The crystal structure of arangasite, Al2F(PO4)(SO4)·9H2O determined using low-temperature synchrotron data

2014 ◽  
Vol 78 (4) ◽  
pp. 889-903
Author(s):  
O. V. Yakubovich ◽  
I. M. Steele ◽  
V. V. Chernyshev ◽  
N. V. Zayakina ◽  
G. N. Gamyanin ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Monoclinic Space Group ◽  
One Dimensional ◽  
Cell Parameters ◽  
Isotropic Approximation ◽  
Similar Chemical ◽  
Fourier Techniques ◽  
Fibrous Mineral ◽  
Difference Fourier

AbstractThe crystal structure of the fibrous mineral arangasite, Al2F(PO4)(SO4)·9H2O from the Alyaskitovoje deposit, Eastern Yakutiya, Russia, was solved using low-temperature single-crystal data from synchrotron radiation and refined against F2 to R = 9.8%. Arangasite crystallizes in the monoclinic space group P2/a, with unit-cell parameters a = 7.073(1), b = 9.634(2), c = 10.827(2) Å, β = 100.40(1)°, V = 725.7(7) Å3 and Z = 2. The positions of all the independent H atoms were obtained by difference- Fourier techniques and refined in an isotropic approximation. The arangasite crystal structure is built from one-dimensional chains of Al octahedra and PO4 tetrahedra sharing vertices, quasi-isolated SO4 tetrahedra and H2O molecules. All O atoms are involved in the system of H bonding, acting as donors and/or acceptors. Hydrogen bonding serves as the only mechanism providing linkage between the main structural fragments, thus maintaining the framework. Chains of corner-sharing Al octahedra and P tetrahedra in the arangasite structure are topologically identical to the chains built from (Fe, Al) octahedra and P tetrahedra in the crystal structure of destinezite, Fe2(OH)(PO4)(SO4)·6H2O. It has been shown that in spite of very similar chemical formulae, arangasite and sanjuanite, Al2(OH)(PO4)(SO4)·9H2O, are not isotypic.

The new mineral novograblenovite, (NH4,K)MgCl3·6H2O from the Tolbachik volcano, Kamchatka, Russia: mineral description and crystal structure

2018 ◽  
Vol 83 (02) ◽  
pp. 223-231 ◽  
Author(s):  
Viktor M. Okrugin ◽  
Sharapat S. Kudaeva ◽  
Oxana V. Karimova ◽  
Olga V. Yakubovich ◽  
Dmitry I. Belakovskiy ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Structure Refinement ◽  
Kamchatka Peninsula ◽  
New Mineral ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Tolbachik Volcano ◽  
Difference Fourier

AbstractThe new mineral novograblenovite, (NH4,K)MgCl3·6H2O, was found on basaltic lava from the 2012–2013 Tolbachik fissure eruption at the Plosky Tolbachik volcano, Kamchatka Peninsula, Russia. It occurs as prismatic, needle-like transparent crystals together with gypsum and halite. Novograblenovite was formed due to the exposure of the host rocks to eruptive gas exhalations enriched in HCl and NH3. Basalt was the source of potassium and magnesium for the mineral formation. Novograblenovite crystallises in the monoclinic space group C2/c, with unit-cell parameters a = 9.2734(3) Å, b = 9.5176(3) Å, c = 13.2439(4) Å, β = 90.187(2)°, V = 1168.91(2) Å3 and Z = 4. The five strongest reflections in the powder X-ray diffraction pattern [dobs, Å (I, %) (h k l)] are: 3.330 (100) (2 2 0), 2.976 (45) ($\bar{1}\; 1\; 4$), 2.353 (29) ($\bar {2}\; 2\; 4$), 3.825 (26) (2 0 2), 1.997 (25) ($\overline {4\; 2} $ 2). The density calculated from the empirical formula and the X-ray data is 1.504 g cm–3. The mineral is biaxial (+) with α = 1.469(2), β = 1.479(2) and γ = 1.496(2) (λ = 589 nm); 2Vmeas. = 80(10)° and 2Vcalc. = 75.7°. The crystal structure (solved and refined using single-crystal X-ray diffraction data, R1 = 0.0423) is based on the perovskite-like network of (NH4,K)Cl6-octahedra sharing chlorine vertices, and comprises [Mg(H2O)6]2+ groups in framework channels. The positions of all independent H atoms were obtained by difference-Fourier techniques and refined isotropically. All oxygen, nitrogen and chlorine atoms are involved in the system of hydrogen bonding, acting as donors or acceptors. The formula resulting from the structure refinement is [(NH4)0.7K0.3]MgCl3·6H2O. The mineral is named after Prokopiy Trifonovich Novograblenov, one of the researchers of Kamchatka Peninsula, a teacher, naturalist, geographer and geologist.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

