Xiurong Hu","doi":"10.1017/S088571562200029X","DOIUrl":"https://doi.org/10.1017/S088571562200029X","url":null,"abstract":"X-ray powder diffraction data, unit-cell parameters, and space group for the topiroxostat form II, C13H8N6, are reported [a = 7.344(9) Å, b = 12.946(7) Å, c = 12.133(5) Å, β = 96.99(3)°, V = 1145.2(4) Å3, Z = 4, and space group P21/c]. The topiroxostat monohydrate, C13H8N6·H2O, crystallized in a triclinic system and unit-cell parameters are also reported [a = 7.422(9) Å, b = 8.552(1) Å, c = 11.193(5) Å, α = 74.85(1)°, β = 81.17(1)°, γ = 66.29(1)°, V = 627.0(6) Å3, Z = 2, and space group P-1]. In each case, all measured lines were indexed and are consistent with the corresponding space group. The single-crystal data of two solid-state forms of topiroxostat are also reported, respectively [a = 7.346(2) Å, b = 12.955(2) Å, c = 12.130(7) Å, β = 96.91(6)°, V = 1146.1(3) Å3, Z = 4, and space group P21/c] and [a = 7.418(6) Å, b = 8.532(8) Å, c = 11.183(9) Å, α = 74.807(1) °, β = 81.13(1)°, γ = 66.32(1) °, V = 624.7(6) Å3, Z = 2, and space group P-1]. The experimental powder diffraction pattern has been well matched with the simulated pattern derived from the single-crystal data.","PeriodicalId":20333,"journal":{"name":"Powder Diffraction","volume":null,"pages":null},"PeriodicalIF":0.5,"publicationDate":"2022-08-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46811920","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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