Zur Polymorphie des Ba(BrO3)2 und Sr(IO3)2, Kristallstruktur, röntgenographische, schwingungsspektroskopische und thermoanalytische Untersuchungen / Polymorphism of Ba(BrO3)2 and Sr(IO3)2 — Crystal Structure, X-Ray, IR, Raman, and Thermoanalytical Data

1990 ◽  
Vol 45 (5) ◽  
pp. 587-592 ◽  
Author(s):  
Heinz Dieter Lutz ◽  
Ekrem Alici ◽  
Thomas Kellersohn ◽  
Peter Kuske

The polymorphic behaviour of Ba(BrO3)2 and Sr(IO3)2 is studied by means of differential thermal analyses and high-temperature X-ray and Raman spectroscopic measurements. On dehydration of the respective monohydrates [Ba(ClO3)2 · H2O type] at low temperatures in a vacuum Ba(BrO3)2 I and α-Sr(IO3)2 (both α-Ba(IO3)2 type, space group C2/c, Z = 4) are formed. On heating these polymorphs above 145 and 240 °C, respectively, phase transitions to Ba(BrO3)2 II [Sr(ClO3)2 type] and the hitherto unknown γ-Sr(IO3)2 occur. On further heating Ba(BrO3)2 II decomposes [partly via the high-temperature polymorph Ba(BrO3)2 III] to BaBr2 and O2, γ-Sr(IO3)2 via the probably only stable polymorph β-Sr(IO3)2 to iodine and strontium paraperiodate. The IR and Raman spectra of Ba(BrO3)2 I and III, α-, β- and γ-Sr(IO3)2, and α-Ba(IO3)2 are given. The crystal structure of Ba(BrO3)2 I has been determined by single crystal X-ray diffraction. The final R value for 1586 reflections with I ≥ 2σI is 0.064. The crystal structures of the a-Ba(IO3)2 type anhydrous halates are very similar to those of the Ba(ClO3)2 · H2O type halate monohydrates.

1993 ◽  
Vol 48 (1) ◽  
pp. 1-6 ◽  
Author(s):  
Michael Schneider ◽  
Peter Kuske ◽  
Heinz Dieter Lutz

The crystal structures of the fast ionic conductors Li6MgBr8 and Li2MgBr4 oC 14 and cF 56 were determined by single crystal X -ray diffraction and neutron powder studies, respectively. At ambient temperature, Li6MBr8 (M = Mg, Mn) crystallize in a Suzuki-type structure (space group Fm3̄̄̄ m , Z = 4, Li6MgBr8: a = 1098.0(1) pm, 114 unique reflections, R = 0.037). Li2MgBr4 oC 14 crystallizes in a SnMn2S4-type structure (space group Cmmm , Z = 2, a = 777.94(2), b = 1104.25(4), and c = 386.55(1) pm , RI, = 0.073, 318 K), the high-temperature polymorph (HTM I) in the Li2MnBr4 cF 56 type (space group Fd 3 m , Z = 8, a = 1124.55(4) pm , RI , = 0.052, 673 K). These structure types are more or less ordered NaCl superstructures. The thermal ellipsoids of the lithium ions are discussed in terms of the conduction pathways and the order-disorder phase transitions observed.


2019 ◽  
Vol 74 (4) ◽  
pp. 357-363
Author(s):  
Daniela Vitzthum ◽  
Hubert Huppertz

AbstractThe mixed cation triel borate Ga4In4B15O33(OH)3 was synthesized in a Walker-type multianvil apparatus at high-pressure/high-temperature conditions of 12.5 GPa and 1300°C. Although the product could not be reproduced in further experiments, its crystal structure could be reliably determined via single-crystal X-ray diffraction data. Ga4In4B15O33(OH)3 crystallizes in the tetragonal space group I41/a (origin choice 2) with the lattice parameters a = 11.382(2), c = 15.244(2) Å, and V = 1974.9(4) Å3. The structure of the quaternary triel borate consists of a complex network of BO4 tetrahedra, edge-sharing InO6 octahedra in dinuclear units, and very dense edge-sharing GaO6 octahedra in tetranuclear units.