Crystal structure of potassium tetraperoxomolybdate (VI) K2[Mo(O2)4]

2005 ◽  
Vol 20 (3) ◽  
pp. 203-206 ◽  
Author(s):  
M. Grzywa ◽  
M. Różycka ◽  
W. Łasocha
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Diffraction Pattern ◽  
Powder Diffraction ◽  
Rietveld Method ◽  
Structure Refinement ◽  
Crystal Structure Refinement ◽  
Unit Cell Parameters ◽  
X Ray ◽  
Cell Parameters

Potassium tetraperoxomolybdate (VI) K2[Mo(O2)4] was prepared, and its X-ray powder diffraction pattern was recorded at low temperature (258 K). The unit cell parameters were refined to a=10.7891(2) Å, α=64.925(3)°, space group R−3c (167), Z=6. The compound is isostructural with potassium tetraperoxotungstate (VI) K2[W(O2)4] (Stomberg, 1988). The sample of K2[Mo(O2)4] was characterized by analytical investigations, and the results of crystal structure refinement by Rietveld method are presented; final RP and RWP are 9.79% and 12.37%, respectively.

Crystal structure determination of 1-pentanol from low-temperature powder diffraction data by Patterson search methods

2005 ◽  
Vol 20 (4) ◽  
pp. 311-315 ◽  
Author(s):  
M. Ramírez-Cardona ◽  
L. Ventolà ◽  
T. Calvet ◽  
M. A. Cuevas-Diarte ◽  
J. Rius ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Diffraction Data ◽  
Least Squares Method ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Search Methods ◽  
Cell Parameters ◽  
Position Sensitive ◽  
Patterson Search

In the course of our research on normal alkanols, the crystal structure of 1-pentanol has been solved by applying Patterson-search methods to laboratory powder X-ray diffraction data recorded on a curved position-sensitive detector (CPS120) at 183 K. The crystal structure was refined with the rigid-body Rietveld least-squares method. The cell is monoclinic, space group P21∕c, Z=4, and the cell parameters are a=15.592(9) Å, b=4.349(1) Å, c=9.157(1) Å, β=104.7(7)°, V=600.6(3) Å3. There is one molecule in the asymmetric unit with the O–H bond in gauche conformation with respect to the alkyl skeleton. Packing is defined by the hydrogen bonds linking the 1-pentanol molecules along zigzag chains parallel to b.

Synthesis and crystal structure of the rare earth borogermanate EuGeBO5

2017 ◽  
Vol 72 (2) ◽  
pp. 95-99 ◽  
Author(s):  
Yang Chi ◽  
Yan Zhuang ◽  
Sheng-Ping Guo
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Earth Metal ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Synthesis And Crystal Structure ◽  
Cell Parameters ◽  
Type Layer ◽  
Related Compounds ◽  
The Rare Earth

AbstractThe synthesis and crystal structure of the rare earth borogermanate EuGeBO5 are reported. It is synthesized by high-temperature solid-state reaction and crystallizes in the monoclinic space group P21/c (no. 14) with the unit cell parameters a=4.8860(5), b=7.5229(8), c=9.9587(10) Å, and β=91.709(3)°. Its crystal structure features a polyanion-type layer (GeBO5)3− constructed by BO4 and GeO4 tetrahedra connected alternatingly. Eu3+ ions are located in cavities and are coordinated by eight O atoms. Various structures of the related compounds REMM′O5 (RE=rare earth metal; M=Si, Ge, and Sn; M′=B, Al, and Ga) are also discussed.

