Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials最新文献_第8页

Crystal engineering of co-crystal of nicotinic acid and pyrogallol: an experimental and theoretical electron density analysis 烟酸与邻苯三酚共晶的晶体工程:实验与理论的电子密度分析

Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials Pub Date : 2021-11-23 DOI: 10.1107/s2052520621009124

Alia Iqbal, A. Mehmood, S. Noureen, C. Lecomte, Maqsood Ahmed

{"title":"Crystal engineering of co-crystal of nicotinic acid and pyrogallol: an experimental and theoretical electron density analysis","authors":"Alia Iqbal, A. Mehmood, S. Noureen, C. Lecomte, Maqsood Ahmed","doi":"10.1107/s2052520621009124","DOIUrl":"https://doi.org/10.1107/s2052520621009124","url":null,"abstract":"Experimental electron density analysis by means of high-resolution X-ray diffraction data up to sinθ/λmax = 1.11 Å−1 at 100 (1) K has been performed to analyze the detailed structure and the strength of intermolecular interactions responsible for the formation of a new solid form of nicotinic acid (NA), cocrystallized with pyrogallol (PY). There are two NA–PY units in the asymmetric unit. The experimental results are compared with the results obtained from theoretical structure factors modeled using periodic boundary DFT calculations. Both refinements were carried out using the Hansen and Coppens multipolar formalism (in MoPro program). The non-centrosymmetric and polar nature of the crystal system rendered the multipolar refinement challenging which was addressed by involving the transferability principle. This study highlights the significance of the transferability principle in electron density modeling in non-routine situations. The 2:2 cocrystal of NA–PY exhibits a zigzag, brickwall and sheet-like layered structure in three dimensions and is stabilized by strong intra- and inter-molecular hydrogen bonding through N—H...O and O—H...O bonds, some of them due to the zwitterion nature of NA as well as weak interactions between the PY molecules. Ranking these interactions via topological analysis of the electron density shows the leading role of the NA–NA substructure which drives the organization of the cocrystals. These strong interactions between the NA zwitterions may explain why Z′ = 2.","PeriodicalId":7080,"journal":{"name":"Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials","volume":"1974 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90240379","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Low-temperature phase transition and highpressure phase stability of 1H-pyrazole-1carboxamidine nitrate 1h -吡唑-1硝酸钾胺的低温相变和高压相稳定性

Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials Pub Date : 2021-11-20 DOI: 10.1107/s2052520621010970

Piotr Rejnhardt, M. Drozd, M. Daszkiewicz

{"title":"Low-temperature phase transition and highpressure phase stability of 1H-pyrazole-1carboxamidine nitrate","authors":"Piotr Rejnhardt, M. Drozd, M. Daszkiewicz","doi":"10.1107/s2052520621010970","DOIUrl":"https://doi.org/10.1107/s2052520621010970","url":null,"abstract":"The phase transition observed in a temperature-dependent experiment at 174 K is unachievable under high-pressure conditions. Negative thermal expansion for phase (II) and negative compressibility for phase (I) were observed. A new salt of 1H-pyrazole-1-carboxamidine, (HPyCA)NO3, for guanylation reaction was obtained in a crystalline form. The compound crystallizes in monoclinic space group P21/c and a phase transition at 174 K to triclinic modification P\u0000 1 was found. An unusual increase of the unit-cell volume was observed just after transition. Although the volume decreases upon cooling, it remains higher down to 160 K in comparison to the unit-cell volume of phase (I). The mechanism of the phase transition is connected with a minor movement of the nitrate anions. The triclinic phase was unreachable at room-temperature high-pressure conditions up to 1.27 GPa. On further compression, delamination of the crystal was observed. Phase (I) exhibits negative linear compressibility, whereas abnormal behaviour of the b unit-cell parameter upon cooling was observed, indicating negative thermal linear expansion. The unusual nature of the compound is associated with the two-dimensional hydrogen-bonding network, which is less susceptible to deformation than stacking interactions connecting the layers of hydrogen bonds. Infrared spectroscopy and differential scanning calorimetry measurements were used to investigate the changes of intermolecular interactions during the phase transition.","PeriodicalId":7080,"journal":{"name":"Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-11-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86744276","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Structures and phase transitions in barium sodium niobate tungsten bronze (BNN) 铌酸钡钠钨青铜(BNN)的结构与相变

Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials Pub Date : 2021-11-19 DOI: 10.1107/s2052520621010301

Thomas A. Whittle, C. Howard, S. Schmid

引用次数: 1

A previously unknown cyclic alkanolamine and molecular ranking using the pair distribution function 一个以前未知的环烷醇胺和分子排序使用对分布函数

Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials Pub Date : 2021-11-17 DOI: 10.1107/S2052520621010088

Gianpiero Gallo, M. Terban, I. Moudrakovski, T. Huber, M. Etter, M. Ernst, B. Hinrichsen, R. Dinnebier

引用次数: 0

Can the results of quantum refinement be improved with a continuum-solvation model? 用连续溶剂化模型可以改进量子精化的结果吗?

Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials Pub Date : 2021-11-17 DOI: 10.1107/S2052520621009574

J. Bergmann, E. Oksanen, U. Ryde

引用次数: 0

Investigation of polar crystalline materials containing hydrochlorothiazide: electron density distribution and optical properties 含氢氯噻嗪极性晶体材料的研究:电子密度分布和光学性质

Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials Pub Date : 2021-11-15 DOI: 10.1107/s2052520621009914

J. Wojnarska, M. Gryl, T. Seidler, K. Stadnicka

{"title":"Investigation of polar crystalline materials containing hydrochlorothiazide: electron density distribution and optical properties","authors":"J. Wojnarska, M. Gryl, T. Seidler, K. Stadnicka","doi":"10.1107/s2052520621009914","DOIUrl":"https://doi.org/10.1107/s2052520621009914","url":null,"abstract":"The polar hydrochlorothiazide polymorph (I) (systematic name: 6-chloro-1,1-dioxo-3,4-dihydro-2H-1,2,4-benzothiadiazine-7-sulfonamide, C7H8ClN3O4S2) and, recently designed by us, the polar 2-aminopyridine hydrochlorothiazide water <1/1/1> (C7H8ClN3O4S2·C5H6N2·H2O), (II), have been investigated. The crystal structures of both materials were determined using the single-crystal X-ray diffraction technique. The intermolecular interactions in (I) and (II) were studied in detail via topological electron-density analysis. The obtained results showed hydrogen bonds with a character intermediate between closed-shell and shared-shell in both crystal structures. The most important hydrogen bonds in (I) are formed between sulfonamide groups, whereas in (II), water molecules play a crucial role as they interconnect 2-aminopyridine and hydrochlorothiazide molecules. Calculations of the optical properties revealed that both materials exhibit large linear birefringence, twice that of calcite. The theoretically predicted second harmonic generation efficiency is four times and five times larger than that of KH2PO4 for (I) and (II), respectively. The information gathered on intermolecular interactions and structure–property correlations was used to identify the best strategies for the future design of new functional materials of this kind.","PeriodicalId":7080,"journal":{"name":"Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials","volume":"5 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-11-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75556003","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Strategic synthon approach in obtaining cocrystals and cocrystal polymorphs of a high-Z′ system deferiprone – an anti-thalassemia drug 获得抗地中海贫血药物高z′系统去铁蛋白共晶和共晶多晶的策略合成方法

Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials Pub Date : 2021-11-12 DOI: 10.1107/s205252062100980x

Satyasree Rajendrakumar, Anuja Surampudi Venkata Sai Durga, S. Balasubramanian

{"title":"Strategic synthon approach in obtaining cocrystals and cocrystal polymorphs of a high-Z′ system deferiprone – an anti-thalassemia drug","authors":"Satyasree Rajendrakumar, Anuja Surampudi Venkata Sai Durga, S. Balasubramanian","doi":"10.1107/s205252062100980x","DOIUrl":"https://doi.org/10.1107/s205252062100980x","url":null,"abstract":"Compounds with more than one molecule in the crystallographic asymmetric unit (Z′ > 1) display a noticeably stronger propensity to form cocrystals. Deferiprone is an anti-thalassemia drug known to exhibit polymorphic behaviour. Previously, three polymorphs were reported out of which one of them exhibited Z′ > 1. In the present manuscript, a fourth polymorph of deferiprone was identified and it also possessed Z′ > 1. All the four polymorphs showed similar hydrogen bonding features and differed in crystal packing. The ability of deferiprone to crystallize as Z′ > 1 prompted us to investigate the hydrogen bonding and synthon variation upon cocrystallization of deferiprone with hydroxyl-group-containing coformers such as catechol, hydroquinone, phloroglucinol, resorcinol and pyrogallol. Crystallization attempts along with PXRD analysis aided in obtaining 11 new cocrystal structures which involve different stoichiometric cocrystals and some polymorphs. Synthon analysis, crystal packing as well as thermal behaviour were assessed and compared. The presence of multiple phases in each cocrystal system in its respective bulk powders was identified and quantified using PXRD and Rietveld analysis. Homosynthons were observed in three co-crystal systems, while a heterosynthon was observed in five systems. The combination of both homo- and heterosynthon was observed in three cocrystal systems. The phase transformation events were observed in most of the systems. In nine co-crystal systems, the melting points were observed intermediate between those of the API and the coformers.","PeriodicalId":7080,"journal":{"name":"Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials","volume":"177 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-11-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85037180","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 1

