Zeitschrift Fur Kristallographie-Crystalline Materials最新文献

{"title":"Crown ether complexes as a possible template for hybrid organic–inorganic borates","authors":"V. Yukhno, D. Charkin, A. Banaru, L. Manelis, A. Gosteva, S. Volkov, S. Aksenov, R. Bubnova","doi":"10.1515/zkri-2023-0020","DOIUrl":"https://doi.org/10.1515/zkri-2023-0020","url":null,"abstract":"Abstract Crystals of the first new organo–inorganic hybrid borate based on potassium crown ether complex, [K(C12H24O6)B5O6(OH)4](H2O) (1), have been produced from aqueous solutions and characterized by single-crystal X-ray diffraction. 1 crystalizes is orthorhombic system, Pnma, a = 10.1684(3) Å, b = 11.6289(3) Å, c = 21.2247(6) Å, V = 2509.76(12) Å3, Robs = 0.059. The structure of 1 consists of molecular [K(C12H24O6)B5O6(OH)4]0 complexes, common for crown ether complexes but yet not among borates, with a very rare monodentate coordination of the common pentaborate anion(1-). The molecular complexes are linked into weak chains via hydrogen bonding to outer-sphere water molecules. Hirshfeld surfaces analysis and complexity measurement of 1 were performed. Perspectives of borate structures containing crown ether complexes as templates are briefly outlined.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":" ","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-06-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49015084","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":"Structure determination through powder X-ray diffraction, Hirshfeld surface analysis, and DFT studies of 2- and 4-(methylthio)benzoic acid","authors":"P. Chatterjee","doi":"10.1515/zkri-2022-0069","DOIUrl":"https://doi.org/10.1515/zkri-2022-0069","url":null,"abstract":"Abstract 2-(methylthio)benzoic acid (1) is an ortho-substituted benzoic acid derivative, whereas 4-(methylthio)benzoic acid (2) is a para-substituted benzoic acid derivative. The structural analysis of both compounds was carried out using PXRD data. 2-(methylthio)benzoic acid shows a triclinic system with the P 1 ‾ $Poverline{1}$ space group, whereas 4-(methylthio)benzoic acid shows a monoclinic system and crystallizes in the P21/a space group. The strength, as well as relative contributions of intermolecular hydrogen bonds, have been examined through Hirshfeld surfaces as well as 2D fingerprint plots. A weak intramolecular hydrogen bond was found only in the case of ortho-substituted 2-(methylthio)benzoic acid. Supramolecular frameworks for 1 are formed by the interplay of intramolecular and intermolecular interactions, whereas for 2, intermolecular contacts form supramolecular assemblies. Intermolecular O–H⋯O interactions involving carboxyl groups form the R22(8) graph-set motif for both compounds. Theoretical DFT calculations using the B3LYP correlation functional reveal that the energy gap of HOMO–LUMO orbitals in compound 1, with the methylthio moiety in the ortho position relative to the carboxyl group, is lower than that of compound 2, with the methylthio moiety in the para position. Vertical and adiabatic ionization energies are also calculated for both compounds.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":" ","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-06-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46373201","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 9,10-bis-((perchloro-phenyl)-ethynyl)anthracene determined from three-dimensional electron diffraction data","authors":"T. Gorelik, Andreas Ulmer, A. Schleper, A. Kuehne","doi":"10.1515/zkri-2023-0009","DOIUrl":"https://doi.org/10.1515/zkri-2023-0009","url":null,"abstract":"Abstract The crystal structure of the title compound was determined using electron diffraction data collected in continuous rotation mode. The structure was successfully solved and refined kinematically in the monoclinic space group P21/c, with a Z value of 2 and Z′ value of 0.5. Within the crystal structure, the entire molecule is predominantly flat. The molecular packing