Benzo-18-krone-6 -Acetonitril (1/2): Kristallisation und Tieftemperatur- Röntgenstrukturanalyse / Benzo-18 -crown-6 -Acetonitrile (1/2): Crystallization and Low-Temperature X-Ray Analysis

1998 ◽  
Vol 53 (12) ◽  
pp. 1528-1530 ◽  
Author(s):  
Karna Wijaya ◽  
Oliver Moers ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Data Collection ◽  
Single Crystals ◽  
Title Complex ◽  
Monoclinic Space Group ◽  
Hydrogen Atoms ◽  
Space Group ◽  
X Ray ◽  
Mecn Solution

Abstract Benzo-18 -crown-6 -Acetonitrile (1/2), Crystal Structure Single crystals of the title complex resulted fortuitously during an attempt to co-crystallise MeN(SO2Me)2 with benzo-18-crown-6 from an MeCN solution at -30 °C. The crystal structure has been determined via data collection at -100 °C (monoclinic, space group P21/n, Z = 4). The nitrile molecules are located with their me­ thyl groups above and below the plane of the 18-membered crown ring, the Me hydrogen atoms being rotationally disordered about the MeCN axes; C(methyl)···O(crown) distances range from 309.4(3) to 384.9(3) pm.

scholarly journals PicW2 fromPicea wilsonii: preparation, purification, crystallization and X-ray diffraction analysis

2018 ◽  
Vol 74 (6) ◽  
pp. 363-366 ◽  
Author(s):  
Bei Zhang ◽  
Gangxing Guo ◽  
Fang Lu ◽  
Ying Song ◽  
Yong Liu ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Gel Filtration ◽  
Three Dimensional ◽  
Temperature Tolerance ◽  
Diffusion Method ◽  
Limiting Factor ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters

Low temperature is a major limiting factor for plant growth and development. Dehydrin proteins are generally induced in response to low-temperature stress. In previous research, a full-length dehydrin gene,PicW2, was isolated fromPicea wilsoniiand its expression was associated with hardiness to cold. In order to gain insight into the mechanism of low-temperature tolerance by studying its three-dimensional crystal structure, prokaryotically expressed PicW2 dehydrin protein was purified using chitosan-affinity chromatography and gel filtration, and crystallized using the vapour-diffusion method. The crystal grew in a condition consisting of 0.1 MHEPES pH 8.0, 25%(w/v) PEG 3350 using 4 mg ml−1protein solution at 289 K. X-ray diffraction data were collected from a crystal at 100 K to 2.82 Å resolution. The crystal belonged to space groupC121, with unit-cell parametersa= 121.55,b= 33.26,c= 73.39 Å, α = γ = 90.00, β = 109.01°. The asymmetric unit contained one molecule of the protein, with a corresponding Matthews coefficient of 2.87 Å3 Da−1and a solvent content of 57.20%. Owing to a lack of structures of homologous dehydrin proteins, molecular-replacement trials failed. Data collection for selenium derivatization of PicW2 and crystal structure determination is currently in progress.

Synthesis and Spectroscopic Investigations of New Linear Heterobimetallic Clusters [Me4N]3[(TOS3 )2Ag] (T = Mo, W). Crystal Structure of [Me4N]3[(MoOS3 )2Ag]

2000 ◽  
Vol 55 (3-4) ◽  
pp. 238-242 ◽  
Author(s):  
A. B. M. Shamsur Rahman ◽  
H. Boiler ◽  
K. O. Klepp
Keyword(s):  
Crystal Structure ◽  
Mass Spectra ◽  
Room Temperature ◽  
Trinuclear Complex ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Absorption Bands ◽  
Variable Parameters ◽  
Cell Parameters ◽  
Complex Anions

Abstract Red-brown crystals of a new bis(thiomolybdate) complex [Me4N]3[(MoOS3)2Ag] were formed at room temperature through the reaction of a solution of [Me4N]2[MoOS3] in MeCN with solid AgCN. They are monoclinic, space group P21/c with unit cell parameters a = 16.662(9), b = 9.464(3), c = 17.890(8) A, /3 = 101.87(2)°, Z = 4. The crystal structure was determined from single crystal diffractometer data (MoKα-radiation) and refined to R = 0.044 (3614 reflections, 236 variable parameters). The structure is characterized by trinuclear complex anions, [(MoOS3)2Ag]3-. According to Weissenberg investigations the homologous tungsten compound is isostructural. The infrared spectrum of the molybdenum complex (KBr powder) shows absorption bands at 884 (vs) and 871 (w) cm-1 (terminal v(Mo-0)), 483 (vs) cm-1 (terminal v(Mo-S)), 451 (vs), and 435 (w) cm-1 (bridging v(Mo-S)). The tungsten complex showed bands at 901 (vs) cm-1 (terminal v(W-O)), 478 (vs) cm-1 (terminal v(W-S)), and 435 (vs) cm-1 (bridging v(W-S)). The anionic mass spectra shows molecular ion peaks at m/z 524 and 700 for [(MoOS3)2Ag]- and [(WOS3)2Ag]-, respectively, as well as peaks for other fragments.

