J. E. Rodrigues, J. Gainza, F. Serrano-Sánchez, N. Nemes, Ó. J. Durá, J. Martínez, J. Alonso
Abstract Thermoelectric M x Co4Sb12 skutterudites are well-known to exhibit a reduced thermal conductivity thanks to the rattling effect of the M-filler at the large cages occurring in the framework, centered at the 2a sites of the I m 3 ‾ $Imoverline{3}$ space group. A novel Eu-filled skutterudite has been synthesized under high-pressure conditions at 3.5 GPa in a piston-cylinder hydrostatic press. The structural refinement from high-angular resolution synchrotron X-ray diffraction (SXRD) patterns unveils an unusual position for Eu filler atoms. By difference Fourier synthesis they are found at 12d sites, conforming statistically occupied octahedra within the mentioned cages around 2a positions. The Debye temperature was estimated by averaging the isotropic displacements by the atomic masses, leading to θ D ${theta }_{D}$ of 273(2) K. Oftedal plots concerning the y and z Sb fractional positions, the unit-cell parameter a and M filling fraction include the novel Eu specimen in the trend observed for other filled materials prepared under high-pressure, including rare-earths, alkali or alkali-earth elements, all accepted as rattlers in filled skutterudites. A total thermal conductivity (κ) of 0.82 W m−1 K−1 is measured at 773 K for Eu0.02(1)Co4Sb12, below that of other filled skutterudites, which is promoted by the enhanced phonon scattering of Eu located at 12d sites. FE-SEM images showed large, homogeneous grains, well compacted after the high-pressure synthesis.
众所周知，热电M x Co4Sb12 skutterudites表现出降低的导热性，这要归功于M-填料在框架中出现的大笼上的震动效应，以I M 3 $Imoverline{3}$空间群的2a个位置为中心。在高压条件下，在活塞缸静压下合成了一种新型的铕填充方菱铁矿。高角分辨率同步x射线衍射(SXRD)模式的结构细化揭示了Eu填充原子的不寻常位置。通过差分傅立叶合成，它们在12d个位点上被发现，符合统计上占据的八面体在上述笼中约2a个位置。通过原子质量平均各向同性位移来估计Debye温度，得到θ D ${theta }_{D}$ (273(2) k)。通常关于y和z Sb分数位置的图，单元格参数a和M填充分数包括新的Eu样品，这是在高压下制备的其他填充材料中观察到的趋势，包括稀土，碱或碱土元素，所有这些都被认为是填充的方块石中的尾端。在773 K下，Eu0.02(1)Co4Sb12的总热导率(κ)为0.82 W m−1 K−1，低于其他填充的方粒矿，这是由于Eu在12d位置的声子散射增强所致。FE-SEM图像显示，高压合成后的材料颗粒大而均匀，压实良好。
{"title":"A novel crystallographic location of rattling atoms in filled Eu x Co4Sb12 skutterudites prepared under high-pressure conditions","authors":"J. E. Rodrigues, J. Gainza, F. Serrano-Sánchez, N. Nemes, Ó. J. Durá, J. Martínez, J. Alonso","doi":"10.1515/zkri-2022-0051","DOIUrl":"https://doi.org/10.1515/zkri-2022-0051","url":null,"abstract":"Abstract Thermoelectric M x Co4Sb12 skutterudites are well-known to exhibit a reduced thermal conductivity thanks to the rattling effect of the M-filler at the large cages occurring in the framework, centered at the 2a sites of the I m 3 ‾ $Imoverline{3}$ space group. A novel Eu-filled skutterudite has been synthesized under high-pressure conditions at 3.5 GPa in a piston-cylinder hydrostatic press. The structural refinement from high-angular resolution synchrotron X-ray diffraction (SXRD) patterns unveils an unusual position for Eu filler atoms. By difference Fourier synthesis they are found at 12d sites, conforming statistically occupied octahedra within the mentioned cages around 2a positions. The Debye temperature was estimated by averaging the isotropic displacements by the atomic masses, leading to θ D ${theta }_{D}$ of 273(2) K. Oftedal plots concerning the y and z Sb fractional positions, the unit-cell parameter a and M filling fraction include the novel Eu specimen in the trend observed for other filled materials prepared under high-pressure, including rare-earths, alkali or alkali-earth elements, all accepted as rattlers in filled skutterudites. A total thermal conductivity (κ) of 0.82 W m−1 K−1 is measured at 773 K for Eu0.02(1)Co4Sb12, below that of other filled skutterudites, which is promoted by the enhanced phonon scattering of Eu located at 12d sites. FE-SEM images showed large, homogeneous grains, well compacted after the high-pressure synthesis.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"47 - 56"},"PeriodicalIF":1.2,"publicationDate":"2022-12-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42555178","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}
Y. Meng, Donghui Liu, Qiao Lan, Ziyu Xie, F. Niu, Xiaolin Zhang, Youming Yang
Abstract A two-dimensional uranyl organic framework (UOF) UO2(L)(DMA) (1) (H2L = 2-aminoisophthalic acid, DMA = N, N-dimethylacetamide) has been solvothermally synthesized and characterized thoroughly by elemental analysis, infrared spectroscopy, single-crystal X-ray diffraction, solid fluorescence, powder X-ray diffraction, thermogravimetric analysis, and UV–visible spectroscopy. Furthermore, the degradation efficiencies of UOF 1 to organic dye methylene blue (MB) and rhodamine B (RhB) are 93.2 and 86.5% under irradiation of visible light which indicates that UOF 1 has remarkable photocatalytic activity. UOF 1 also displayed a certain selectivity for mixed dyes of MB & RhB.
