On verdigris, part II: synthesis of the 2-1-5 phase, Cu3(CH3COO)4(OH)2·5H2O, by long-term crystallisation from aqueous solution at room temperature

The title compound bis(1,4-diazoniabicyclo[2.2.2]octane) di-μ-chlorido-bis[tetrachloridobismuthate(III)] dihydrate, (C6H14N2)2[Bi2Cl10]·2H2O, was obtained by slow evaporation at room temperature of a hydrochloric aqueous solution (pH = 1) containing bismuth(III) nitrate and 1,4-diazabicyclo[2.2.2]octane (DABCO) in a 1:2 molar ratio. The structure displays a two-dimensional arrangement parallel to (100) of isolated [Bi2Cl10]4−bioctahedra (site symmetry -1) separated by layers of organic 1,4-diazoniabicyclo[2.2.2]octane dications [(DABCOH2)2+] and water molecules. O—H...Cl, N—H...O and N—H...Cl hydrogen bonds lead to additional cohesion of the structure.

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Ion-Exchange Reaction Of A-Site In A2Ta2O6 Pyrochlore Crystal Structure

Archives of Metallurgy and Materials ◽

10.1515/amm-2015-0234 ◽

2015 ◽

Vol 60 (2) ◽

pp. 941-944 ◽

Cited By ~ 4

Author(s):

M. Matsunami ◽

T. Hashizume ◽

A. Saiki

Keyword(s):

Crystal Structure ◽

Aqueous Solution ◽

Ion Exchange ◽

Room Temperature ◽

Electrode Materials ◽

Pyrochlore Structure ◽

Rechargeable Battery ◽

Ion Exchange Reaction ◽

Li Ion ◽

A Site

Abstract Na+ or K+ ion rechargeable battery is started to garner attention recently in Place of Li+ ion cell. It is important that A+ site ion can move in and out the positive-electrode materials. When K2Ta2O6 powder had a pyrochlore structure was only dipped into NaOH aqueous solution at room temperature, Na2Ta2O6 was obtained. K2Ta2O6 was fabricated from a tantalum sheet by a hydrothermal synthesize with KOH aqueous solution. When Na2Ta2O6 was dipped into KOH aqueous solution, K2Ta2O6 was obtained again. If KTaO3 had a perovskite structure was dipped, Ion-exchange was not observed by XRD. Because a lattice constant of pyrochlore structure of K-Ta-O system is bigger than perovskite, K+ or Na+ ion could shinny through and exchange between Ta5+ and O2− ion site in a pyrochlore structure. K+ or Na+ ion exchange of A2Ta2O6 pyrochlore had reversibility. Therefore, A2Ta2O6 had a pyrochlore structure can be expected such as Na+ ion rechargeable battery element.

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Crystal structure of 6-deoxy-α-L-psicofuranose

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989015022215 ◽

2015 ◽

Vol 71 (12) ◽

pp. o993-o994

Author(s):

Akihide Yoshihara ◽

Tomohiko Ishii ◽

Tatsuya Kamakura ◽

Hiroaki Taguchi ◽

Kazuhiro Fukada

Keyword(s):

Crystal Structure ◽

Aqueous Solution ◽

Cell Volume ◽

Title Compound ◽

Room Temperature ◽

Ring Structure ◽

Compound C

The title compound, C6H12O5, was crystallized from an aqueous solution of 6-deoxy-L-psicose (6-deoxy-L-allulose, (3S,4S,5S)-1,3,4,5-tetrahydroxyhexan-2-one), and the molecule was confirmed as α-furanose with a3T4(orE4) conformation, which is a predominant tautomer in solution. This five-membered furanose ring structure is the second example in the field of the 6-deoxy-ketohexose family. The cell volume of the title compound [742.67 (7) Å3,Z= 4 at room temperature] is only 1.4% smaller than that of β-D-psicopyranose, C6H12O6(753.056 Å3,Z= 4 at room temperature).