exhibits a herringbone pattern, distinct from that of the unchlorinated analogue molecule. The largest facet of the crystals, which faces the supporting carbon film, is designated as (01‾1‾$bar{1}bar{1}$).","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":" ","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47514916","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":"Structural basis for fluorine substitution on a new naphthalene–chalcone analog","authors":"L. Sallum, L. Silva, J. E. Queiroz, Vitor Duarte, Wesley F. Vaz, M. Hernandes, G. Aquino, A. Camargo, H. Napolitano","doi":"10.1515/zkri-2022-0066","DOIUrl":"https://doi.org/10.1515/zkri-2022-0066","url":null,"abstract":"Abstract Fluorinated chalcones are organic compounds with diverse biological activities and are of interest for drug development due to their improved properties, such as lipophilicity, bioavailability, and metabolic stability. Therefore, the correlation between structure and properties is fundamental to discover the potential use on pharmaceutical and technological applications. In this sense, we synthesized and characterized a novel fluorinated chalcone (E)-1-(4-fluorophenyl)-3-(naphthalen-1-yl)prop-2-en-1-one (FCH), and compared its supramolecular arrangement and topological analysis with a chalcone (E)-1-(4-hydroxyphenyl)-3-(naphthalen-1-yl)prop-2-en-1-one (HCH). The molecular electrostatic potential, QTAIM, and frontier molecular orbitals of both chalcones were investigated using the M06-2X/6-311++G(d,p) level of theory. Our findings show that the FCH exhibits a herringbone packing with intermolecular interactions of C–H⋯F and C–H⋯π, while the HCH assumes a staircase packing coordinated by O–H⋯O and π⋯π intermolecular interactions. Furthermore, the electrostatic potential analysis shows that FCH is susceptible to electrophilic attack, while HCH is susceptible to nucleophilic attack. Finally, the structural basis analysis for both chalcones indicated that FCH has a higher lipophilicity than HCH due to the stronger hydrogen bond of HCH with water.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":" ","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43670307","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":"Frontmatter","authors":"","doi":"10.1515/zkri-2023-frontmatter5-6","DOIUrl":"https://doi.org/10.1515/zkri-2023-frontmatter5-6","url":null,"abstract":"","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"16 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134992303","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":"Twinned single crystal structure of Li4P2S6","authors":"H. Ben Yahia, K. Motohashi, S. Mori, Atsushi Sakuda, A. Hayashi","doi":"10.1515/zkri-2023-0013","DOIUrl":"https://doi.org/10.1515/zkri-2023-0013","url":null,"abstract":"Abstract Yellow needles-like single crystals of Li4P2S6 were obtained serendipitously during the preparation of Li7P3S10O. The twinned crystal structure of Li4P2S6 was determined from single-crystal X-ray diffraction data [wR(F2) = 0.069, 716 reflections, 40 variables]. Li4P2S6 crystallizes in the trigonal system, space group P 3 ‾ m 1 $Poverline{3}m1$ (N° 164), a = 10.5042(8) Å, c = 6.5837(6) Å, V = 629.11(9) Å3 and Z = 2. The lithium octahedra form a [Li4S6]8− honeycomb-like structure within which diphosphate units are located. The comparison of our crystal structure to those of P63/mcm-, P 3 ‾ 1 m $Poverline{3}1m$ -, and P321-Li4P2S6 demonstrated group-subgroup relationships and associated the disorder or order of the phosphorus atoms within the identical [Li4S6]8− 3d-frameworks to the choice of the unit cell (the subcell with a ∼ 6.07 Å vs. the supercell with a ∼ 10.5 Å).","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"209 - 216"},"PeriodicalIF":1.2,"publicationDate":"2023-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42678311","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":"Jana2020 – a new version of the crystallographic computing system