{"title":"Synthesis, structure, and photocatalytic properties of a two-dimensional uranyl organic framework","authors":"Y. Meng, Donghui Liu, Qiao Lan, Ziyu Xie, F. Niu, Xiaolin Zhang, Youming Yang","doi":"10.1515/zkri-2022-0012","DOIUrl":"https://doi.org/10.1515/zkri-2022-0012","url":null,"abstract":"Abstract A two-dimensional uranyl organic framework (UOF) UO2(L)(DMA) (1) (H2L = 2-aminoisophthalic acid, DMA = N, N-dimethylacetamide) has been solvothermally synthesized and characterized thoroughly by elemental analysis, infrared spectroscopy, single-crystal X-ray diffraction, solid fluorescence, powder X-ray diffraction, thermogravimetric analysis, and UV–visible spectroscopy. Furthermore, the degradation efficiencies of UOF 1 to organic dye methylene blue (MB) and rhodamine B (RhB) are 93.2 and 86.5% under irradiation of visible light which indicates that UOF 1 has remarkable photocatalytic activity. UOF 1 also displayed a certain selectivity for mixed dyes of MB & RhB.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"65 - 71"},"PeriodicalIF":1.2,"publicationDate":"2022-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42942094","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}
Abstract The intermetallic barium compounds BaTMg2 (T = Pd, Ag, Pt, Au) and BaAuCd2 were synthesized by reactions of the elements in sealed tantalum ampoules in muffle furnaces. The five compounds crystallize with the orthorhombic MgCuAl2 type structure, space group Cmcm, with small differences in chemical bonding between the magnesium and cadmium series. All samples were characterized through their Guinier powder diffraction patterns. The structures of BaPdMg2 (a = 444.57(4), b = 1174.67(10), c = 827.58(7) pm, wR2 = 0.0460, 475 F2 values, 16 variables), BaAuMg2 (a = 450.27(6), b = 1183.94(16), c = 838.76(11) pm, wR2 = 0.0355, 473 F2 values, 16 variables) and BaAuCd2 (a = 463.31(5), b = 1112.79(12), c = 826.63(8) pm, wR2 = 0.0453, 469 F2 values, 16 variables) were refined from single crystal X-ray diffraction data. The large barium atoms push the [TMg2] respectively [AuCd2] substructures apart. This allows fast moisture attack and leads to fast hydrolyzes of the samples when they get in contact with water. The influence of the difference in electronegativity between magnesium and cadmium is reflected for the pair of compounds BaAuMg2 and BaAuCd2. The magnesium compound shows the higher auridic character, while the cadmium compound shows a tendency towards a three-dimensional cadmium substructure.