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Synthese und Kristallstruktur von Dinatrium-di-μ/-oxo-bis[trihydroxo-methylantimonat(V)] / Synthesis and Crystal Structure of Disodium-di-μ-oxo-bis[trihydroxo-methylantimonate(V)]

Zeitschrift für Naturforschung B ◽

10.1515/znb-1991-0202 ◽

1991 ◽

Vol 46 (2) ◽

pp. 139-142 ◽

Cited By ~ 7

Author(s):

Markus Wieber ◽

Udo Simonis ◽

Dieter Kraft

Keyword(s):

Crystal Structure ◽

Aqueous Solution ◽

Hydrogen Peroxide ◽

Thermal Decomposition ◽

Sodium Hydroxide ◽

Spectroscopic Properties ◽

Membered Ring ◽

Dimeric Molecule ◽

Synthesis And Crystal Structure

The oxidation of dialkoxymethylstibine with hydrogen peroxide in the presence of sodium hydroxide leads to the formation of disodium-di-μ-oxo-bis[trihydroxo-methylantimonate(V)]. The salt can be synthesized also by dissolving methanestibonic acid in an aqueous solution of sodium hydroxide. The crystal structure has been determined; it shows a dimeric molecule containing a four-membered ring with Sb -O -Sb linkages. Thermal decomposition and spectroscopic properties o f the com pound are discussed.

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Synthesis and Structure of 2D Cobalt(II)-tartrate Hydrate Coordination Polymers Crystallised from Aqueous Solution

BULLETIN OF CHEMICAL REACTION ENGINEERING AND CATALYSIS ◽

10.9767/bcrec.13.2.1342.213-219 ◽

2018 ◽

Vol 13 (2) ◽

pp. 213 ◽

Cited By ~ 1

Author(s):

Mohammad Misbah Khunur ◽

Yuniar Ponco Prananto

Keyword(s):

Crystal Structure ◽

Aqueous Solution ◽

Coordination Polymer ◽

Single Crystal ◽

Chemical Reaction ◽

Coordination Polymers ◽

Room Temperature ◽

Reaction Engineering ◽

X Ray ◽

Hexadentate Ligand

Cobalt(II)-tartrate hydrate coordination polymer is successfully crystallisedfrom aqueous solution at room temperature. Unlike previous methods, diammonium tartrate was used and reacted directly with an aqueous solution of cobalt(II). Single crystal X-ray and ATR-IR analyses were performed toward the synthesized crystal. The crystal structure displaysa (6,3) 2D sheet which then grow into a 3D hydrogen-bonded network. Tetra- and hexa-dentate dianionic tartaric ligands are observed in the crystal structure, in which the hexadentate ligand connects four different cobalt centres. This method is considered feasible, affordable, and simple for the production of functional polymeric cobalt(II)-tartrate hydrate. Copyright © 2018 BCREC Group. All rights reservedReceived: 17th July 2017; Revised: 30th October 2017; Accepted: 30th October 2017; Available online: 11st June 2018; Published regularly: 1st August 2018How to Cite: Khunur, M.M., Prananto, Y.P. (2018). Synthesis and Structure of 2D Cobalt(II)-tartrate Hydrate Coordination Polymers Crystallised from Aqueous Solution. Bulletin of Chemical Reaction Engineering & Catalysis, 13 (2): 213-219 (doi:10.9767/bcrec.13.2.1342.213-219)

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Crystal Structure of Two Different Hydrate Phases of Bis[2,4,6-tri(2-pyridyl)-1,3,5-triazine]cobalt(II) Diiodide

Australian Journal of Chemistry ◽

10.1071/ch9901269 ◽

1990 ◽

Vol 43 (7) ◽

pp. 1269 ◽

Cited By ~ 9

Author(s):

BN Figgis ◽

ES Kucharski ◽

S Mitra ◽

BW Skelton ◽

AH White

Keyword(s):