1995 ◽  
Vol 50 (7) ◽  
pp. 1025-1029 ◽  
Author(s):  
J. Baurmeister ◽  
A. Franken ◽  
W. Preetz

By reaction of [N(C4H9 )4]2 [B6H6] with iodomethyl-trimethylsilane in acetonitrile a solution with trimethylsilylm ethyl-closo-hexaborate(1-)anions, [B6H6 (CH2Si(CH3)3)]-, is formed. The crystal structure of [P(C6H5 )4][B6H6(CH2Si(CH3)3)] has been determined by single crystal X-ray diffraction analysis; monoclinic, space group P21/n with a = 16.140(2), b = 11.646(8), c = 16.731(3) Å, β 109.664(11)°. The 11B NMR spectrum reveals features of a mono hetero substituted octahedral B6 cage. The 13C NMR spectrum exhibits a quartet at +0.18 ppm with 1J(C,H) = 118 Hz for the three methyl groups and a weak multiplet at -0.65 ppm for the methylene bridge due to quadrupole coupling with the boron atoms. In the 29Si NMR spectrum a decet at +2.25 ppm with 2J(C,H ) = 6.9 Hz is observed. The B -C stretching vibration is observed at 1155 cm-1 in the IR and Raman spectrum.


2015 ◽  
Vol 70 (3) ◽  
pp. 183-190 ◽  
Author(s):  
Gerhard Sohr ◽  
Nina Ciaghi ◽  
Klaus Wurst ◽  
Hubert Huppertz

AbstractSingle crystals of the hydrous cadmium borate Cd6B22O39·H2O were obtained through a high-pressure/high-temperature experiment at 4.7 GPa and 1000 °C using a Walker-type multianvil apparatus. CdO and partially hydrolyzed B2O3 were used as starting materials. A single crystal X-ray diffraction study has revealed that the structure of Cd6B22O39·H2O is similar to that of the type M6B22O39·H2O (M=Fe, Co). Layers of corner-sharing BO4 groups are interconnected by BO3 groups to form channels containing the metal cations, which are six- and eight-fold coordinated by oxygen atoms. The compound crystallizes in the space group Pnma (no. 62) [R1=0.0379, wR2=0.0552 (all data)] with the unit cell dimensions a=1837.79(5), b=777.92(2), c=819.08(3) pm, and V=1171.00(6) Å3. The IR and Raman spectra reflect the structural characteristics of Cd6B22O39·H2O.


Minerals ◽  
2019 ◽  
Vol 9 (8) ◽  
pp. 486 ◽  
Author(s):  
Andrey A. Zolotarev ◽  
Elena S. Zhitova ◽  
Maria G. Krzhizhanovskaya ◽  
Mikhail A. Rassomakhin ◽  
Vladimir V. Shilovskikh ◽  
...  

The technogenic mineral phases NH4MgCl3·6H2O and (NH4)2Fe3+Cl5·H2O from the burned dumps of the Chelyabinsk coal basin have been investigated by single-crystal X-ray diffraction, scanning electron microscopy and high-temperature powder X-ray diffraction. The NH4MgCl3·6H2O phase is monoclinic, space group C2/c, unit cell parameters a = 9.3091(9), b = 9.5353(7), c = 13.2941(12) Å, β = 90.089(8)° and V = 1180.05(18) Å3. The crystal structure of NH4MgCl3·6H2O was refined to R1 = 0.078 (wR2 = 0.185) on the basis of 1678 unique reflections. The (NH4)2Fe3+Cl5·H2O phase is orthorhombic, space group Pnma, unit cell parameters a = 13.725(2), b = 9.9365(16), c = 7.0370(11) Å and V = 959.7(3) Å3. The crystal structure of (NH4)2Fe3+Cl5·H2O was refined to R1 = 0.023 (wR2 = 0.066) on the basis of 2256 unique reflections. NH4MgCl3·6H2O is stable up to 90 °C and then transforms to the less hydrated phase isotypic to β-Rb(MnCl3)(H2O)2 (i.e., NH4MgCl3·2H2O), the latter phase being stable up to 150 °C. (NH4)2Fe3+Cl5·H2O is stable up to 120 °C and then transforms to an X-ray amorphous phase. Hydrogen bonds provide an important linkage between the main structural units and play the key role in determining structural stability and physical properties of the studied phases. The mineral phases NH4MgCl3·6H2O and (NH4)2Fe3+Cl5·H2O are isostructural with natural minerals novograblenovite and kremersite, respectively.


2009 ◽  
Vol 180 (17-19) ◽  
pp. 1034-1039 ◽  
Author(s):  
Takeshi Ohzeki ◽  
Shinya Hasegawa ◽  
Misa Shimizu ◽  
Takuya Hashimoto

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