Preparation and crystal structure of SbV1.50InIII0.50(PO4)3 and (SbV0.50InIII0.50)P2O7

2008 ◽  
Vol 23 (3) ◽  
pp. 232-240
Author(s):  
Abderrahim Aatiq ◽  
Rachid Bakri ◽  
Aaron Richard Sakulich
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Room Temperature ◽  
Rietveld Method ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Orthorhombic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Synthesis and structure of two phosphates belonging to the ternary Sb2O5–In2O3–P2O5 system are realized. Structures of SbV1.50InIII0.50(PO4)3 and (SbV0.50InIII0.50)P2O7 phases, obtained by solid state reaction in air at 950 °C, were determined at room temperature from X-ray powder diffraction using the Rietveld method. SbV1.50InIII0.50(PO4)3 have a monoclinic (space group P21/n) distortion of the Sc2(W O4)3-type framework. Its structure is constituted by corner-shared SbO6 or InO6 octahedra and PO4 tetrahedra. Monoclinic unit cell parameters are a=11.801(2) Å, b=8.623(1) Å, c=8.372(1) Å, and β=90.93(1)°. (Sb0.50In0.50)P2O7 is isotypic with (Sb0.50Fe0.50)P2O7 and crystallizes in orthorhombic system (space group Pna21) with a=7.9389(1) Å, b=16.0664(2) Å, and c=7.9777(1) Å. Its structure is built up from corner-shared SbO6 or InO6 octahedra and P2O7 groups (two group-types). Each P2O7 group shares its six vertices with three SbO6 and three InO6 octahedra, and each octahedron is connected to six P2O7 groups.

Synthese und Kristallstrukturen von N-[ω-(Dimethylammonio)alkyl]- N´,N´,N´´,N´´-tetramethylguanidinium-chlorid-tetraphenylboraten / Synthesis and Crystal Structures of N-[ω-(Dimethylammonio)alkyl]-N´,N´,N´´,N´´- tetramethylguanidinium Chloride Tetraphenylborates

2010 ◽  
Vol 65 (7) ◽  
pp. 907-916 ◽  
Author(s):  
Ioannis Tiritiris ◽  
Falk Lissner ◽  
Thomas Schleid ◽  
Willi Kantlehner
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Room Temperature ◽  
Chloride Ions ◽  
Monoclinic Space Group ◽  
Temperature Structure ◽  
Space Group ◽  
Temperature Modification

Dicationic N,N´,N´,N´´,N´´-pentasubstituted guanidinium dichlorides 4a, b are obtained from the chloroformamidinium salt 2 and diamines 3a, b. N-[2-(Dimethylammonio)ethyl]-N´,N´,N´´,N´´-tetramethylguanidinium chloride tetraphenylborate (5a) and N-[3-(dimethylammonio)propyl]-N´,N´,N´´,N´´-tetramethylguanidinium chloride tetraphenylborate (5b) were synthesized from 4a, b by anion metathesis with one equivalent of sodium tetraphenylborate. The thermal properties of the salts 5a, b were studied by means of DSC methods, and their crystal structures were determined by single-crystal X-ray diffraction analysis. For 5a a solid-solid phase transition is observed at −156 ◦C to a low-temperature structure. The room-temperature modification (α-5a) crystallizes in the centrosymmetric orthorhombic space group Pbca (a = 13.1844(4), b = 13.8007(4), c = 34.7537(11) A° ).The guanidinium ions are interconnected via chloride ions through bridging N-H· · ·Cl hydrogen bonds, providing isolated units. The tetraphenylborate ions show some dynamic disordering in the crystal structure. The low-temperature modification (β -5a) also crystallizes orthorhombically, but in the non-centrosymmetric space group Pna21 (a = 13.1099(4), b = 69.1810(11), c = 13.5847(5) A° ) and consists of four crystallographically independent cations and anions in the unit cell. Compared with the room-temperature structure, a similar N-H· · ·Cl hydrogen bond pattern is observed in the β -phase, but the tetraphenylborate ions are now completely ordered. 5b crystallizes in the monoclinic space group P21/c (a = 10.8010(3), b = 14.1502(5), c = 20.9867(9) A° , β = 94.322(1)◦). In the crystal structure the guanidinium ions are linked via chloride ions through N-H· · ·Cl hydrogen bonds, but in contrast to 5a two infinite strands are formed along the a axis with the tetraphenylborate ions interspersed between them for charge compensation.

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