{"title":"Magnesium and barium in two substructures: BaTMg2 (T = Pd, Ag, Pt, Au) and the isotypic cadmium compound BaAuCd2 with MgCuAl2 type structure","authors":"M. Reimann, R. Pöttgen","doi":"10.1515/zkri-2022-0059","DOIUrl":"https://doi.org/10.1515/zkri-2022-0059","url":null,"abstract":"Abstract The intermetallic barium compounds BaTMg2 (T = Pd, Ag, Pt, Au) and BaAuCd2 were synthesized by reactions of the elements in sealed tantalum ampoules in muffle furnaces. The five compounds crystallize with the orthorhombic MgCuAl2 type structure, space group Cmcm, with small differences in chemical bonding between the magnesium and cadmium series. All samples were characterized through their Guinier powder diffraction patterns. The structures of BaPdMg2 (a = 444.57(4), b = 1174.67(10), c = 827.58(7) pm, wR2 = 0.0460, 475 F2 values, 16 variables), BaAuMg2 (a = 450.27(6), b = 1183.94(16), c = 838.76(11) pm, wR2 = 0.0355, 473 F2 values, 16 variables) and BaAuCd2 (a = 463.31(5), b = 1112.79(12), c = 826.63(8) pm, wR2 = 0.0453, 469 F2 values, 16 variables) were refined from single crystal X-ray diffraction data. The large barium atoms push the [TMg2] respectively [AuCd2] substructures apart. This allows fast moisture attack and leads to fast hydrolyzes of the samples when they get in contact with water. The influence of the difference in electronegativity between magnesium and cadmium is reflected for the pair of compounds BaAuMg2 and BaAuCd2. The magnesium compound shows the higher auridic character, while the cadmium compound shows a tendency towards a three-dimensional cadmium substructure.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"57 - 63"},"PeriodicalIF":1.2,"publicationDate":"2022-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47324776","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}
Abstract The xBa(Ti(1−y)Zry)O3–(1−x)PbTiO3 ceramic samples with x = 0.3, y = 0.95; x = 0.3, y = 0.7; x = 0.3, y = 0.3; x = 0.3, y = 0.05; x = 0.5, y = 0.05 were synthesized by a solid state reaction technique. The XRD patterns of these samples have anisotropic broadening of diffraction peaks. The crystallographic data were analyzed by the Rietveld method. During the refinement process the Stephens’s approach was used. All the samples studied are solid solutions with the tetragonal perovskite structure. The degree of tetragonal distortion of these solid solutions decreases with an increase in the Zr content. The microstructure analysis showed that the broadening of the diffraction peaks on the XRD patterns is due to both strains and small crystallite sizes.
{"title":"Structural study of ceramic samples of the PbTiO3–BaTiO3–BaZrO3 system with a high PbTiO3 content studied by the Rietveld method","authors":"Vladimir Sirotinkin, A. Bush, V. Kozlov","doi":"10.1515/zkri-2022-0028","DOIUrl":"https://doi.org/10.1515/zkri-2022-0028","url":null,"abstract":"Abstract The xBa(Ti(1−y)Zry)O3–(1−x)PbTiO3 ceramic samples with x = 0.3, y = 0.95; x = 0.3, y = 0.7; x = 0.3, y = 0.3; x = 0.3, y = 0.05; x = 0.5, y = 0.05 were synthesized by a solid state reaction technique. The XRD patterns of these samples have anisotropic broadening of diffraction peaks. The crystallographic data were analyzed by the Rietveld method. During the refinement process the Stephens’s approach was used. All the samples studied are solid solutions with the tetragonal perovskite structure. The degree of tetragonal distortion of these solid solutions decreases with an increase in the Zr content. The microstructure analysis showed that the broadening of the diffraction peaks on the XRD patterns is due to both strains and small crystallite sizes.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"39 - 46"},"PeriodicalIF":1.2,"publicationDate":"2022-11-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48235800","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}
M. Horiacha, G. Nychyporuk, Judith Bönnighausen, F. Stegemann, V. Pavlyuk, R. Pöttgen, V. Zaremba
Abstract YNiIn and YCuIn form complete solid solutions YNiIn1−x Al x and YCuIn1−x Al x , which were characterized on the basis of X-ray powder diffraction. The ZrNiAl type crystal structures (space groups P 6 ‾ 2 m $Poverline{6}2m$ ) of YNiAl (a = 0.70386(9), c = 0.38327(4) nm, wR 2 = 0.0424), YNiIn0.77Al0.23 (a = 0.73895(9), c = 0.37707(4) nm, wR 2 = 0.0498) and YCuIn0.63Al0.37 (a = 0.73404(7), c = 0.39045(4) nm, wR 2 = 0.0314) were refined from the single crystal X-ray diffraction data. Exemplarily the electronic structure of YNiAl was studied, manifesting substantial Ni–Al bonding within the three-dimensional [NiAl] substructure. Comparison of YNiAl with isotypic YNiIn shows stronger Ni–Al bonding as compared to Ni–In. Magnetic susceptibility measurements of YNiIn1−x Al x (x = 0.1, 0.2, 0.7 and 0.9), YNiIn and YNiAl in the temperature range 3–300 K indicated Pauli paramagnetic behaviour with molar magnetic susceptibility of about 0.15–0.22 × 10−3 emu/mol.