Crystal Structure ◽

Aqueous Solution ◽

Ground State ◽

Room Temperature ◽

Spin Component ◽

Asymmetric Unit ◽

Tridentate Ligands ◽

X Ray ◽

Structure Determinations ◽

Electronic Ground

The title compound crystallizes at room temperature from aqueous solution as two distinct hydrated phases, both monoclinic and characterized by single-crystal X-ray structure determinations. The dihydrate ('blocks') is C2/c, a 42.58(2), b 9.099(8), c 21.14(1)Ǻ, β 112.12(4)°, Z= 8; R was 0.048 for 3784 'observed' reflections. The c. 3.75 hydrate ('Tetrahydrate'?) ('needles') is P21/c, a 9.348(2), b 36.663(8), c 23.071(8)Ǻ, β 93.51(2)°, Z 8; R was 0.050 for 6042 'observed' reflections. There are one and two independent cations in the asymmetric unit of each structure; all cations have the metal atom 'mer' coordinated by a pair of tridentate ligands. In the C2/c phase, Co-N (central) are 2.057(4) and 2.063(4)Ǻ with N-Co-N 175.8(2)°; Co-N (distal) are 2.163(6)-2.187(6)Ǻ. In the P21/c phase, in the first cation, Co-N are 2.045(8) and 2.050(7)Ǻ (central) [with N-Co-N, 167.0(3)°] and 2.193(8)-2.216(8)Ǻ (distal), while, in the second, Co-N (central) are 2.030(8) and 2.042(8)Ǻ with N-Co-N, 168.3(3)°; Co-N (distal) are 2.164(8)-2.227(8)Ǻ. These Co-N distances are longer than those observed in the [Co( tpy )2]2+ cations hitherto studied ( tpy = 2,2′:6′,2′-terpyridine), in which the electronic ground state has an appreciable low-spin component.

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207Pb and 205Tl NMR on Perovskite Type Crystals APbX3 (A = Cs, Tl, X = Br, I)

Zeitschrift für Naturforschung A ◽

10.1515/zna-1987-1115 ◽

1987 ◽

Vol 42 (11) ◽

pp. 1313-1320 ◽

Cited By ~ 8

Author(s):

Surendra Sharma ◽

Norbert Weiden ◽

Alarich Weiss

Keyword(s):

Crystal Structure ◽

Aqueous Solution ◽

Chemical Shift ◽

Single Crystals ◽

Room Temperature ◽

Saturated Aqueous Solution ◽

Chemical Shift Tensor ◽

Chemical Shift Tensors ◽

Perovskite Type

By 205Tl and 207Pb NM R the chemical shift in polycrystalline samples of binary halides AX, BX2 and ternary halides ABX3 (A = Cs, Tl; B = Pb; X = Br, I) was studied at room temperature. The chemical shift tensors δ ( 205Tl) and δ (207Pb) were determined in magnitude and orientation on single crystals of the orthorhombic TlPbI3. The components of the δ(205Tl) tensor are δx (205Tl) || a = 611ppm; δy (205Tl) || b = 680 ppm; δZ(205Tl) || c = 1329 ppm; δiso(205Tl) = 873.3 ppm (with respect to 3.4 molar aqueous solution of TlOOCCH3). The chemical shift tensor of 207Pb in TlPbI3 shows two orientations. One of them is: δx (207Pb) = 3760 ppm, inclined 30° from b towards c, δy(207Pb) || a = 3485 ppm, δz(207Pb) = 2639 ppm inclined 120° from b towards c. δiso(207Pb) = 3295 ppm (with respect to saturated aqueous solution of Pb(NO3)2). The results are discussed with respect to the crystal structure and a model to explain orientation and anisotropy of the tensors δ(205Tl) and δ(207Pb) in TlPbI3 is proposed.In the system CsPbBr3-x Ix δ(207Pb) was studied on polycrystalline samples. The chemical shift increases with increasing x and negative excess shift is observed.

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Crystal structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II)

Acta Crystallographica Section E Crystallographic Communications ◽

10.1107/s2056989015007707 ◽

2015 ◽

Vol 71 (5) ◽

pp. 555-557 ◽

Cited By ~ 3

Author(s):

Marwa Mghandef ◽

Habib Boughzala

Keyword(s):

Crystal Structure ◽

Aqueous Solution ◽

Hydrogen Bonds ◽

Dihedral Angle ◽

Room Temperature ◽

Asymmetric Unit ◽

Slow Evaporation ◽

Acta Cryst

The title salt, (C5H6ClN2)2[CoCl4], was synthesized by slow evaporation of an aqueous solution at room temperature. The asymmetric unit consists of two essentially planar (C5H6ClN2)+cations [maximum deviations = 0.010 (3) and 0.014 (3) Å] that are nearly perpendicular to each other [dihedral angle = 84.12 (7)°]. They are bonded through N—H...Cl hydrogen bonds to distorted [CoCl4]2−tetrahedra, leading to the formation of undulating layers parallel to (100). The structure is isotypic with the Zn analogue [Kefiet. al(2011).Acta Cryst.E67, m355–m356.]