Jana","authors":"V. Petříček, L. Palatinus, J. Plášil, M. Dušek","doi":"10.1515/zkri-2023-0005","DOIUrl":"https://doi.org/10.1515/zkri-2023-0005","url":null,"abstract":"Abstract We present the crystallographic program Jana2020, the successor of Jana2006. Jana2020 has new, technically different graphics and structure plot-driven intuitive control. Tools known from Jana2006 were revised and inserted into a new logical scheme, and their control connected with the structure plot. Some of the tools were considerably improved. We focus on the details of the most dynamically developing parts, namely twinned structures, magnetic structures, and structure analysis based on electron diffraction data.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"0 1","pages":""},"PeriodicalIF":1.2,"publicationDate":"2023-04-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42945626","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":"Incorporation of Pb in (Al,Ge)-mullites in the presence of Fe, Cr, Nd, and Sm","authors":"Samuel Abdelmaseh, M. Burianek, J. Birkenstock, L. Fischer, H. Schneider, R. Fischer","doi":"10.1515/zkri-2022-0026","DOIUrl":"https://doi.org/10.1515/zkri-2022-0026","url":null,"abstract":"Abstract Single crystals of five (Al,Ge)-mullites incorporating Pb, and four of which also incorporating foreign cations (Fe,Cr,Nd,Sm) were grown by flux techniques in a PbO-MoO3 flux. They were characterized by scanning electron microscopy, electron microprobe analyses, single-crystal X-ray diffraction. In addition, the refractive indices of mullite containing Nd were determined by spindle-stage optical investigations. Careful inspection of the single-crystal X-ray diffraction data revealed that weak superstructure reflections observed in all doped crystals violating the reflection conditions can be attributed to λ/2 contributions in the primary X-ray beam. Consequently, all crystal structures were refined in space group Pbam, thus avoiding a symmetry lowering to a noncentrosymmetric subgroup as done in earlier work on a (Al,Ge)-mullite doped with Pb and Nd (Saalfeld & Klaska, Z. Kristallogr. 1985, 172, 129–133). The following phases with chemical compositions used in the refinements were obtained: undoped mullite (Al4.50Ge1.50O9.75; a = 7.6559(4) Å, b = 7.7763(4) Å, c = 2.9233(2) Å, V = 174.04(2) Å3); (Pb,Fe)-doped mullite (Pb0.02Fe0.68Al3.95Ge1.37O9.70; a = 7.7125(7) Å, b = 7.8527(7) Å, c = 2.9528(2) Å, V = 178.83(3) Å3); (Pb,Cr)-doped mullite (Pb0.01Cr0.63Al3.90Ge1.47O9.75; a = 7.6917(6) Å, b = 7.8168(6) Å, c = 2.9522(2) Å, V = 177.50(2) Å3); (Pb,Nd)-doped mullite (Pb0.06Nd0.02Al4.82Ge1.18O9.69; a = 7.6585(7) Å, b = 7.7666(7) Å, c = 2.9164(3) Å, V = 173.47(3) Å3); (Pb,Sm)-doped mullite (Pb0.06Sm0.02Al4.55Ge1.45O9.79; a = 7.6563(3) Å, b = 7.7873(3) Å, c = 2.9236(1) Å, V = 174.31(1) Å3); Pb is only incorporated into the crystal structure when a co-dopant element is present. Then it resides together with Nd or Sm in the oxygen-vacancy sites created by the formation of triclusters of AlO4 and GeO4 tetrahedra. In the case of (Pb,Fe)-doped mullite, Fe shares the same position as Al and Ge. In contrast to the (Al,Si)-mullites, Ge is located in both tetrahedral sites T and T*. The occupancies follow a substitution scheme according to Pb q (Nd,Sm) r (Cr,Fe) z Al4+2v−zGe2−2vO10−v+q+3/2r. With v = number of vacancies, such a mullite can be understood as a “stuffed mullite” derived from a related “open mullite” (no vacancies filled with large cations) of composition (Cr,Fe) z Al4+2v−zGe2−2vO10−v and then “stuffed” with qPb2+ + r(Nd3+,Sm3+) formula units where concurrently the number of available O3-vacancies is reduced by q + 3/2r units of extra oxygen. Thus, charge compensation upon incorporation of Pb2+ and (Nd,Sm)3+ is achieved by adding the amount of oxygen corresponding to the oxidation state of divalent Pb2+ and trivalent rare-earth elements. Based on this description, the maximum number of large cations which can be stuffed into the mullite structure can directly be calculated from