摘要YNiIn和YCuIn形成完整的固溶体YNiIn1−x Alx和YCuIn1−xAlx，并用x射线粉末衍射对其进行了表征。ZrNiAl型晶体结构（空间群P6‾2 m$Poverline{6}2m$）、YNiIn0.77Al0.23（a=0.73895（9），c=0.37707（4）nm，wR2=0.0498）和YCuIn0.63Al0.37（a=0.73404（7），c=0.39045（4）纳米，wR2=0.0314）。例如，研究了YNiAl的电子结构，在三维[NiAl]亚结构中表现出实质性的Ni–Al键合。与Ni–In相比，YNiAl与同型YNiIn的比较显示出更强的Ni–Al键合。YNiIn1−x Al x（x=0.1、0.2、0.7和0.9）、YNiIn和YNiAl在3–300 K温度范围内的磁化率测量表明，泡利顺磁行为的摩尔磁化率约为0.15–0.22×10−3 emu/mol。
{"title":"Structure and properties of phases from solid solutions YTIn1−x Al x (T = Ni and Cu)","authors":"M. Horiacha, G. Nychyporuk, Judith Bönnighausen, F. Stegemann, V. Pavlyuk, R. Pöttgen, V. Zaremba","doi":"10.1515/zkri-2022-0052","DOIUrl":"https://doi.org/10.1515/zkri-2022-0052","url":null,"abstract":"Abstract YNiIn and YCuIn form complete solid solutions YNiIn1−x Al x and YCuIn1−x Al x , which were characterized on the basis of X-ray powder diffraction. The ZrNiAl type crystal structures (space groups P 6 ‾ 2 m $Poverline{6}2m$ ) of YNiAl (a = 0.70386(9), c = 0.38327(4) nm, wR 2 = 0.0424), YNiIn0.77Al0.23 (a = 0.73895(9), c = 0.37707(4) nm, wR 2 = 0.0498) and YCuIn0.63Al0.37 (a = 0.73404(7), c = 0.39045(4) nm, wR 2 = 0.0314) were refined from the single crystal X-ray diffraction data. Exemplarily the electronic structure of YNiAl was studied, manifesting substantial Ni–Al bonding within the three-dimensional [NiAl] substructure. Comparison of YNiAl with isotypic YNiIn shows stronger Ni–Al bonding as compared to Ni–In. Magnetic susceptibility measurements of YNiIn1−x Al x (x = 0.1, 0.2, 0.7 and 0.9), YNiIn and YNiAl in the temperature range 3–300 K indicated Pauli paramagnetic behaviour with molar magnetic susceptibility of about 0.15–0.22 × 10−3 emu/mol.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"17 - 25"},"PeriodicalIF":1.2,"publicationDate":"2022-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43109277","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}
Marius Wolpmann, M. Etter, A. Kirsch, F. Balzaretti, W. Dononelli, L. Robben, T. Gesing
Abstract Sodalites of the general type |Na8X2|[T1T2O4]6 with X = Cl−, Br−, I− have been synthesized for Al–Si, Ga–Si, Al–Ge and Ga–Ge as T1–T2 frameworks. The structures were examined using in-house and synchrotron X-ray diffraction, Raman spectroscopy, force-field structure optimizations and DFT based ab-initio molecular dynamics (MD) computations. Calculated phonon density of states (PDOS) of the 12 compounds show only minor differences within a framework composition with a lowering of certain phonon energies with increasing anion size. Earlier published Debye and Einstein temperatures obtained with a Debye-Einstein-anharmonicity (DEA) model approach are confirmed using the determined low-temperature lattice parameters (18 K–293 K) and show no correlation with the respective PDOS. Small-box refinements against radial pair distribution functions (PDF) allowed the determination of anisotropic displacement ellipsoids (ADP) for Na+ and O2−, indicating a strong dependency of the ADP of Na+ on the chemical composition. Significantly lower thermal displacements from MD calculations suggested an influence of structural displacements. For compounds with an aspherical ADP for sodium, structural models could be refined in which the sodium is located on two 8e or one 24i site (both partially occupied), and also temperature-dependent (100 K–300 K) for the compounds with Ga–Ge framework. 3D-plots of the bond-valence sums of Na+ further validate the structural differences. These results imply that the local structure of halide-sodalites in many cases is not best described by the known average structure and may even not be cubic.