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Synthese und Kristallstruktur neuer 1,1,1,3,3,3-Hexaamino-1λ5,3λ5- diphosphazenium-Salze/ Synthesis and Crystal Structure of Novel 1,1,1,3,3,3-Hexaamino-1λ5,3λ5- diphosphazenium Salts

Zeitschrift für Naturforschung B ◽

10.1515/znb-1999-1105 ◽

1999 ◽

Vol 54 (11) ◽

pp. 1363-1370 ◽

Cited By ~ 1

Author(s):

Kai Landskron ◽

Wolfgang Schnick

Keyword(s):

Crystal Structure ◽

Aqueous Solution ◽

Temperature Gradient ◽

Single Crystals ◽

Room Temperature ◽

Gauche Conformation ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Acetonitrile Solutions ◽

Ray Methods

1,1,1,3,3,3-Hexaamino-1λ5,3λ5-diphosphazenium bromide [(NH2)3PNP(NH2)3]Br, nitrate [(NH2)3PNP(NH2)3][NO3], and toluene-4-sulfonate [(NH2)3PNP(NH2)3][CH3C6H4SO3] have been prepared by anion exchange in aqueous solution. Single crystals were obtained from acetonitrile solutions in a temperature gradient between 60 °C and room temperature. The crystal structures were determined by single crystal X-ray methods at room temperature. ([(NH2)3PNP(NH2)3]Br: P1̄̄ , Z = 2, a = 596.2( 1 ),b = 744.5( 1), c = 1114.4( 1) pm, α = 108.78( 1), β = 104.18(1), γ = 90.64(1)°, R 1 = 0.048, wR2 = 0.104; [(NH2)3PNP(NH2)3][NO3]: P1̄̄, Z = 2, a = 550.9( 1), b = 796.3( 1), c = 1115.7( 1) pm, α = 94.45( 1), β= 99.55( 1), γ = 101,53( 1)°, R1 = 0.033, wR2 = 0.095; [(NH2)3PNP(NH2)3][CH3C6H4SO3]: P21/c, Z = 4, a = 804.1(1), b = 596.1(1), c = 3218.7(3) pm, β = 94.59(1)°, R1 = 0.052, wR2 = 0.136). In the solid the three salts consist of discrete [(NH2)3PNP(NH2)3]+ cations and their corresponding anions. The PN4 tetrahedra in [(NH2)3PNP(NH2)3]Br are staggered, while in [(NH2)3PNP(NH2)3][NO3] the eclipsed conformation is preferred. The PN4 tetrahedra of [(NH2)3PNP(NH2)3][CH3C6H4SO3] show gauche conformation.

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A new hydrate of magnesium carbonate, MgCO3·6H2O

Acta Crystallographica Section C Structural Chemistry ◽

10.1107/s2053229620001540 ◽

2020 ◽

Vol 76 (3) ◽

pp. 244-249

Author(s):

Christine Rincke ◽

Horst Schmidt ◽

Wolfgang Voigt

Keyword(s):

Crystal Structure ◽

Aqueous Solution ◽

Diffraction Pattern ◽

Raman Spectra ◽

Room Temperature ◽

Magnesium Carbonate ◽

Water Molecules ◽

X Ray Diffraction ◽

X Ray ◽

New Phase

During investigations of the formation of hydrated magnesium carbonates, a sample of the previously unknown magnesium carbonate hexahydrate (MgCO3·6H2O) was synthesized in an aqueous solution at 273.15 K. The crystal structure consists of edge-linked isolated pairs of Mg(CO3)(H2O)4 octahedra and noncoordinating water molecules, and exhibits similarities to NiCO3·5.5H2O (hellyerite). The recorded X-ray diffraction pattern and the Raman spectra confirmed the formation of a new phase and its transformation to magnesium carbonate trihydrate (MgCO3·3H2O) at room temperature.

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