New Rubidium Zinc Hydrogen Phosphate, Rb2Zn2(HPO4)3:  Synthesis, Crystal Structure, and31P Single-Crystal NMR

2000 ◽  
Vol 39 (10) ◽  
pp. 2026-2032 ◽  
Author(s):  
Torben R. Jensen ◽  
Rita G. Hazell ◽  
Thomas Vosegaard ◽  
Hans J. Jakobsen

2020 ◽  
Vol 151 (9) ◽  
pp. 1317-1328
Author(s):  
Matthias Weil ◽  
Berthold Stöger

Abstract The caesium phosphates Cs3(H1.5PO4)2(H2O)2 and Cs3(H1.5PO4)2 were obtained from aqueous solutions, and Cs4P2O7(H2O)4 and CsPO3 from solid state reactions, respectively. Cs3(H1.5PO4)2, Cs4P2O7(H2O)4, and CsPO3 were fully structurally characterized for the first time on basis of single-crystal X-ray diffraction data recorded at − 173 °C. Monoclinic Cs3(H1.5PO4)2 (Z = 2, C2/m) represents a new structure type and comprises hydrogen phosphate groups involved in the formation of a strong non-symmetrical hydrogen bond (accompanied by a disordered H atom over a twofold rotation axis) and a very strong symmetric hydrogen bond (with the H atom situated on an inversion centre) with symmetry-related neighbouring anions. Triclinic Cs4P2O7(H2O)4 (Z = 2, P$$\bar{1}$$ 1 ¯ ) crystallizes also in a new structure type and is represented by a diphosphate group with a P–O–P bridging angle of 128.5°. Although H atoms of the water molecules were not modelled, O···O distances point to hydrogen bonds of medium strengths in the crystal structure. CsPO3 is monoclinic (Z = 4, P21/n) and belongs to the family of catena-polyphosphates (MPO3)n with a repetition period of 2. It is isotypic with the room-temperature modification of RbPO3. The crystal structure of Cs3(H1.5PO4)2(H2O)2 was re-evaluated on the basis of single-crystal X-ray diffraction data at − 173 °C, revealing that two adjacent hydrogen phosphate anions are connected by a very strong and non-symmetrical hydrogen bond, in contrast to the previously described symmetrical bonding situation derived from room temperature X-ray diffraction data. In the four title crystal structures, coordination numbers of the caesium cations range from 7 to 12. Graphic abstract



ChemInform ◽  
2010 ◽  
Vol 31 (30) ◽  
pp. no-no
Author(s):  
Torben R. Jensen ◽  
Rita G. Hazell ◽  
Thomas Vosegaard ◽  
Hans J. Jakobsen


Author(s):  
Süheyla Özbey ◽  
F. B. Kaynak ◽  
M. Toğrul ◽  
N. Demirel ◽  
H. Hoşgören

AbstractA new type of inclusion complex, S(–)-1 phenyl ethyl ammonium percholorate complex of R-(–)-2-ethyl - N - benzyl - 4, 7, 10, 13 - tetraoxa -1- azacyclopentadecane, has been prepared and studied by NMR, IR and single crystal X-ray diffraction techniques. The compound crystallizes in space group



2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.



1999 ◽  
Vol 84 (4) ◽  
pp. 536-549 ◽  
Author(s):  
Edward S. Grew ◽  
Guenther J. Redhammer ◽  
Georg Amthauer ◽  
Mark A. Cooper ◽  
Frank C. Hawthorne ◽  
...  


2020 ◽  
Vol 96 (3s) ◽  
pp. 148-153
Author(s):  
С.Д. Федотов ◽  
А.В. Бабаев ◽  
В.Н. Стаценко ◽  
К.А. Царик ◽  
В.К. Неволин

Представлены результаты изучения морфологии поверхности и структуры слоев AlN, сформированных аммиачной МЛЭ на темплейтах 3C-SiC/Si(111) on-axis- и 4° off-axis-разориентации. Опробован технологический режим низкотемпературной эпитаксии зародышевого слоя AlN на поверхности 3C-SiC(111). Среднеквадратичная шероховатость поверхности (5 х 5 мкм) слоев AlN толщиной 150 ± 50 нм составила 2,5-3,5 нм на темплейтах 3C-SiC/Si(111) on-axis и 3,3-3,5 нм на 4° off-axis. Показано уменьшение шероховатости смачивающего слоя AlN при изменении скорости роста. Получены монокристаллические слои AlN(0002) со значениями FWHM (ω-геометрия) 1,4-1,6°. The paper presents the surface morphology and crystal structure of AlN layers formed by ammonia MBE on 3C-SiC/Si(111) on-axis and 4° off-axis disorientation. It offers the technological approach of low-temperature epitaxy of the AlN nucleation layer on the 3C-SiC (111) surface. Root mean square roughness (5 х 5 |xm) of AlN layers with thickness of 150 ± 50 nm was 2,5-3,5 nm onto on-axis templates and 3.3-3.5 nm onto 4° off-axis. It appears that the RMS roughness of the AlN surface is changing with the growth rate variation. Single-crystal AlN(0002) layers with FWHM values (ω-geometry) of 1.4-1.6° have been obtained.



2015 ◽  
Vol 71 (4) ◽  
pp. 330-337 ◽  
Author(s):  
Sabina Kovač ◽  
Ljiljana Karanović ◽  
Tamara Đorđević

Two isostructural diarsenates, SrZnAs2O7(strontium zinc diarsenate), (I), and BaCuAs2O7[barium copper(II) diarsenate], (II), have been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. The three-dimensional open-framework crystal structure consists of corner-sharingM2O5(M2 = Zn or Cu) square pyramids and diarsenate (As2O7) groups. Each As2O7group shares its five corners with five differentM2O5square pyramids. The resulting framework delimits two types of tunnels aligned parallel to the [010] and [100] directions where the large divalent nine-coordinatedM1 (M1 = Sr or Ba) cations are located. The geometrical characteristics of theM1O9,M2O5and As2O7groups of known isostructural diarsenates, adopting the general formulaM1IIM2IIAs2O7(M1II= Sr, Ba, Pb;M2II= Mg, Co, Cu, Zn) and crystallizing in the space groupP21/n, are presented and discussed.



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