摘要以Al-Si, Ga-Si, Al-Ge和Ga-Ge为T1-T2骨架，合成了X = Cl−，Br−，I−的一般型|Na8X2|[T1T2O4]6钠盐。利用内部和同步加速器x射线衍射、拉曼光谱、力场结构优化和基于DFT的从头算分子动力学(MD)计算对这些结构进行了检测。12种化合物的声子态密度(PDOS)在一个框架组成中只有很小的差异，随着阴离子大小的增加，某些声子能量降低。先前发表的Debye-Einstein-anharmonicity (DEA)模型方法得到的Debye和Einstein温度，使用确定的低温晶格参数(18 K - 293 K)进行了验证，并且显示与各自的PDOS没有相关性。基于径向对分布函数(PDF)的小盒改进可以确定Na+和O2−的各向异性位移椭球体(ADP)，表明Na+的ADP与化学成分有很强的依赖性。明显较低的热位移从MD计算表明结构位移的影响。对于具有非球面ADP的钠化合物，可以改进结构模型，其中钠位于两个8e或一个24i位点(均部分占据)，并且具有Ga-Ge框架的化合物也依赖于温度(100 K - 300 K)。Na+的键价和的3d图进一步验证了结构差异。这些结果表明，在许多情况下，卤化物钠石的局部结构不能用已知的平均结构来最好地描述，甚至可能不是立方结构。
{"title":"Halide-sodalites: thermal behavior at low temperatures and local deviations from the average structure","authors":"Marius Wolpmann, M. Etter, A. Kirsch, F. Balzaretti, W. Dononelli, L. Robben, T. Gesing","doi":"10.1515/zkri-2022-0037","DOIUrl":"https://doi.org/10.1515/zkri-2022-0037","url":null,"abstract":"Abstract Sodalites of the general type |Na8X2|[T1T2O4]6 with X = Cl−, Br−, I− have been synthesized for Al–Si, Ga–Si, Al–Ge and Ga–Ge as T1–T2 frameworks. The structures were examined using in-house and synchrotron X-ray diffraction, Raman spectroscopy, force-field structure optimizations and DFT based ab-initio molecular dynamics (MD) computations. Calculated phonon density of states (PDOS) of the 12 compounds show only minor differences within a framework composition with a lowering of certain phonon energies with increasing anion size. Earlier published Debye and Einstein temperatures obtained with a Debye-Einstein-anharmonicity (DEA) model approach are confirmed using the determined low-temperature lattice parameters (18 K–293 K) and show no correlation with the respective PDOS. Small-box refinements against radial pair distribution functions (PDF) allowed the determination of anisotropic displacement ellipsoids (ADP) for Na+ and O2−, indicating a strong dependency of the ADP of Na+ on the chemical composition. Significantly lower thermal displacements from MD calculations suggested an influence of structural displacements. For compounds with an aspherical ADP for sodium, structural models could be refined in which the sodium is located on two 8e or one 24i site (both partially occupied), and also temperature-dependent (100 K–300 K) for the compounds with Ga–Ge framework. 3D-plots of the bond-valence sums of Na+ further validate the structural differences. These results imply that the local structure of halide-sodalites in many cases is not best described by the known average structure and may even not be cubic.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"27 - 38"},"PeriodicalIF":1.2,"publicationDate":"2022-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47454512","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}
Abstract Single crystals of three mixed-valent oxidotellurates(IV/VI) with general formula M2TeIVTeVIO6 (H2O) x (M = Na, K, Rb) were grown under hydrothermal conditions at 210 °C from M2CO3, TeO2 and Te(OH)6 in a 4:1:1 molar ratio. Na2Te2O6·11/8H2O (where TeIVTeVI is abbreviated as Te2) crystallizes as a monoclinic eightfold superstructure with occupational modulation of the water molecules. The structure is built of diperiodic corrugated [Te2O6]2− networks interleaved by the Na atoms and H2O molecules. The hexagonal crystal structures of M2Te2O4(OH)4 (M = K, Rb; x = 2) with P63/mmc symmetry are made up of [Te2O4(OH)4]2− rods extending in the [001] direction. The rods are connected by the M atoms. The [TeIVO2(OH)2] units are disordered about the threefold axis, resulting in pronounced three-dimensional diffuse scattering.