On the transfer of theoretical multipole parameters for restoring static electron density and revealing and treating atomic anharmonic motion. Features of chemical bonding in crystals of an isocyanuric acid derivative 恢复静态电子密度和揭示和处理原子非简谐运动的理论多极参数的传递。异氰尿酸衍生物晶体中化学键的特征

Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials Pub Date : 2021-11-10 DOI: 10.1107/s2052520621009690

S. A. Shteingolts, J. Voronina, L. Saifina, M. Shulaeva, V. Semenov, R. Fayzullin

{"title":"On the transfer of theoretical multipole parameters for restoring static electron density and revealing and treating atomic anharmonic motion. Features of chemical bonding in crystals of an isocyanuric acid derivative","authors":"S. A. Shteingolts, J. Voronina, L. Saifina, M. Shulaeva, V. Semenov, R. Fayzullin","doi":"10.1107/s2052520621009690","DOIUrl":"https://doi.org/10.1107/s2052520621009690","url":null,"abstract":"The crystal and electronic structure of an isocyanuric acid derivative was studied by high-resolution single-crystal X-ray diffraction within the Hansen–Coppens multipole formalism. The observed deformation electron density shows signs of thermal smearing. The experimental picture meaningfully assigned to the consequences of unmodelled anharmonic atomic motion. Straightforward simultaneous refinement of all parameters, including Gram–Charlier coefficients, resulted in more significant distortion of apparent static electron density, even though the residual density became significantly flatter and more featureless. Further, the method of transferring multipole parameters from the model refined against theoretical structure factors as an initial guess was employed, followed by the subsequent block refinement of Gram–Charlier coefficients and the other parameters. This procedure allowed us to appropriately distinguish static electron density from the contaminant smearing effects of insufficiently accounted atomic motion. In particular, some covalent bonds and the weak π...π interaction between isocyanurate moieties were studied via the mutual penetration of atomic-like kinetic and electrostatic potential φ-basins with complementary atomic ρ-basins. Further, local electronic temperature was applied as an advanced descriptor for both covalent bonds and noncovalent interactions. Total probability density function (PDF) of nuclear displacement showed virtually no negative regions close to and around the atomic nuclei. The distribution of anharmonic PDF to a certain extent matched the residual electron density from the multipole model before anharmonic refinement. No signs of disordering of the sulfonyl group hidden in the modelled anharmonic motion were found in the PDF.","PeriodicalId":7080,"journal":{"name":"Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials","volume":"338 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82900398","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 2

Interpreting the different emissive properties of cyclic triimidazole-based CuI and AgI coordination polymers: a QTAIM and IQA study 环三咪唑基CuI和AgI配位聚合物的不同发射性质:QTAIM和IQA研究

Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials Pub Date : 2021-11-05 DOI: 10.1107/S2052520621009707

A. Forni, E. Cariati, L. Carlucci, E. Lucenti, D. Marinotto, S. Pieraccini, M. Sironi

引用次数: 2

Crystal structure of the high-P polymorph of Ca2B6O6(OH)10·2(H2O) (meyerhofferite) Ca2B6O6(OH)10·2(H2O) (meyerhoferite)高磷晶型的晶体结构

Acta Crystallographica Section B Structural Science, Crystal Engineering and Materials Pub Date : 2021-11-05 DOI: 10.1107/s2052520621009768

D. Comboni, T. Porȩba, F. Pagliaro, Tommaso Battiston, P. Lotti, G. Gatta, G. Garbarino, M. Hanfland

引用次数: 2