the v-value of the related “open mullite”. In contrast, the smaller cations Fe3+ and Cr3+ are directly substituting Al3+. In the stuffed mullites, Pb and (Nd,Sm) could ","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"151 - 166"},"PeriodicalIF":1.2,"publicationDate":"2023-04-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48708466","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":"Ternary amalgams: expanding the structural variety of the Gd14Ag51 family","authors":"T. Hohl, L. Nusser, Jessica Wulfes, C. Hoch","doi":"10.1515/zkri-2023-0007","DOIUrl":"https://doi.org/10.1515/zkri-2023-0007","url":null,"abstract":"Abstract In intermetallic chemistry, the Gd14Ag51 structure type is rather common and has many amalgam representatives. Up to today, binary amalgams of this type have been described for M = Na, Ca, Sr, Eu, Yb, and the structure family still is growing. Yb11Hg54 is the only representative with a fully ordered crystal structure, and all other representatives exhibit individual disorder phenomena or patterns. The diversity of disorder phenomena in this structural family is unique. In order to shed a light on the underlying reasons for this unexpected structural complexity, we compare the available literature structure models with three new ternary variants, Yb10.7Sr0.3Hg54, Ca4.5Eu6.5Hg54 and Ca6.9Na4.1Hg54 (all in space group type P 6 ‾ $Poverline{6}$ , a = 13.5379(12), 13.5406(8) and 13.564(5) Å, c = 9.7488(14), 9.7149 and 9.810(7) Å for Yb10.7Sr0.3Hg54, Ca4.5Eu6.5Hg54 and Ca6.9Na4.1Hg54, respectively). Their crystal structures have been examined in detail on the basis of both single crystal and powder X-ray diffraction data. Each of the three new amalgams exhibits its own set of disorder phenomena that is again different from those of the respective binary variants. The synopsis of the crystal structures and their individual disorder phenomena indicates that the reason for the disorder phenomena cannot be found only by analyzing geometric details such as atomic radii quotients or coordination polyhedral volumina, and additional electronic reasons must be assumed.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"187 - 199"},"PeriodicalIF":1.2,"publicationDate":"2023-04-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44262041","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":"Ternary orthorhombic Laves phases Sr2Pd3Sn, Eu2Pd3Sn and Eu2Pd3In","authors":"Joshua Wiethölter, Aylin Koldemir, T. Block, M. Reimann, Steffen Klenner, Rainer Pöttgen","doi":"10.1515/zkri-2023-0014","DOIUrl":"https://doi.org/10.1515/zkri-2023-0014","url":null,"abstract":"Abstract The ternary Laves phases Sr2Pd3Sn, Eu2Pd3Sn and Eu2Pd3In were synthesized by induction melting of the elements in sealed tantalum ampoules. The polycrystalline products were characterized through their powder X-ray diffraction patterns. The structure of Eu2Pd3Sn was refined from single crystal X-ray diffractometer data: Mg2MnGa3 type, Cmcm, a = 583.36(5), b = 908.31(7), c = 958.06(8) pm, wR2 = 0.0366, 557 F2 values, 23 variables. The palladium and tin atoms show the inverse coloring on the network of condensed tetrahedra of Mg2MnGa3, i.e., MnGa3 versus Pd3Sn. Refinement of the occupancy parameters revealed small defects for the europium site, leading to composition Eu1.962(6)Pd3Sn for the studied crystal. Sr2Pd3Sn is a Pauli paramagnet and Eu2Pd3Sn shows Curie-Weiss paramagnetism (7.86(1) µB Eu atom−1 and ΘP = 48.1(1) K). Ferromagnetic ordering is observed below TC = 46.1(1) K. The 119Sn and 151Eu Mössbauer spectra of Sr2Pd3Sn and Eu2Pd3Sn are discussed with respect to electron density changes as a function of the tin content and the ionicity in the sequence of the stannides Sr2Pd3Sn/Eu2Pd3Sn → Sr2Pd2Sn/Eu2Pd2Sn → EuPdSn → EuPdSn2.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"201 - 208"},"PeriodicalIF":1.2,"publicationDate":"2023-04-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45789869","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}