{"title":"Mixed-valent 1:1 oxidotellurates(IV/VI) of Na, K and Rb: superstructure and three-dimensional disorder","authors":"Hermann Völkl, F. Eder, B. Stöger, M. Weil","doi":"10.1515/zkri-2022-0036","DOIUrl":"https://doi.org/10.1515/zkri-2022-0036","url":null,"abstract":"Abstract Single crystals of three mixed-valent oxidotellurates(IV/VI) with general formula M2TeIVTeVIO6 (H2O) x (M = Na, K, Rb) were grown under hydrothermal conditions at 210 °C from M2CO3, TeO2 and Te(OH)6 in a 4:1:1 molar ratio. Na2Te2O6·11/8H2O (where TeIVTeVI is abbreviated as Te2) crystallizes as a monoclinic eightfold superstructure with occupational modulation of the water molecules. The structure is built of diperiodic corrugated [Te2O6]2− networks interleaved by the Na atoms and H2O molecules. The hexagonal crystal structures of M2Te2O4(OH)4 (M = K, Rb; x = 2) with P63/mmc symmetry are made up of [Te2O4(OH)4]2− rods extending in the [001] direction. The rods are connected by the M atoms. The [TeIVO2(OH)2] units are disordered about the threefold axis, resulting in pronounced three-dimensional diffuse scattering.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"7 - 15"},"PeriodicalIF":1.2,"publicationDate":"2022-11-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45894550","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}
D. Charkin, P. Chachin, Evgenii V. Nazarchuk, O. Siidra
Abstract Singe crystals of four new AIMII[ReO4]3 perrhenates (AI = Na, MII = Pb; AI = Na, MII = Sr, Ag, K) have been prepared from the respective AI[ReO4] and MII[ReO4]2 perrhenates using melt and solution evaporation techniques. All new compounds belong to the hexagonal CdTh[MoO4]3 structure type, similar to previously known NaCa[ReO4]3. We discuss the crystal chemical relationships within this structure type and suggest existence of some more representatives involving other tetrahedral anions.
{"title":"A contribution to the perrhenate crystal chemistry: the crystal structures of new CdTh[MoO4]3-type compounds","authors":"D. Charkin, P. Chachin, Evgenii V. Nazarchuk, O. Siidra","doi":"10.1515/zkri-2022-0043","DOIUrl":"https://doi.org/10.1515/zkri-2022-0043","url":null,"abstract":"Abstract Singe crystals of four new AIMII[ReO4]3 perrhenates (AI = Na, MII = Pb; AI = Na, MII = Sr, Ag, K) have been prepared from the respective AI[ReO4] and MII[ReO4]2 perrhenates using melt and solution evaporation techniques. All new compounds belong to the hexagonal CdTh[MoO4]3 structure type, similar to previously known NaCa[ReO4]3. We discuss the crystal chemical relationships within this structure type and suggest existence of some more representatives involving other tetrahedral anions.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"238 1","pages":"1 - 5"},"PeriodicalIF":1.2,"publicationDate":"2022-10-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48342138","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}
Jun-Xia Li, Linying Xiong, Xiao-jie Xu, Chang Liu, Zheng-Guo Wang
Abstract Triclopyr ethyl ester (1) has been co-synthesized through one-pot solvothermal reaction and the crystal structure has been determined by single crystal X-ray structure analysis. The compound C18H16Cl6N2O6 crystallizes in the monoclinic crystal system, P21/c space group with unit-cell parameters: a = 4.9615(2) Å, b = 30.9297(14) Å, c = 15.9155(10) Å, β = 91.466(4)° and Z = 4. Each unit cell is composed of two discrete, similar but reversely arranged triclopyr ethyl ester organic molecules. In the 3D packing plot, 1 is further assembled into a network structure via rich Cl⋯Cl halogen bond interactions. In addition, the crystal structure, the flexible conformation of phenoxy methylene group of 1 has been carefully compared and discussed with those of triclopyr acid.
摘要采用一锅溶剂热反应共合成了三氯吡啶乙酯(1)，并用单晶x射线结构分析确定了其晶体结构。化合物C18H16Cl6N2O6在单斜晶系P21/c空间群中结晶，晶胞参数为:a = 4.9615(2) Å， b = 30.9297(14) Å， c = 15.9155(10) Å， β = 91.466(4)°，Z = 4。每个细胞是由两个离散的，相似的，但反向排列的三氯吡啶乙酯有机分子。在3D填充图中，1通过丰富的Cl⋯Cl卤素键相互作用进一步组装成网络结构。此外，还对苯氧基亚甲基1的晶体结构、柔性构象与三氯吡啶酸的进行了比较和讨论。
{"title":"The synthesis, crystal structure and conformation analysis of triclopyr ethyl ester","authors":"Jun-Xia Li, Linying Xiong, Xiao-jie Xu, Chang Liu, Zheng-Guo Wang","doi":"10.1515/zkri-2022-0047","DOIUrl":"https://doi.org/10.1515/zkri-2022-0047","url":null,"abstract":"Abstract Triclopyr ethyl ester (1) has been co-synthesized through one-pot solvothermal reaction and the crystal structure has been determined by single crystal X-ray structure analysis. The compound C18H16Cl6N2O6 crystallizes in the monoclinic crystal system, P21/c space group with unit-cell parameters: a = 4.9615(2) Å, b = 30.9297(14) Å, c = 15.9155(10) Å, β = 91.466(4)° and Z = 4. Each unit cell is composed of two discrete, similar but reversely arranged triclopyr ethyl ester organic molecules. In the 3D packing plot, 1 is further assembled into a network structure via rich Cl⋯Cl halogen bond interactions. In addition, the crystal structure, the flexible conformation of phenoxy methylene group of 1 has been carefully compared and discussed with those of triclopyr acid.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"237 1","pages":"385 - 391"},"PeriodicalIF":1.2,"publicationDate":"2022-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44653236","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}
David Hamani, Lyna Torzuoli, A. Bouzid, P. Thomas, O. Masson
Abstract New and refined bond valence parameters related to ion pairs constituted of the tellurium Te4+ cation and non-oxide X n− anions (X = F, S or Se) are proposed. After a selection of specific crystalline structures, the optimization of the bond valence parameters R and b with a cutoff distance is carried out by minimizing the root mean square deviation of the Te4+ cation valence. The results are R = 1.728 Å and b = 0.622 Å with cutoff = 5.3 Å for the Te4+–F− pair and R = 2.444 Å and b = 0.387 Å with cutoff = 4.5 Å for the Te4+–S2− pair. These parameters lead to a lower dispersion of the calculated valences around the formal valence compared to that obtained with the parameters available in the literature. As for the new set related to the Te4+–Se2− pair, we find R = 2.578 Å and b = 0.296 Å with cutoff = 3.7 Å.
{"title":"New and refined bond valence parameters for Te4+–F−, Te4+–S2− and Te4+–Se2− ion pairs","authors":"David Hamani, Lyna Torzuoli, A. Bouzid, P. Thomas, O. Masson","doi":"10.1515/zkri-2022-0042","DOIUrl":"https://doi.org/10.1515/zkri-2022-0042","url":null,"abstract":"Abstract New and refined bond valence parameters related to ion pairs constituted of the tellurium Te4+ cation and non-oxide X n− anions (X = F, S or Se) are proposed. After a selection of specific crystalline structures, the optimization of the bond valence parameters R and b with a cutoff distance is carried out by minimizing the root mean square deviation of the Te4+ cation valence. The results are R = 1.728 Å and b = 0.622 Å with cutoff = 5.3 Å for the Te4+–F− pair and R = 2.444 Å and b = 0.387 Å with cutoff = 4.5 Å for the Te4+–S2− pair. These parameters lead to a lower dispersion of the calculated valences around the formal valence compared to that obtained with the parameters available in the literature. As for the new set related to the Te4+–Se2− pair, we find R = 2.578 Å and b = 0.296 Å with cutoff = 3.7 Å.","PeriodicalId":48676,"journal":{"name":"Zeitschrift Fur Kristallographie-Crystalline Materials","volume":"237 1","pages":"435 - 443"},"PeriodicalIF":1.2,"publicationDate":"2022-09-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48046524","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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